Microelectronics Using Electron-Beam-Activated Machining Techniques

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Microelectronics Using Electron-Beam-Activated

Machining Techniques*

KENNETH R . SHOULDERS

Stanford Research Institute


Menlo Park. California

I . Iiitrodurtiorl . . . . . . . . . . . . . . . . . . 137
A . General <!oticepts . . . . . . . . . . . . . . . . 137
I3. Background of The Present. Program . . . . . . . . . . 139
(!. 0bjectivc.s . . . . . . . . . . . . . . . . . . 142
D. Time Schedule for Various Objectives . . . . . . . . . . 141
I I . ltesearch Plan . . . . . . . . . . . . . . . . . . 144
A . General Coinponelit Considerations . . . . . . . . . . 145
U. Tunnel Etrect Component Dcaiyn and Inter(-onnection . . . . . 145
(1 . Accessory Component Design . . . . . . . . . . . . 146
11. Substrate Considerati0n.s . . . . . . . . . . . . . . 146
F. . Material Deposition . . . . . . . . . . . . . . . 147
F . Material Etching . . . . . . . . . . . . . . . . 148
G . Resist Production . . . . . . . . . . . . . . . 148
I3 . b:lec:tron Optical Systeiii . . . . . . . . . . . . . . 14!1
I . Equipment Integration . . . . . . . . . . . . . . 150
111 . Rlicroelectronic Component Consideratiotis . . . . . . . . . 150
A . General ('onsiderations . . . . . . . . . . . . . . 150
1% The Over-All System Specifivatioii . . . . . . . . . . 156
I V . Tunnel Effcct Conlponents . . . . . . . . . . . . . . 158
A. C;eornetry . . . . . . . . . . . . . . . . . . 15!)
B. Time Constants . . . . . . . . . . . . . . . . 1G3
(! . Tube Characterist.iw . . . . . . . . . . . . . . . 163
1> . Ihvironment . . . . . . . . . . . . . . . . . 165
14. Heating Effects . . . . . . . . . . . . . . . . 1G6
F. Cathode Formation and Properties . . . . . . . . . . . 167
C. . Vacuum Encapsulation . . . . . . . . . . . . . . 172
11. (!oinponcrit Lifetime . . . . . . . . . . . . . . . 175
I . Solid Stat(&'l'un~irl1CtTcc.t 1)evicw . . . . . . . . . . . 178
* This article was prepared with the sponsorship of the Information Systems Branch,
Ofice of Naval Research, under contract Nonr-2887(00) . Reprotkuclion i n whole OT ifl part
.
as permilled f O T any purpose of the United Stales G'overnmenl
135
136 KENNETH R . SHOULDERS
V . Accessory Components . . . . . . . . . . . . . . . 180
A. Secondary Emission Devices . . . . . . . . . . . . 180
B. Light Detectors . . . . . . . . . . . . . . . . 183
C. Light Generators . . . . . . . . . . . . . . . . 184
D. Micro Document Storage . . . . . . . . . . . . . . 185
E. Electrostatic Relays . . . . . . . . . . . . . . . 188
F. Electromechanical Filters . . . . . . . . . . . . . . 189
VI . Component Interconnection . . . . . . . . . . . . . . 190
A. Vacuum Tunnel Effect Amplifiers . . . . . . . . . . . . . 190
B . Memory Devices . . . . . . . . . . . . . . . . 193
C. Electromechanical Components . . . . . . . . . . . . 195
D. Steerable Electron Guide . . . . . . . . . . . . . 195
E. Plasma System . . . . . . . . . . . . . . . . . 197
VII . Sitbstrate Preparation . . . . . . . . . . . . . . . 197
A. Mechanical Formirig . . . . . . . . . . . . . . . 198
B. Substrate Cleaning . . . . . . . . . . . . . . . 199
C. Substrate Smoothing . . . . . . . . . . . . . . . 201
D. Terminals . . . . . . . . . . . . . . . . . . 202
E. Substrate Testing Methotls . . . . . . . . . . . . . 203
VIII . Material Deposition . . . . . . . . . . . . . . . . 204
A . Thermal Evaporation . . . . . . . . . . . . . . 205
€3 . Substrate Heater . . . . . . . . . . . . . . . . 213
C . Reactive Deposition . . . . . . . . . . . . . . . 215
1). Single Crystal Growth . . . . . . . . . . . . . 221
E. Instrumentation Methods . . . . . . . . . . . 222
IX. Material Etching . . . . . . . . . . . . . . . . 224
A. Molecular Beam Etching . . . . . . . . . . . . . . 224
B. Atomic Beam Etching . . . . . . . . . . . . . . 2'28
C. Ion Beam Sputtering . . . . . . . . . . . . . . . 229
D. Depth Control . . . . . . . . . . . . . . . . . 229
X. Reairct Production . . . . . . . . . . . . . . . . . 230
A. Evaporated Resists . . . . . . . . . . . . . . . 231
B. Chemical Decomposition Resists . . . . . . . . . . . 232
C . Multilayer Resist Production Methods . . . . . . . . . . 234
D. Compatibility with Electron Optical System . . . . . . . . 235
XI . Electron Optical System . . . . . . . . . . . . . . . 236
A. Micromachining Mode . . . . . . . . . . . . . . 237
B . Scanning Electron Microscope . . . . . . . . . . . . 246
C. Scanning X-Ray Fluorescence Probe . . . . . . . . . . 249
D . Mirror Microscope . . . . . . . . . . . . . . . . 251
E . Multiple-Cathode Field-Emission Microscope . . . . . . . . 253
F. Pattern Generator . . . . . . . . . . . . . . . 25'4
G . Construction Details . . . . . . . . . . . . . . . 256
XI1. High-Vacuum Apparatus . . . . . . . . . . . . . . . . 260
A . Requirements . . . . . . . . . . . . . . . . . 260
B . High-Vacuum Apparatus . . . . . . . . . . . . . . 261
C. Ultrahigh-Vacuum System . . . . . . . . . . . . . 265
.
D Integration of Apparatus . . . . . . . . . . . . . 273
XI11. Electron Microscopo Installutior! . . . . , . . . . . . . 275
MICROELECTRONICS 137

S I V . Domonst.rat,ionof hlirroma(.tiining . . . . . . . . 27G


A. Substrate Prcpn.ratiori . . . . . . . . . . . . .
. 277
13. Film Drposition . . . . . . . . . . . . . . .277.
C. Resist Exposing . . . . . . . . . . . . . . .278.
D. Etching. . . . . . . . . . . . . . . . . .280.
E. Disciission of IlrsiiltR . . . . . . . . . . . . . .281.
S V . Summary . . . . . . . . . . . . . . . . . .283.
A. hIicrorlect,ronic Component C'onsidcr,ztions . . . . . . .283.
B. Tunnel Effect Components . . . . . . . . . . . . . 285
C. Accessory Components . . . . . . . . . . . . . . 2%
D. Component Interconnection . . . . . . . . . . . . . 286
E. Substrate Preparation. . . . . . . . . . . . . . . 287
F. Material Deposit,ion . . . . . . . . . . . . . . . 287
G. Material Etching . . . . . . . . . . . . . . . . 287
H. Resist Production . . . . . . . . . . . . . . . . 288
I. Electron Optical System . . . . . . . . . . . . . . 288
J. Vacuum Apparatus . . . . . . . . . . . . . . . 289
References . . . . . . . . . . . 289

1. Introduction

A. General Concepts

It has become increasingly apparent that electronic data processing


machines have been applied as of now to only a few relatively simple prob-
lems, compared to the vast array of complex problems of the future. It is
conceivable that in only a few machine generations, TIC will be aided by
complex machines designed to perform economically many of the functions
of a n intelligent technician. Machines of the kind that we postulate might
well require over lo1' electronically active components-a number com-
parable in size to that of highly developed biological systems.
The greatest single obstacle to fabricating machines complex enough to
cope with future problems is our iiiabilit,y to organize matter effectively.
Many pertinent basic electronic effects are now known and usable; more
will undoubtcdly become acceFsible. To use these effects for the construc-
tion of complex systems, processes permitting the manipulation of matter
must proceed a t video frequency rates with due regard to the specialized
properties of electronic materials.
If we are to build machines to permit performance approaching-and
perhaps exceeding-that of biological systems, why not attempt to use
biological building methods and biological information-processing methods?
After all, the processes do work, and they can do so in a garbage can without
supervision. Nevertheless, it is suggested that there are other means within
the scope of our developing technology that are more suitable to our present,
138 KENNETH R. SHOULDERS
and future needs. Let us examine a few of the major differences betwrrn
biological organisms and our proposed electronic systems.
We would like to remove the severe environmental limitatioiis of bio-
logical systems. Preferably, our proposed machines should be able to func-
tion in a varuum, in corrosive atmospheres, i n a furnace, in Conditions of
strong nuclear radiation, and under the forces induced by high acceleration
or any other disorganizing conditions. Obviously, such machines should
give superlative performance under what is presently considered “normal”
environmental conditions-for example, in such an important matter as
long lived stability. Furthermore, such environmental immunity should
permit efficient coupling to the new and more energetic energy sources that
are becoming available. The rugged environment suggested above would
eliminate most, if not all, biological procesees. There are, however, elec-
tronic effects and materials that can survive and function in such an
environment.
We would like to pass on-from one generation of ninchinc to the next-
a i l organization that has been acquired or “learned” by the previous
generation. In the higher biological species, offspring must learn by personal
experience much of the information accumulated by their predecessors. I n
man, the learning process may take a third of man’s useful life-span. It
would appear advantageous for our projected electronic machine to have
built-in, initially, a considerable amount of previously acquired organiza-
tion; it, should also have the additional capability of reorganization and
expansion. This impoees on the building process a necessary capability
for passing detailed data on to the machine that is being built. Data in
the form of instructions as to components, interconnections, and states
appears to be needed; a previously organized machine would serve as a
model.
From the foregoing considerations, important constraints have been im-
posed on the selection of building processes, ueable electronic effects, and
materials. The process must be such that all the fabrication data of a
successful predecesEor can be communicated to the successive generations
of machines, in an economical length of time and with a minimum of human
mpervision. The fabrication processes themselves should be rapid enough
to tic able to take advantage of the very high rates of electronic communica-
tion now available. It appears mandatory to use parallel processing-
processing that would involve the fabrication and interconnection of many
components simultaneously.
The ability to function in extremely severe environments demands the
selection of refractory metals and dielectrics possessing the highest binding
energies. The properties of these materials make normal mechanical or
thermal methods of fabrication for complete machines too difficult to cope
MICROELECTRONICS 139

with ;subtle chemical reactions, which can replacc “brute force” mechanical
working or thermal burning, are required. Cleanliness, in extreme form, is
imposed as a necessary condition for reliable long-term operation. Such
cleanlincss of process can be achieved a t present only in ultrahigh vacuum
in which material is transported in elemental or vapor form during fabri-
cation.
What size ehould our proposed machine be? Let us assume that the
desired 10” electronic devices are built layer by layer on two-dimensional
surfaces; then the average size per device is determined principally by the
resolution of the process that can selectively localize necessary materials.
The process to be presented here has achieved a resolution of several
hundred angstrom units. From this consideration, and others described
later, the size of the ultimate machine appears to lie in the range between
one and several cubic inches. One may speculate on the implications of the
portability of such a complex machine. It would appear to be possible for
it to accompany a human-acting as a highly organized clerk-in order to
aid him in solving with unmatched speed and precision complex problems
a t the site of the problem. Direct communication between man and ma-
chine, in a language understood by man, through optical, acoustical, or
other means compatible with the human senses, would be essential to
surmount the artificial barriers usually imposed.
Looking beyond the boundaries of this program, it becomes apparent
that ultimately we would wish to divorce ourselves from the limitations
imposed by the low binding energies of solid materials. We require organ-
ization of matter to effect order, permitting growth in our intelligence
machine; a t the same time, increased operating rates imply increased
temperatures, with an ensuing tendency to disorganize. To surmount the
low binding energies of solids, it may be possible to construct plasma-like
structures in which elementary particles are organized spatially and tem-
porally in dynamic equilibrium, under the influence of applied fields.
Several aspects of the present program can be extended to form a natural
transition into this postulated class of machine.
In summary, we would like to build machines operating a t electronic
speeds, almost completely immune to the effects of a harsh environment,
with components and versatility sufficient to attain a critical degree of
organized complexity such that the machine itself may participate in the
further development of ever more powerful machines.
8. Background of the Present Program
This report is a qualitative and semiquantitative discussion of the various
problems that are being dealt with in an effort to explore the possibilities
and limitations of a class of integrated microelectronic devices, systems, arid
140 K E N N E T H R. SHOULDERS

fabrication methods. It is hoped that this review will help others select a
similar field of endeavor and that some of the devices and techniques dis-
cussed here will have direct application. It is recognized that this project
is a very ambitious one and that the end goal will not be reached for some
time. On the other hand, the author does not feel compelled to deviate
from the course he has taken of pursuing the end goal, rather than directing
effort toward interim devices and methods; the latter approach would surely
lengthen the time required to attain the more desirable goal.
I n the beginning of the writer’s work in this field, vacuum material
manipulation methods were used to fabricate resistors, capacitors, induc-
tors, vacuum tubes having secondary emission and field emission cathodes,
photoconductors, and electrostatic relays. Masking methods were used
with conventional thermal evaporation sources and the resolution of these
masks was carried to an extreme degree in order to investigate the prop-
erties of the microelectronic devices. No important deviations from the
expected characteristics of the devices were found due to scaling down the
size, but many material deposition limitations of masking and thermal
evaporation methods resulted in poor over-all results for the components.
Various unsuccessful methods were tried in an effort to overcome the
masking limitations. Among these were the application of ion beam tech-
niques, xerographic methods, optically produced thermal effects, and opti-
cally produced chemical resists in vacuum. The use of electron beams bc-
came the most promising method of producing the desired localized images
on a surface during the micromachining mode and also for the analysis of
various effects produced on the surface. Among the first methods tried, a n
electron beam was used to bun1 through a low tempemturc masking mate-
rial such as condensed carbon dioxide, but the energy density requiremeiit
was very high and breakdown of adjacent arcas resulted from inadvertent
electrical discharge. Later, oil films were polymerized on various surfaces in
a fashion described by Carr [ 11 and the resulting composite was developed
in vapors of substances such as mercury and zinc. Although interesting pat-
terns could be produced, they had very limited electronic application. It was
then discovered that silicone pump oils could be decomposed to silica by
the action of an electron beam, and that this resist layer of silica could serve
to protect an underlying film of material during a subsequent etching
process. Eventually, this etching process was carried out in a vacuum
chamber a t reduced pressure and became compatible with the deposition
and resist production operation.
At the present time the basic micromachining process is this: to deposit
a material to be selectively removed later; to deposit a thin layer of resist-
producing material and to expose this with elcctrons in some desired
MICROELECTRONICS 141

pattern; then filially l o etch thc first lnycr of material with :t mol(wd,zr
heam of an element that inakcs a volatile compound of thc mixterid bring
machined. Ilcfinemcnts in apparatus and tcchniqucs hnvc produccd rcso-
lutions in excess of 100 A for the process with very short csposure times a t
low current density for the electron beam.
Vacuum apparatus was developed for the processing of the chemicals
that had been introduced into the system. This consisted essentially of
providing w r y high bakeout temperatures for the apparatus and using
materials that were not affected by the chemicals. A great deal of me-
chanical manipulation is used in the various phases of the process. To
introduce motion it has been found advantageous to use differential pump-
ing methods in which the ultrahigh-vacuum chamber is surrounded by a
vacuum of mm Hg in which “0”rings for the many entry ports can
he used. The inner ultrahigh-vacuum chamber, on the other hand, which
can he raised to temperatures of 900°C, does not require the use of such
seals. I n this way the manipulation can be introduced into the ultrahigh-
vacuum chamber through small holes without undue leaks or contamina-
tion from organic materials.
The design of an electron optical system has been undertaken with the
aim of providing the many functions of analysis and micromachiniirg that
are needed without impairing the ultrahigh-vacuum condition desirable
throughout the processing of a system of electronic components.
Deposition equipment has heen improved; it is nearing the point where
knowing what to do with it is of more concern than further improvements.
The chief effort in the deposition equipment design is in iiitegrating it)
properly with the vacuum apparatus and other equipments so that it is
not limiting their performance. The design of a mass spectrometer is being
undertaken, and upon completion it will be incorporatcd in the process
control of the deposition apparatus.
Aftcr working with and considering many components of thc film type-
such as cryotrons, magnetic devices, and semiconductors-for application
to microelectronic systems, it appears that devices based upon the quaiitmi
mechanical tunneling of electrons into vacuum (field emission) possess many
advantages. They seem relatively insensitive to temperature variations
and ionizing radiation and they permit good communication with other
similar components in the system as well as with optical input and output
devices. The switching speeds seem reasonably high, and the devices lend
themselves to fabrication mcthods that could economically produce large
uniform arrays of interconnected componeiits. These componeiits are bascd
on the phenomena of field emission into vacuum, which has been under
investigation for many years by competent people and has a firm scientific
142 KENNETH R. SHOULDERS

basis. In our future discussion of thc hasic emission process the term “ficltl
emission" will usually bc used, and thr complete roniponrni will he referred
to as a “tunnel effect component.”
At prcsent the phase of integrating many isolated hits of thought and
apparatus has been reached. The isolated bits seem to fit together in a n
interesting pattern; however, only by actually going through the motions
of physical tests can the complete plan be verified or modified to accomplish
thc desired end. To accommodate unforeseen changes in any of the various
aspects of the program, the maximum flexibility in equipment design has
been sought. Flexibility tends to increase the initial effort and cost, hut]
this should be the most economical course in the long run.
The author would like to acknowledge the invaluable technical and moral
support of his many associates through the past years, as well as the
financial support of Stanford Research Institute; the Information Systems
Branch of the Office of Naval Research; the Electron Tubes Division,
Techniques Branch, of the U. S. Army Signal Research and Development
Laboratory; and the Solid State Branch of the Air Research and Develop-
ment Command, Air Force Cambridge Research Center.

C. Objectives
The general objectives in this area of research are to develop the proper
apparatus and techniques for electron-beam-activated micromachining and
to apply these tools to the fabrication of integrated groups of electronic
components.
Ultimately, such a program, aided by logic and system studies, will lead
to the fabrication of complete machines that could be used for real-world
general pattern recognition, real-time language translation, and should have
problem-solving and decision-making capabilities which are not available
in present machines.
The specific objectives for this program would be to first obtain the
proper tools for electron-beam-activated micromachining, such as the elec-
tron optical system, ultrahigh-vacuum apparatus, and mass spectrometer
controlled deposition and etching apparatus. Following the development, of
these tools, the techniques for micromachining would be developed to an
advanced stage while being applied to the fabrication of small groups of
selected electronic components. The components to be developed would he
selected to integrate well with themselves, their construction process, and
the microscopic size range in which they must function. These components,
based largely upon the quantum mechanical tunneling of electrons into
vacuum, would seem to suffice for high-speed computer switching and
memory, provide low noise amplification and communication filtering, and
MICROELECTRONICS 143

give optical coupling means in and out, of the system. The specific objectives
are listed as follows:
( I ) Provide an electron optical system capable of analyzing the phys-
ical, chemical, and electrical properties of microscopic components so that
they can he optimized without undue difficulty in spite of their reduced
size, This electron optical system u ould consist of a mirror microscope,
xannirig electron microscope, and X-ray fluorescence probe. The mirror
microscope would be capable of voltage measurements down to 0.2
volts and have a maximum rePolution of approximately 500 A. The scan-
ning microscope would h a w a resolution limit of 100 A. The X-ray
fluorescence probe would have the ability to analyze 10-13 grams of
material to 1% accuracy.
(2) Integrate the electron optical system with mabs spectrometer coil-
trolled deposition and etching apparatus in an ultrahigh-vacuum system
capable of reaching 10-lGmm Hg in one-half hour or less.
(3) Deviee vacuum tunnel effect devices of micron size with switching
times in the 10-lo Fec region which (a) operate a t about 50 volts (b) have
high input impedance (c) are insensitive to temperature effects u p to
1000°C (d) are insensitive to ionizing radiation effects up to the limits
of the best knovn dielectric materials, and (e) have a useful lifetime of
many hundreds of years.
(4) Devise light sensing devices of fractional niicroii size based upon
photoelectron emission from metal-dielectric matrices under high electric
field, which have a frequency response in the range of 100 Mc/sec, and
which have environmental immunity similar to the tuniiel effect devices.
(5) Devise cathodoluminescent light generating sources of fractional
niicroii size based upon the stimulation of a refractory phosphor by
field-emitted electrons.
(6) Deviee electromechanical devices ubing microscopic diaphragms
operated by electric fields in the lo7volt/cm region for low-voltage relays
and communication filters.
(7) Deviw modular groups of interconnected vacuum tunnel devices
which take advantage of the large dynamic range of lolo in operating
current to permit very low power dissipation in the quiescent operating
states. These circuits would t e specifically designed to eliminate low-
value plate resistors in active memories in order that the power dissipation
levels of both states of two-state devices are approximately 1O'O below
the dissipation level during switching.
(8) Investigate the limitations of periodically focused, electrically
steerable, electron beam guides to provide interconnections between ac-
tive components which will be less lossy than submicron sized wires, and
144 K E N N E T H R. SHOULDERS

to reduce power requirements and heating effects by conducting a n


electron bunch or pulse through relatively long paths giving up energy
only upon termination; making use of the interconnection flexibility such
that a considerable amount of logic can be performed by interconnection
control rather than by dcpendcnce on the logical properties of the active
devices only.
(9) Develop eclf-formation nicthods for active components in which
a chemical process, during formation, is controlled by a significant
electrical property of the component in such a way that the component
characteristics are automatically modified to conform to some previously
specified range of operation.
(10) Develop a document storage system by using electron-beam-
activated micromachining processes to store information in the form of
1O'O defined areas on a one-inch-square glass plate, each area representing
ten optical intensity levels-to be read by fractional micron-sized light-
sensing devices.
D. Time Schedule for Various Objectives
The work outlined above will not contribute to the nest generation of
machines made from micromodule components. I n the following generation
of devices, employing solid state integrated techniques, there may be some
slight interaction with electron-beam-activated machining methods such
as the selective masking of semiconductor surfaces for control of diffusion;
the various electron beam analysis tools may also contribute information
about the microscopic behavior of diffusion processes and give data on
surface effects.
The third generation of machiiies would seem to be the one to which
these techniques and devices would begin to contribute strongly. A great
deal of effort is needed to carry this program to the point of showing com-
pleted systems being fabricated in a few hundred hours, but one thing
that should become evident with such an electronic construction process
is that there would be a very short delay between engineering and manu-
facture of electronic systems made by these methods. No tooling u p is
needed for this electronic material handling process othcr than the construc-
tion of additional identical processing chambers and auxiliary control
equipment.

II. Research Plan

The problems listed iii the outliiic that follows represent most of the
areas of investigation that were indicated at the beginning of this work.
Initially, most of the scientific problems were worked on in a superficial
MICROELECTRONICS 145

or qualitative fashion iii ordcr to cxplorc economically thc wide latitudc of


problems and efficiently converge on desired results.
This exploration has removed the need for work in a great many areas
and has shown the confines of the experimental work, which in turn
allows the design and construction of integrated equipment without the
fear of obsolescence. Future phases of the work will begin to fill in scientific
gaps and generate new problems which cannot be seen in this first phase.
The following paragraphs detail in summary form the gcneral work plan:

,4.General Component Considerations


I . Application of scaling laws to determine optimum size range for
various electronic components for complex data processing sys-
tems.
2. Investigation of manufacturing feasibility for various one-micron-
sized electronic components.
13. Tunnel Effect Component Design and Interconnection
1. Component Design
(a) Determination of area of application for solid state and high-
vacuum devices.
(b) Determination of optimum impedance for vacuum tunnel ef-
fect devices and device of a geometry that optimizes gain and
bandwidth while minimizing current intercepted by control
and screen grids.
2. Interconnections and Circuits
(a) Design of low-loss circuits having negligible quiescent power
dissipation.
(b) Investigation of direct coupling, secondary emission coupling,
and optical coupling methods to provide minimum constraints
for logic operations.
(c) Investigation of periodically focused electron beam guides to
be used as electrically steered communication paths in micro-
electronic systems.
(d) Investigation of electron beam parametric amplifiers for low-
noise amplification in microelectronic systems.
3. Fabrication
(a) Determination of stability of metal-dielectric combinations
under operating conditions involving high thermal shocks and
intense electron bombardment.
1 46 KENNETH R. SHOULDERS

(1)) Investigation of encapsulation effcctivcncss using thin filnis


made by reactive deposition methods.
(c) Investigation of self-formation mcthods for vacuum tuniicl
effect devices having multiplc-tip cathodcs.
4. Test Methods
(a) Use of field emission microscopy and field ion microscopy to
determine physical, chemical, and electrical properties of ma-
terials used in tunnel effect, devices.
(b) Development of electron mirror microscopy to show operating
voltages and switching waveforms of microelectronic com-
ponents.
C. Accessory Component Design
1. Investigation of high current density, low voltage secondary cmis-
sion surfaces for tunnel effect component interconnection.
2. Investigation of photoelectron-emitting light detectors coupled
with current amplifying secondary electron multipliers.
3. Investigation of light emission from field emitted electron stim-
ulated phosphors.
4. Investigation of microdocument storage system using fractional
wavelength optical reading methods.
5. Investigation of electrostatic electromechanical relays.
6. Investigation of electrostatically driven electromechanical filters.

D. Substrate Considerations
I . Materials Determination-Determination of materials to bc used
and the optimum shape and size of the substrate.
2, Mechanical Preparation Methods
(a) Investigation of economical limits to grinding and polishing
operations.
(t)) Study of the effects of vacuum firing for normalizing polishrd
surfaces.
(c) Investigation of porosity of raw samples.
3. Terminals
(a) Study of the termination of thin films to gross terminals and
their encapsulation to prevent corrosion a t high temperature.
MICROELECTRONICS 147

(1)) Investigation of sturdy strain-frcc lend wire connections to


subst rat P .
4. Cleaning and Smootliirig
(a) Optimization of ultrahigh-vacuum electron beam cleaning and
smoothing methods for substrate preparation and intralaycr
smoothing.
(b) Application of test methods to indicate faulty surface.
E. Material Deposition
1. Thermal Evaporation-Determination of methods for obtaining
the maximum cleanliness of deposits.
2. Reactive Deposition
(a) Determination of smoothness, crystalline properties, and elec-
trical properties of various metals, metal carbides, borides,
osides, nitrides, silicides, and sulfides.
(b) Investigation of diffusion characteristics between adjacent
layers of material.
3. Crystal Growth
(a) Investigation of single crystal growth in presence of sweeping
thermal gradient on substrate with and without reversible
chemical reactions.
(b) Investigation of reduction of crystalline size by alloying and
admixing materials so as to obtain uniform and stable
polycrystalline materials.
4. Instrumentation
(a) Design and construction of X-ray fluorescence probe film
thickness monitor.
(b) Design and construction of ion gauge evaporation rate con-
trollers.
(c) Design and construction of rf mass spectrometer for evapora-
tion rate monitors, etching control, and destructive analysis
of film materials.
(d) Utilization of field emission and field ion microscopy to deter-
mine cleanliness of deposits, activation energy, and stabilities
of materials.
148 KENNETH R. SHOULDERS
F. Material Etching
1. Molccular Beam Etching
(a) Fundamental study of low pressure surface chemical reactions
so as to allow prediction of proper etchants and temperatures.
(b) Study of surface migration of etchant with intention of con-
trolling undercutting of resist and material redistribution.
(c) Investigation of multiple component etchants to increase va-
por pressure of material being etched.
(d) Investigation of side reactions produced with multiple com-
ponent etchants.
(e) Study of etching rate of various crystal faces and methods
of causing uniform etching by selective adsorption of different
materials.
(f) Investigation of depth control methods with and without
chemical barriers.
2. Atomic Beam and Sputtering Etch Methods
(a) Determination of effect of molecular beam etch a t a surface
bombarded by a high current density electron beam which
produces atoms and ions.
(b) Study of electrical property damage resulting from sputtering
and atomic beams.
3, Instrumentation
(a) Design and construction of high temperature substrate heater
that is chemically nonreactive.
(b) Design and construction of accurate temperature regulating
devices to control substrate heat.

G. Resist Production
1. Classification-Classification of electron sensitive reactions and
application of the ones best suited to micromachining.
2. Efficiency Limitations
(a) Study of polymerization mechanism in simple reactions and
electron multiplication process in multilayer complex reac-
tions.
(b) Analysis of maximum attainable efficiency vs. resolution in
optimum process.
MICROELECTRONICS 149
( c ) Study of electron absorption process in resist producing ma-
terials.
(d) Study of efficiency as a function of temperature and electric
field.
3. Resolution Limitations
(a) Investigation of electron scatter processes and X-ray pro-
duction and adsorption as fog-producing mechanisms.
(b) Study of material migration due to thermal and field enhanced
mechanisms.
(c) Investigation of etch-back methods to reduce background fog
effects.
4. Integration Investigations-Development of optimum resist-
production methods which integrate well with other system func-
tions, such as noncontamination of lens and film materials and
the adaptability of resist materials to vacuum handling methods.

13. Electron Optical System-Determination of the system most suited


to micromachining and analysis, which includes making a comparison
between magnetic and electrostatic instruments, cylindrical vs.
spherical lens elements, and a select ion of optimum electron velocities
for various modes of use.
1. Resolution and Sensitivity Limits
(a) Determination of rrsolution and coiitrast limit for scanning
microscope.
(I)) Determination of accuracy, sensitivity, arid resolution limit
for X-ray fluoresccncc probe.
(c) Study of voltage sensitivity, bandwidth, and resolution limit
of mirror microscope.
(d) Determination of resolution limit, for multiple field emission
cathode imaging microscope.
2. Distortion Liniitations
(a) Investigation of distortioii effects xhich would limit uniforni-
ity of field.
(b) Determin:Ltioii of maximtiin 1iuml)cr of rcsolva1)lc bits per
field.
(c) Study of mechaiiical and electrical instability which would
limit rcproducibility and registration.
150 KENNETH R. SHOULDERS
(d) Study and suppression of contamination effects and stray
charging.
3. Accessory Apparatus
(a) Design and construction of combiiicd X-ray detector and
electron multiplier.
(b) Design and construction of electrically operated substrate
micromanipula tor.
(c) Design and construction of pattern generator for micro-
machining.
(d) Assembly of monitor console to integrate various display
functions.
I. Equipment Integration
1. Ultrahigh-Vacuum Apparatus
(a) Design and construction of rapid-access equipnieiit capable
of being baked a t high temperature to remove chemical resi-
due betwceii deposition and encapsulation operations.
(b) Design and construction of contamination-free pumps for
ultrahigh vacuum.
2. Valves-Design and construction of large diameter, ultrahigh-
vacuum valves for separation of various operations having volatile
reaction products.
3. Manipulation-Design and construction of multichannel manip-
ulator having great, operational flexibility.

111. Microelectronic Component Considerations

A. General Considerations
1. CONSTHUCTION PROCESS CONSIDERATIONS

Our over-all component size is constrained by the construction techniques


to be within the limits of one-tenth of a micron and two microns. The
lower limit is set by the resolution of' the machining process. The upper
limit is indirectly determined by the maximum thickness to which films
can be deposited with desirable properties. Films thicker than a few microns
can be obtained, but i n this size range mechanical iorces come into play
which tend to cause severe strain a t the film boundaries unless the thermal
expansion coeficients of the various materials are matched. These strains
MICROELECTRONICS 151

niay not rcsult iii pecliiig of the filiris, hiit, tlicy ciihaiicc tliv diffuhion of
forcign matcrial along boundaricx
Thc dimensional aspect ratio of a d ivc devices is prcdoiniiitlully coii-
trolled by consideration of the impedancc level, both of the device itself
and of the coupling means between similar components. For semi-conductor
and vacuum devices, this aspect ratio usually approaches unity. Thus
since the component thickness will approximate one micron, the width and
length will also approach one micron, and the resolution of the machining
process must considerably exceed this value so as to produce the detailed
structure needed. When the Component size approaches the resolution of
the construction process there is a severe problem in obtaining uniformity.
At times it may be possible to couple a self-forming process with the prin-
cipal construction process and effect an improvement in over-all resolution
without complicating the primary process. An example of this that can be
found in normal machine processes might be the use of electropolishing to
remove burrs caused by an inexact machine tool cutting process; the
electropolishing does not necessarily affect the basic dimensions.
Some components seem inherently simple in geometry but require prop-
erties of materials which are either difficult to obtain or are unstable.
Other components require simple material properties, but have complicated
geometry. A transistor is an example of the first class and a transformer or
saturable reactor is an example of the second class. An ideal component
taxes neither the geometry nor the materials. One reason for the selecqion
of vacuum tunnel effect devices is that they seem to fit both of these require-
ments better than any class of component examined thus far. A single metal
and a single dielectric, chosen particularly for their stability, seem to be
the only materials needed to give a large range of electronic effects. The
geometry is extremely simple because the device consists principally of
the termination of the various wircs coming into the active area, as shown
in Fig. 1 (p. 160).
A choice is always possible between fabricating two-state or multilevel
devices. The multilevel dcvices usually require a higher resolution con-
struction process for any particular over-all size. The stability requirements
for the materials may also be higher, but carcful analysis of each case secms
in order, because occasionally the two-state device design has latent pos-
sibilities of being a multilevel device with the same stability, and therefore
is not being used in an optimum fashion. For the present, we will be con-
cerned only with two-state devices.
2. SCALING O F ELECTRICAL PROPERTIES

This program is investigating the reduction of size of electronic com-


ponents by about three orders of magnitude, namely, from one millimeter
152 KENNETH R. SHOULDERS

to onc micron. This reduction i n sizo will bring almit c.limgc~sin tdia h-
havior of materials, componcrits, mid thc m:Lnncr in which thc compoiictits
are used.
(a) Trunsrnission Line Loss. Oric of thc more unforturiate effects in
reducing the size of electronic systems is thc increased loss experienced by
transmission lines and tuned circuits. Assuming no change in resistivity,
a transmission line made from a suitably stable material like molyb-
denum-3000 A diameter, one inch long-has 100,000 ohms dc resistance.
Materials like copper or silver, having lower resistivity, are considered too
unstable for this purpose. The 3000 A diameter is the largest convenient
wire size that could be used with a 10,000 A, or one-micron-sized compo-
nent. Any calculation of line loss should consider the possibility of high
temperature operation of line sections rcsulting from cnergy dissipation
during component switching.
If conventional transmission lines arc to bc used for iiitcrroiinecting
microelectronic componcrits then the components should have a high input
impedance to avoid excessive current in the line and the attendant loss.
There is no rigorous relation between the input impedance of a component
and its output impedance, but the two are not usually independent. Thus
most semiconductor and magnetic devices operate, input and output, a t
relatively low impedance levels, while a few semiconductor and most vac-
uum devices operate at high impedance levels.
With the high resistance transmission lines described above, the choice
of high impedance level devices becomes mandatory if line loss is not to be
excessive. For example, if one component is to couplc with another located
10,000 component diameters away, approximately one inch, then the input
impedance of the most distant component should be a t least 100,000 ohms,
considering only dc losses in the transmission line. Highcr input impedances
would be required if ac losses were included.
(b) Q of Circuits and Filtering. The Q of tuned circuits is drastically
reduced when the components are scaled down uniformly by a factor N .
The resistance R varies as 1/N, the capacitance C and inductance L vary
as N , the product LC varies as N 2 , and the product RC is constant. The
Q of a circuit can be defined as wLlR. If the frequency w remains the same,
then the Q scales down as N 2 . Thus if all dimensions for a n inductor are
reduced from 1 centimeter to 1 micron-a scale change of 10-4-the Q of
the inductor would be reduced by a factor of lo", for the same frequency.
It will be difficult indeed to perform filtering operations in the conventional
manner unless other energy storage mechanisms are used.
RC filters are not affected by scaling their size, but they require stable
gain elements to achieve stable over-all performance. This stability may
be achieved by degeneration of active elements up to the limit of stability
MICROELECTRONICS 153

imposed by the temperature sensitivity of the resistance elements. In


scaling down a resistor all dimensions are assumed to be reduced, but in
fact the present day resistors are already films so that it would be difficult to
scale the thickness. The net result of this is that microresistors will either
have to have very low resistance values, and thereby couple poorly to the
active elements, or they will have to he made from materials of high resis-
tivity. A n unfortunate circumstance of high-resistivity materials is that
they are usually temperature sensitive to a very high degree, thus causing
large changes in filter characteristics when used in a n RC network. Sim-
ilarly, reactatnces-capacitive and inductive-may be produced by active
semiconductor dcviccs, hut these devices also exhibit considerable tenipera-
t ure instability .
The very fast thermal time constants of micro devices could tcmperature-
modulate filters in the megacyclc region and if the filter is temperature
sensitive a spurious signal results; i n addition, a drift is caused by slow
heating.
A useful filter for the micron size range can be devised, using bistable
switching elements in a data processing unit which handles the incoming
signals as digital data after appropriate time sharing and quantization
circuits have sliced up the signal. These methods are not very good for
handling small signals in the presence of large ones and may have to be
coupled with drift-prone RC filters to improve the over-all results.
Mechanical and acoustical filters scale nicely into the micron size range
for radio frequencies. The most important rcquirement for these devices
is that they be mechanically uncouplcd from the solid lattice that surrounds
them. This problem is somewhat equivalent to the vacuum encapsulatioii
problem where a membrane must be suspended free of the lattice over most,
of its area. Effective driving and pickup transducers for these mechanical
filter clrments can be clcctric field operated, being quite effective when sub-
jected to bias fields of about lo7 volt/cm.
Ultimately some of the molecular resoiiance arid adsorption properties
of materials may come into UFC as filters, but none have been investigated
in any detail.
(c) Optinziiin Time Constant. On first examiliation it would appear that
scaling down all dimensions of active componcnts would dccrease the RC
time coilstant and therefore increase the system opcratiiig speed almost
indefinitely. There is, however, a lower resistance set by efficient energy
transfer requirements, i t . , the resistance should not be less than the maxi-
mum transmission line resistance between two interconnected devices.
Furthermore, in most active devices the current rises faster than linearly
with applied field, and the resistancc scales down more rapidly than linearly.
Present, semiconductor tunnel diodes represent a component that exhibits
154 KENNETH R. SHOULDERS

too low an impedance for a system composed of one-micron-sized devices.


Although the vacuum tunnel tetrode, which is discussed in a later section,
tends to be a high impedance device, it may be possible to reduce its
impedance level to around the optimum of 100,000 ohms. Such a micron-
sized device will have an interelectrode capacitance of approximately 10-l6
farads, yielding a time constant of about 10-" sec. This value appears opti-
mum when based upon efficient energy transfer between components, one
inch apart. It is further to be noted that a one-inch transmission line op-
erating with a velocity of propagation approaching that of light, has a
10-lo sec delay, a time compatible with the switching time of the above
device.
(d) Heating Eflects. The integration of a large number of components into
a closely packed structure introduces thermal coupling between elements
to a degree not experienced in large-scale systems. Thus, if a number of
devices are to operate simultaneously, they must either operate a t con-
siderably reduced power density, be spaced sufficiently far apart, or the
circuit design must be such that large numbers of adjacent devices will never
be energized simultaneously. Generally, high power density is required for
high operating speed. Furthermore, low operating power density two-state
devices usually are quite temperature-sensitive. For example, the cryotron
is very temperature sensitive and is also a very low power density switching
device; ferroelectric and ferromagnetic devices, which operate at medium
power density, are fairly temperature sensitive; the power density and
temperature sensitivity of semiconductor devices depend somewhat 011 the
width of the energy gap of the material used.
The vacuum tunnel effect device appears to be the only device which
can satisfy most of the heating requirements. It operates at a very high
powcr density and up to temperatures barely under those which destroy
the refractory materials from which it is made. Individual micron-sized
devices, having a large surface to volume ratio, and made of refractory
materials, such as molybdenum and aluminum oxide, can be projected to
operate continuously a t a power density of lo* watt/cm2 C2.31.
It appears possible to operate LL vacuum tunnel device with a dynamic
dissipation range of loiobetween active switching and quiescent states. If
the dissipation during switching is watts for a 10-13 watt quiescent
condition, then the quiescent power for 10" such devices would be
watts, an entirely acceptable level. In comparison with the above, a con-
ventional solid state tunnel diode, with a dynamic dissipation range of only
20 to 1, would involve a quiescent power dissipation of watts per
device, and a total of lo6 watts quiescent dissipation for 10" devices.
Solid state tunnel devices made from only metals and dielectrics, as will
MICROELECTRONICS 155

be discussed later, seem to leiid themselves to low standby powcr but


would not exhibit a negativr resistance characteristic.
3. SCALING OF MATERIAL PROPERTIES

For metallic films 3000 A thick the bulk rrsistivit,y values may be used.
Traiismissioii lines haviiig 3000 A diiznicters may also exhibit bulk charac-
teristics even though the surface arca and electron scatter is very high.
Dielectric breakdown strength increases to loBvolt/cm for 3000 A thick
films of material that arc properly prepared [4].This is primarily because
the thickness is near the value for the electron mean free path in the
dielectric. An electron avalanche is not likely to occur under such conditions
and breakdown is forestalled. High field electrostatic devices can use this
increased breakdown strength to advantage.
As the size of our coniponents is scaled dowii the surface-to-volume ratio
rises and surface-tension forces play a profound role in determining the
shapes of the objects we can make. Materials tend to minimize their sur-
face energies and assume a spherical shape instead of remaining sharply
pointed. One of the limits to the smallness of the tip size that can be used
for field emission cathodes is the blunting caused by material migration and
surface tension forces at high temperatures [5, 61. Another limit that can
frequently be seen is the way that a surface layer of material, that is to be
diffused into a semiconductor device, tends to agglomerate and form into
sniall droplets [7]. This is partly caused by impurities accidentally present
a t the interface, and partly by surface tension forces.
Special problems in crystallinity are encountered when dimensions are
reduced to the few thousand angstrom unit region. Single crystal materials
require an unusually high degree of perfection over a large area if pinholes,
dislocations, or other anomalies, which could cause accidental diffusion of
materials from one laycr to another, are to be avoided.
Polycrystalline films are usually composed of arrays of single crystals
with few grain boundaries parallel to the film surface thickness but with
many grain boundaries perpendicular to the surface, permitting easy dif-
fusion paths in the thickness direction. Polycrystalline films having many
crystals in series in the thickness direction can be formed by evaporation
methods, but these are unstable and tend to recrystallize a t elevated tem-
perature to crystals having all sides approximately equal to the film thick-
ness. By proper admixing of materials such crystal growth can be
forestalled, but even with 300 A crystal size, which is considered small, there
would be only 10 crystals in a 3000 A-thick film, and the possibility of
having a direct diffusion path is large.
Certain electronic devices, like semiconductors, have detrimental sur-
156 KENNETH R. SHOULDERS
face recombination effccts which can adversely affect the electrical prop-
erties of the device with the reduction in thc sizc of these devices by thc
ensuing increased surface-to-volume ratio. The surface under consideration
includes not only the free surfacc but internal boundaries which represent
discontinuities in properties.
B. The Over-All System Specification
Many detailed considerations are needed to dictate the requirements
of a complex data processing machine [7a]. At this early stage of the pro-
gram the opinions formed about the details of the eventual machine are
not likely to be firm conclusions; however, opinions are needed to guide the
day-by-day activity. The tentative specifications for a complete machine
are presented here in order to show why various endeavors have been
undertaken.
1. NUMBER OF COMPONENTS

Based on a number of coiisidcrations a maximum system sizc of 10"


components, contained wit,hin a one-cubic-inch volume, has been selected.
The most important single factor in thc selection of this size is the resolution
of the machining process. Other factors that are strongly related to size
are : electronic effects, interconnection problems, uniformity of manufac-
ture, and stability of components. Furthermore, the economics of fabricat-
ing such a large system, with the methods to be described, have been
considered and found to be reasonable.
2. THE SHAPE AKD NUMBER O F LAYERS

A cube, one inch on a side, has been selected to house the data processing
system because of the adaptability of this shape to the manufacturing
process. Vacuum deposition mcthods lend themselves to the deposition of
material on a singlc surfacc. Past cxperiments have shown the feasibility
of depositing fifty layers of material 3000 A thick. More layers could con-
ceivably be dcpositcd but the resulting unevenness of thc top layers is
difficult to cope with. When thesc layers of materials arc used to make
components, wiring, shields, and crossovers, approximately ten layers of
components could bc made on each substrate from the 50 deposited layers.
The thinnest substrate that would secm reasonable to handle in the polish-
ing and lead wire connection operations would be 0.01 inch thick. The
major dimensions of the substrate are belicvcd to bc optimum a t about
one inch square. Larger sizes arc difficult to heat uiiiformly to the high
temperatures needed for reactive deposition and arc too flexible during
exposure by the electron image. Smaller sizcs are more desirable to work
with but entail a rrduction of thc numbcr of lead wircs that can bc attached
MICROELECTRONICS 157

to the substrate as well as a reduction of the area available for optical


communication to the machine. One hundred substrates would thus stack
to a one-inch cube.
Approximately lo8 one-micron-sized components can be accommodated
on one layer of a one square inch substrate when a 25% packing factor
for components is used. A cubic inch machine mould thus be composed of
100 substrates having tell layers or lo9 components per substrate, for a
total of 10" components.
3. EXTEItNAL COMMUEiICATION

Electrical, optical, and meclianical methods would bc available for


coupling the microelectronic system to the surrounding world. Lead wires
can be attached to each of the substrate edges and up to 80 wires per plate
could be secured; however, the difficulty of attaching and accounting for
these wires would tend to h i t the number to a smaller value. A few
hundred megacycles bandwidth per wire appears attainable. These wires
could serve as intersubstrate coupling and coupling to external devices.
Optical coupling between the adjacm t substrates could serve to connect
up to lo4parallel data channels with over 10 Mc of bandwidth per channel.
It is estimated that approxiinatcly 10% of the components would be used
as electrooptical generating and receiving t raiisducers. The light detecting
device would be a simple photoemissive surface coniiectcd to a vacuum
tunnel effect tetrode employcd as an amplifier. If more sensitivity is
needed, a secondary electron niultiplicr could be interposed between the
two units without undue complexity. l'he light generator would be a
refractory phosphor stimulated by elect roils drawn from a field emission
source and coiltrolled by a grid stiucturc in a triode geometry.
It is necessary to have a t,hin transparent substrate in order to allow
many channels of communicatioii between substrates without the use of
a lens. The light emitted from a small fluorescent source diverges until
it strikes the photoreceptor. If the substrate is 0.01 inch thick, then the
light that falls on the adjaceiit substrate could be confined to within
approximately 0.01 inch by moderate collimation a t the source. A 0.01 inch
resolution yields lo4 separate areas on the suhstratc. The optical channel
or surface that is to communicate with the external surroundings of the
machine could use a lens; this \voulCl allow over 10: optical channels in
the input field. The output of the machiiic to human observers or to rc-
motely located machines would also contain 106 individual channels.
It would also be possible t o ohtaiii ~nrchanicalor acoustical inter-
conunuriication with machiiic cireuith by providing thin hard diaphragms
as the encapsulation that vary the spacing of field emission diodes, thus
causing a current change. Thcse transducers could be czs m a l l as one micron.
158 KENNETH R. SHOULDERS

4. ENERGY SOURCE AND DISTRIBUTION

Under conditions of the maximum rate of processing data, up to 100


watts of power could be dissipated by this one-cubic-inch machine. The
data processing rate a t this power input would be approximately 10l6bits
per second. It is not expected that this rate would be used often, but, in
the event it was reached, the prime energy source would be a 100 volt
direct current supply drawing 1 amp. Auxiliary low current supplies for
electron multipliers and the like could be provided from external sources
or from internal converters.
The power distribution system would have to be an elaborate arrange-
mcnt to prevent faulty sections from disturbing the entire machine. Fuse
links built into the machine construction in the form of marginal wire
diameters would serve as an irreversible protection device. Electrostatic
relays could be employed as fault sensing devices and act as reusable
circuit breakers.

IV. Tunnel Effect Components

The quantum mechanical tunneling of electrons through an energy barrier


under the action of a high electric field is the basis of many known effects.
The source of electrons for an electrical avalanche leading to destructive
breakdown niay frequently be traced to field emitted or tunneling electrons.
The Malter effect [8] is reported to be a process for obtaining very high
secondary emission yield from a surface in vacuum; the effect is caused by
a positive charge being deposited on the surface of a thin dielectric which
covers a metal base and results in field-emitted electrons being drawn from
the metal through the dielectric and into the vacuum system. Cold
cathode tubes based on self-sustained secondary emission from MgO have
been reported to use a Malter effect or field emission source for their
emitted electrons [9]. Some dc electroluminescence has been reported to
stem from field emission [lo] and the Mott and Gurney explanation of
corrosion processes in thin films invokes quantum mechanical tunneling as
the source of the electrons needed to carry on a thin film corrosion process
[ll]. The utilizatioq of quantum mechanical tunneling in tunnel diodes has
recently become an active area of investigation for electronic components,
and before this, investigators of high-vacuum field emission have applied
the phenomena to various microwave, tetrode, and cathode ray tube designs
[12, 13, 13al.
It is our intention to use the principal and best understood form of field
emission, namely, the emission from a metal into vacuum, as the basis for
MICROELECTRONICS 159

a11 active rlrrtroiiic~romponriit in n microrlrci roiric. data processing sys-


trm. 111 addif ioii, infrared rlrtrc.tors a i d olrcf roluminrsc.enrc! genrrators
will hc iiivcstigatcd that niakr U ~ C of
' licltl emissioii from aiid into semi-
conductors.
A type of solid state tunnel effect c.oinpoiicnt has brcn investigated in
which only a metal aiid a dielectric arc used, the mctal supplying the
electxons and the dielectric giving the ricc~ssaryenergy gap. Experience
thus far with this class of dcvice show ail unfavorably low impedance, as
well as other problems such as traps caused by poor crystal structure in the
dielectric.
The greatest problem in applying field emission to devices is the in-
stability of the final device due to impurities and material migration.
Field emission can be a very high energy density effect, and when it is
coupled with low activation energy materials, as is done in most appli-
cations attempted thus far, material decomposition and instability is the
inevitable result. By using stable materials and very specific geometries
to avoid electron collision with dielectric supports, a much higher stability
could be expected.

A. Geometry
The most essential design criterion in a vacuum tunnel effect device is
to provide a method of changing the field a t the cathode in such a way that
the electrons that are emitted under the action of the field are not inter-
cepted by the control electrode (grid) that caused it. Thc use of the emitted
electrons depends upon normal elcctron ballistics, and conventional tube
design considerations are adequate. Many geometries are possible that will
achieve the desired results; two geometries that lend themselves to film
construction techniques are shown in Figs. 1 and 2. These configurations
could be constructed by successive deposition and machining operations.
The only part of the process that is not obvious upon inspection is the
method of supporting the conductor layer over the cavity in the lower
dielectric, and the closing of the entire cavity with encapsulating material.
These details will be discussed in Section IV, G. The multilayer geometry
shown in Fig. 2 is more difficult because of the higher registration needed
between layers.

1. THE CATHODE

The cathode preferably is made in the form of an array of small tips


superimposed upon a larger cathode lead wire. Tips having a radius of
approximately 100 A would be desirable from the standpoint of lowering
the operating voltage but wouId be difficult to fabricate and have a tend-
160 KENNETH R. SHOULDERS

CATHODE ANODE

CONTROL G R I D SCREEN G R I D

TOP VIEW

CATHODE ~
-SCREEN GRID

CONTROL G R I D - -ANODE

SIDE VIEW

FIG.1. Tunnel cffcct vacuum tetrode-single-layer type.

ency toward instability due to surface tension forces. It would be desirable


to fabricate an array of at lcast ten of these tips on the cathode area. Some
of the pertinent fabrication processes will be considered in Section IV, F.
The work function of the cathode material should be approximately

- TOP VIEW

SIDE VIEW

FIG.2. Tunnel effect vacuum triode-multilayer type.


MICROELECTRONICS 161

FIG.3. Field emission current density J as a function of applied surface electric field
F lor three values of work function in clcctron volts.

4.5 ev, the same as tungsten. If highcr work functions are used the voltage
requirements of the device are increased, as are heating effects. Low work
functions reduce the slope of the emission
current-grid voltage characteristic and thus
10 - I I I

lower the gain of the device. If the work -


function is carried to very low values,
loosely bound monolayers of materials such
as cesium are usually used and instability
results. At very low work functions the
devices also becotne slight,ly temperature
sensitive.
Graphs taken from “Advances in Elec-
tronics,” [G, pp. 94, 961 and plotted in Figs.
3 and 4 show the dependence of cathode cur- 5
2
rent density upon field, work function, and
-2 -
temperature. The range of current densities
of interest for 1O-Io cm2 cathodes is between I ,
-4
5 X lo6 amp,’cm? during tthe conducting 1 2 3 4 5
state to 5 X amp/cm2 during the qui- IO’/F (F IN VOLTS/CM)

escent state. This is a dynamic current FIG. 4. Field emission current


swing of loLo, which corresponds to 5x1 actual density J as a function of ap-
current swirlg of from 10-4 to 10-14 plied surface electric field F a t
and can be achieved by a change in field a t four temperatures for a 4.5 elec-
tron volt work function.
the cathode of approximately five to one.
Young [14] has observed a velocity distribution of 0.15 ev for field
emitted electrons, indicating that this is not a noisy source and that
162 KENNETH R. SHOULDERS
the energy spread is low enough to allow easy control of the emitted
electrons.
2. GRIDS

A geometry must be selected for the control and screen grids that will
allow their fields to effect the cathode without the electrons emitted from
the cathode being intercepted by the grids. The control grid would normally
operate positive with respect to the cathode potential and, by keeping the
grid near the plane of the cathode, electron current to it can be reduced to
very low values. The control grid may be run negative if it has a higher
work function than the cathode, or is smoother than the cathode. Normally
the grid would be formed smoother than the cathode so that negative
operation is possible, but a negative grid is more difficult to incorporate in
circuits because it cannot be connected directly to a preceding anode as a
positive grid can.
At a field intensity of lo7 volt/cm the mechanical force on the grids
amounts to about (540psi, and this force increases with the square of the
applied field. The grid electrodes must be firmly supported only a short
distance from their active regions to prevent distortion in the field and
unwanted mechanical resonances due to electromechanical effects. These
effects will be discussed later in the section on electromechanical filters.
The screen grid has the dual role of shielding the control grid from the
anode field while acting as a bias field electrode. In an effort to lower the
switching voltage of tunnel effect components it may be desirable to main-
tain the screen grid at a potential of 100 volts while the control grid and
anode swing between 3 and 10 volts. The high field from the screen would
serve as a bias field at the cathode while the control grid caused the nec-
essary current change. The secondary electrons and reflected primary
electrons at the plate must be effectively suppressed and prevented from
returning to the screen grid if this method is to reduce over-all heating
effects, including dissipation a t the screen grid. Secondary electron coupling
effectsto be discussed later would be ineffective a t low voltages and there-
fore low voltage operation would not be desirable if secondary emission
effects were required.
3. THE ANODE

Efficient collection of the emitted electrons is the principal function of


the anode, and heating effects caused by electron impact must be dissi-
pated to the surrounding lattice. The anticipated current density at the
anode is lo4amp/cm2 and the average electron velocity may be anywhere
from 3 volts to 100 volts, depending upon the final outcome of some of the
techniques for producing and stabilizing cathodes.
MICROELECTRONICS 163

The power density in a one-square-micron area could reach lo6watt/cm2


in operation. As will be discussed later in Section IV, E on Heating Effects,
the power density is lower by two orders of magnitude than the maximum
allowed.
The high field strength used in tunnel effect components effectively sup-
presses space charge effects. It has been shown that current densities of
lo' amp/cm2 can be obtained in the region of the field emission cathodes
with only a 25% space charge effect [15]. This low space charge would
allow efficient collection of electrons a t the anode for a current density of
lo4amp/cm2. By shaping the anode in the form of a shallow cup, a space
charge cloud may be purposely established as a means for suppressing
secondary electrons.
B. Time Constants
By considering the major energy storage mechanism, a n order of mag-
nitude calculation of time constant may be made for the vacuum tunnel
tetrodc. In this case, the interclectrode capacitance between screen grid
and anode is of major importance. Roughly this capacitance is 10-l6 farads,
assuming no increased capacitance due to interconnection wiring or charge
carriers in the grid-plate region. The discharge resistance, based on a current
of amp and a voltage swing of 50 volts between screen and anode, is
5 X lo6 ohms. The RC time constant is thus 5 X lo-" sec.
The transit time of an electron between cathode and anode in this partic-
ular micron sized device, operating a t 50 volts, would be about 10-13 see,
and no grid loading effects would be observed even a t 100,000 Mc, thus
reducing the need for complex geometries such as traveling wave tubes to
achieve high frequency gain.
C. Tube Characteristics
Tube characteristics for vacuum tuniiel effect devices have been obtaiiied
by both analytical and experimental methods; however, the analytical
methods have been applied only to geometries that involve high voltage
operation, in an effort to compare operation with the large-sized cathodes
that have been thoroughly explored by previous investigators.
I n early experimental work by the author, diodes and triodes were
fabricated by film techniques using high resolution masking and vacuum
evaporation methods. The masks were guided into position by a micro-
manipulator using a point projection field emission microscope to view
the results. The geometries employed had largely undetermined dimensions,
but over-all operating characteristics could still be determined. Operating
voltages in the range between 20 volts and 100 volts were readily obtained
with currents as high as 100 p a for short times. The devices were formed
164 KENNETH R. SHOULDERS

in a poor vacuum and not encapsulated, so that effects of contamination


caused the destruction of the device a t high current levels. This contamina-
tion causes a build up of a carbonaceous material on the cathode and other
structures by electron bombardment of the pump oils in the vacuum system.
The build up process produces a runaway emission and eventual destruc-
tion. Tube characteristics showing an amplification factor up to 100, a
plate resistance of several hundred thousand ohms, and a transconductance
of over 1000 pmhos per ma have been obtained in experiments operated
in the higher current range for a short time before destruction occurred.
Both negative grid and positive grid characteristics were obtained; the
most favorable case of positive grid operation gave a grid current suffi-
ciently low to measure a dc power gain of lo4.
Recent work a t Stanford Research Institute [l5s] on applied research
in microminiature field emission tubes has partly confirmed the earlier
findings by showing diode operation a t voltages as low as 25 volts for 10 pa
of current, yielding a power density of lo4watt,/cm2 on an anode of stain-
less steel which had not been outgassed. In other tests using molybdenum
anodes a power density in excess of lo7 watt/cm2 has been obtained. A
spacing of 2000 A was used in this test, or essentially the same dimension
anticipated for the final grid-to-cathode spacing. By using a 1000 mesh
screen of copper as a grid and micromanipulating a 1000 A radius tungsten
field emitter into one of the mesh openings, triode characteristics have been
obtained even though the anode was located more than one centimeter
from the grid. The voltage amplification for the triode geometry used was
over 5000 and the grid current was less than lo4below the anode current
when the grid was positive. A grid voltage of around 400 volts was neces-
sary for this experiment because of the large hole size in the 1000 mesh
screen. Tentative results using 5000 A hole diameters have shown good
cont,rol grid action with 25 volts applied.
A geometry similar to the triode shown in Fig. 2, but having a single
emitter tip, has been chosen for analytical treatment. The dimensions
chosen were: cathode radius 1000 A, cathode-to-anode spacing 7750 A,
control grid hole diameter 5000 A, spaced 7750 A from the anode. The
analysis considered grid emission and intercept currents. An amplification
factor of 20, a transconductance of 50 pmho/ma, a plate resistance of
lo7 ohms, and a power gain of 20 were found for the geometry chosen.
The grid voltage was 250 volts for an anode voltage of 1500. These operating
characteristics are far from ideal, but are in line with the large tip radius
used in the calculations. Complete data on this project can be found in
[15a]. It is the aim of this program to investigate analytically and experi-
mentally the properties of field emission tubes in an effort to optimize their
geometry arid determine the compatibilit,y of certain metal and dielectric
MICROELECTRONICS 165
c.on~binat,ioiisfor thcir coiistruction. Thc expcrinicntal appsrat 11s uscd oil
this program is csscntially a point projection electron microscope using tho
field emission tip as thc source. Rlicromaiiipulators arc provided that can
position the emitter in 5000 A diamctcr grid holes while under observation
by the microscope a t magnifications up to onc million diameters. The
micromanipulators have been calibrated to give about 40 A of motion per
dial division in any onc of three mutually perpendicular axes so that
variations in gcometry can be investigated. It has been the aim of this
program to use methods that are independent of electron beam micro-
machining so that early results can be obtained to help guide the later
application of micromachining work. The features that are readily observed
from this work to date arc that the operating current range is exceedingly
large-which will be a great asset in obtaining low quiescent power dissipa-
tion-and that the power gain and voltage gain are adcquatc.
D. Environment
It can be seen from Fig. 4 that the effect of tcmpcraturc on a cathode
having 4.5 electron volts work function is negligible for the conducting
state until a temperature of 3OOO"Ii is reached. The most important effect
of increased temperature for the entire array of 10" components is the
increase in quiescent current for the various deviccs. If 10" devices each
having 10-'0 cm2 of cathode area are raised to a temperature of lOOO"K,
under conditions which correspond to a current density of 5 x amp/cm2
per device and a field intensity of 2 x 107 volts pcr centimeter, then ap-
proximately 50 watts would bc dissipated by the entire group of components
(total current 0.5 amp, opcratiiig v o l t ~ ~ g100
c volts). Since thc maximum
continuous powcr dissipation for the system was postulated to be 100
watts, this leavcs only 50 watts available for dissipation of all the com-
ponents that are not in thc quiescent state, thus reducing the data process-
ing rate t o less than one half the original rate.
A temperature limit may also be imposed by electrical conduction within
the aluminum oxide lattice used for the dielectric of the system. Tests have
been made by the author, which are described in Sections IV, I, and VIII,
C, on aluminum oxide a t elevated temperatures by depositing the alumina
onto the tips of field emission microscopes, observing the emission current
that can be conducted through the lattice a t various temperatures, and
studying thc ability of the surfacc to retain a charge. The tests indicate
that properly deposited alumina is an adequate diclcctric for our purposes
to temperatures in the ordcr of 12OO0I<.
Mechanical cflects caused by the thermal cxpansioii of the construction
materials introduce another source of variation with temperature. Heating
the tunnel effect components would tend to reduce the field a t the cathode
166 KENNETH R. SHOULDERS
and rcducc the current,. This cffcct partly offscts thc quiesceiitncurrent!
iiicrensc from thc cathodc iipon heating.
Itadiat,ion damagc to vacuum tunncl cffcct coniponcmts would not RCCIkl
to be a problem until the radiation destroyed the dielectric. Radiation
damage study of field emission tips has been carried out by Mueller using
alpha particles and observing the effect on the lattice by field ion micro-
scopy [l6]. In this way Mueller was able to see the individual dislocations
caused by the radiation and to count the displaced atoms. Alpha particles
completely penetrate the small diameter tips and recoil collisions can be
seen and measured. The most obvious effect of radiation damage to the
cathode is to produce sharp projections which emit more easily; in addition,
the dislocations produced cause an increased migration of the cathode
materials and chiseling [17].
No data is available on the breakdown of dielectric materials a t high
fields in the presence of ionizing radiation, but results directly applicable
to tunnel effect components could be obtained by depositing dielectric
material on a field emission tip and irradiating it while observing the results.
By using inorgainic materials, and having device properties independent of
crystallography, it appears possible to operate vacuum tunnel effect devices
a t 10s/cm2more neutron flux than semiconductor devices. This value was
arrived at by comparing the effects of radiation on semiconductor devices
and a mica capacitor, which is somewhat equivalent to a tunnel effect
device insofar as radiation damage is concerned. The reduction in the size
of components causes fewcr ionizing events for any particular flux level,
but the events would be more devastating because they involve a larger
percentage, by volume, of the component.
E. Heating Effects
I t has been stated that the steady state power density for a one micron
sized device is as high as lo* watt/cm2. The principal energy transfer
mechanism is thermal conductivity; Holm [IS] has given the analysis of
the problem as it pertains to relay contact theory. Point projection X-ray
microscopy [ 2 ] shows that a 20 kv electron beam at 50 pamps for a total
input power of one watt may be continuously absorbed in a one micron
spot size. The target for this beam is usually a thin film of metal such as
aluminum or copper. In another X-ray source [3] a point of tungsten having
3X cm2 area was bombarded so as to give lo8 watt/cm2. The heat
conductivity in the film and the needle shape is shown to be adequate t o
allow many hours of continuous operation. Germer [19] has calculated the
power density of relay contacts just before closure, in which the principal
conduction mechanism is field emission, and his results agree with the
previous data. Evidently individual micron-sized devices could be expected
MICROELECTRONICS 167
to operate a t high power density as long as no other components were
immediately adjacent, in their nonquiescent states. A complicating effect
is that the thermal conductivity is not uniform, but depends upon the
location of wires and shields, since most of the conductivity is contributed
by the metal in the system. I t is espccted that although thermal conduction
will be the principal mode of heat transfer for individual components, when
the temperature rises due to switching activity in a cluster of components,
radiative processes will contribute largely to heat transfer to the external
environment .
The heating effects are not simple steady-state effects, but rather pulses
that will probably result in high thermal shock. No analytical or experi-
mental data is available to show the effect of this thermal shock on the
metal dielectric combiiiatioii in thc 10-lO sec region. Experimental data
obtained by the author in the 0.1 psec region using evaporated alumina
on the side of a tungsten field emission microscope tip did not show any
deviation from the steady state heating effects. The techniques, dimensions,
and materials used in these tests were the same as these intended for the
final component. The methods described by Mueller [20] allow quantitative
determination of the surface activation energies of alumina by steady state
methods, which permits interpretation of dielectric damage and migration.
Under the action of high temperature and high electric fields, electrolytic
action can occur in dielectrics and must be avoided a t all costs. Tesls by
the author on simple high temperature capacitorsusing reactively-deposited
aluminum oxide with molybdenum electrodes have been carried out in the
past and have showii that the dielectric is stable a t 800°C and lo7volts/cm.
These tests were not exhaustive and were only carried on for a few hours;
the tests are described in Section VIII, C on Material Deposition.
The work being conducted a t SRI on microminiature field emission tubes
[15a] is adequately iiistrumeiited to conduct investigations into the various
heating effects and will greatly assist the design of components and systems.

F. Cathode Formation and Properties

1. MULTIPLE TIP (’.%THOLIE FORMATION

1.ow voltage operation of tuniiel effect deviccs depends upon having small
cathode radii, but high current operation requires a large cathode area
because the current density per tip is limited to about lo7 amp/cm2. Some
geometry of small tips covering the 3000 A cathode surface will produce
thfl optiniuni opcratiiig coiiditioiis. ‘1’00 inany tips tightly bunched will
~cduc etlie field a t tlie tips and require highcr voltage, while too few tips
and widely spaced oiies will lower the niaximuni available current. In
addition to placement, thc tips will havc an optimum length-to-diameter
168 KENNETH R. SHOULDERS

ratio from the standpoint of fabrication ease. Field plots have been made
to help determine the optimum placement of tips; from various other
qualitative considerations the optimum tip size appears t o be about 200 A
diameter, 400 A long, and spaced about 1000 A center to center. An array
this size would have about 10 tips on the end of the 3000 A cathode. It
would not be economical to try to machine these tips on the surface of the
cathode; therefore, they must be grown by the use of crystallographic and
surface tension forces.
Tests have becri conducted by the author to confirm various opinions
about these growth methods. It has becn found that a film of cathode
metal such as molybdenum or tungsten can be made to agglomerate into
small isolated patches having roughly the shape desired. This is done by
depositing the cathode metal on a multiple layer of, first, aluminum oxide,
then aluminum, and then heating the composite until the aluminum
evaporates. The film thickness of the layers is 50 A for the aluminum oxide,
100 A for the aluminum, and 200 A for the molybdenum.
One possible explanation for the growth of isolated islands of molyb-
denum is that the molybdenum is alloyed with the aluminum and then
subsequently migrates on the aluminum oxide substrate film until surface
tension forces gather the material into small clusters where the aluminum
evaporates upon further heating. The tests were carried out on thin alumi-
num oxide films and the results were viewed directly in the electron micro-
scope. No tests have been made on field emission microscope cathodes to
verify the findings, or to check for foreign materials. I t is to be expected
that the aluminum oxide is iiichded in the cathode structure; this may have
distinct advant,agcs, as will he discussed later in t,hc section on cathodc
stability.
The development of a trustworthy method of forming multiple cathodes
is a very worthwhile undertaking for vacuum tunnel effect components,
and should be assisted by adequate instrumentation such as an electron
lens having high resolution t o image the multiple cathode array. The
field emission point microscope merges all images into one-if they originate
from a relatively plane surface-and docs not allow the investigation of
individual tips. One of the features of the high resolution electron optical
system to be dcscribcd later is that it will allow a large plane of material,
which has been proccsscd so as to produce a multiple cathode array, to be
viewed by imaging selected portions of the array and thus determine the
clectrical characteristics without removing the surface from thc ultrahigh-
vacuum system in which it is made. In addition, the features of scanning
clectroii microscopy, and X-ray fluorescciice spectroscopy, can be employed
to help converge the techniques to produce the desired surface. If desired,
this lens system can operate with a high temperature substrate, in the
MICROELECTRONICS 169

presence of strong clectrost,atic fields, to help promote the growt,h of tips


having high length-to-diameter ratios.
One of the limits that can be seen for the formation process is the inability
to heat the metal structures, for cleaning purposes, to a temperature beyond
the point where the dielectric and substrate become mobile. This corre-
sponds to approximately 1500°C for aluminum oxide. In our construction
process it is possible to use chemical methods to remove certain material
that is normally retained a t very high temperatures. An example of this is
the use of a hydrogen molecular beam to remove carbon from tungsten
[all. The uniformity of these formation methods may not be very high;
however, when they are coupled with self-formation processes, which are
discussed later, a high over-all uniformity may result.
2. CATHODE STlBILITY

The geometry of the cathodes must remain unchanged if electrical sta-


bilitry is t o be maintained in tunnel effect components. The cathodes may
become dulled in time by surface migration and surface tension forces at
elevated temperatures, or the tips may become sharper by surface migra-
tion in the presence of electrostatic fields [22]. Most of the work on the
stability of field emission cathodes has been done with 1000 A tip radii made
by electrolytically etching wire stock, and then heating the wire in vacuum
to 2800°C for cleaning. This cleaining operation requires very high tcmpera-
tures and results in diffusion of material and blunting of tips, thus making
the use of small radius tips difficult. Some experimenters have used 100 h
tip radii, but a great deal of care must be used in processing the tips. One
of the advantages offered by film deposition methods for the construction
of cathodes is that the tips are clean and gas-free upon completion, thus
avoiding the need for high temperature processing. In addition, certain
high vacuum chemical cleaning methods, such a s the removal of oxides
and carbides by hydrogen, can be used at lower temperatures [21].
The stability of small cathodes depends somewhat upon the geometry
being used. Herring [23] has pointed out that if the field emission point is
a slightly bulbous knob on a cylindrical column, and if the portion of the
knob a t its region of maximum perimeter contains a flat facet,, no blunting
is possible without an outward motion of this facet. Since an outward
motion would require two-dimensional nucleation, it would be practically
impossible under the weak motivat,ion of surface tension; consequently, the
shape would remain unchanged in time, even though it might be far from
an equilibrium shape. In addition to geometrical stabilization methods,
chemical barriers can be included in the system to stabilize migration.
The addition of alumina or thoria and certain metal carbides such as
hafnium carbide to the tungsten or molybdenum cathodes may serve as
170 KENNETH R. SHOULDERS

a diffusioii barrier. It, has bceii a long-standing practice in the vacuum tube
industry to carboiiizc thoriat>edtungsten filamcnts which contain thoria,
t o increase thc stability of thc surfacc.
In actual operation these small tips would always be under the action
011 an electric field to prevent dulling whenever heating occurs. The pos-
sihility of the small tips hecoming sharper during operation seems less
likely than the sharpening of larger tips because crystallographic binding
forcrs become stronger as the size is reduced. It has been noted that it
is not possible t o smooth a surface of anything except glassy materials
beyond a roughness of a few hundred angstrom units by heating processes
alone, because of the tendency of materials to crystallize. Mueller [24] has
shown the application of field evaporation using exceedingly strong fields
to smooth surfaces, but these fields exert more force than we use by a factor
of approximately 100.
:<.SELF-FORMATIOX
Sclf-formation methods are a class of supplementary process that follow
the principal micromachining process and simultaneously adjust the elec-
trical properties of all components in the topmost layer of components to
a uniform characteristic. This method of producing uniform components
drpeiids upon the activation of a chemical process by a significant electrical
property of the component in such a way that the component is modified to
conform more closely to a desired characteristic. The formation chemicals
must then be removed without, altering the uniformity. The formation of a n
electrolytic capacitor in which the applied voltage controls the dielectric
thickness is the most common example of self-formation methods applied
to a passive component.
To obtain uniform emission currents from each of a large number of
tunnel effect components having a single applied voltage is a most desirable
application of self-formation methods. Additional requirements for the
process would be to reduce grid emission by removing sharp projections
from the grid and to prevent grid current being intercepted from the
cathode by removing high emission angle anomalies from the cathode of
each device.
For the formation of tunnel effect components it is proposed that a n
entire array of lo8 devices ‘be fabricated by the micromachining process,
leaving off the final encapsulation layer, with all of the cathodes having been
deliberately formed too sharp for use. A voltage would then be applied to
all electrodes simultaneously in the presence of a molecular beam etchant
a t an elevated temperature. The voltage would then be raised slowly until
the sharpest tips begin emitting. These emitted electrons would supply the
necessary activation energy for the chemical process to modify the sharp
MICROELECTRONICS 171

tips only. This process should result in a degenerative dulling action that
will give a uniformly cmitting array as the voltage is raised to the operating
value. After operating voltage is reached the etchant is discontinued and
the tcmperature is raised to drivc off residues; finally the entire array is
sealed a t high temperature in ultrahigh vacuum. The variations of spacings,
work functions, and tip geometry would all be corrected by a change in
tip radius.
Vacuum tunnel effect devices appear to be a class of electronic component
very suitable for self-formation methods. The process requires a component
that is not sensitive to temperature, because elevated temperatures are
needed to volatilize the reaction products from the electronic surface. An
intermittent process using alternately low temperature reacting and high
temperature purging could accomplish the same end, however. The com-
ponent should have a geometry that allows the easy removal or redistribu-
tion of the materials, and vacuum devices have the highest dcgrec of
accessibility t o the surface being formed. A further requircmcnt is that the
electrical properties of the devicc havc similar operating characteristics
after the cleanup phase as they did during the formation phase. The work
function is the only property affected in tunnel effect devices during forma-
tion, being higher during the etching than in the clean state. After cleanup,
the work function returns to the clean metal value in a vcry uniform and
predictable way.
Cryogenic devices appear to be the least likely class of component to
self-form because they operate a t temperatures too low for chemical action.
For magnetic devices, self-forming would be difficult but possible. Semi-
conductor devices would be the next most likely class. Vacuum devices
appear t o be the best of all.
The tcsts that have been carried out by the author to indicate to what
extcnt the above notions are valid involvc etching tcsts on a single tip
field cmission microscope and then cleaning of the tip to determine residual
contamination. The formation-tests were performed on small tips having
an external applied potential of about 300 volts in order to prevent destruc-
tive sputtering of the tips by high energy ions. High vclocity ions formed
far away from the tip are known to strike the shank of the tip below thc
originating point of the ionizing electron because of the inability of the
high velocity ion to follow the field lines. This effect has the undesirable
tendency to sharpen the tip [25]. The forming agent (chlorine) was admitted
to the system in the form of a gas a t about mm Hg pressure and the
molybdenum tip was held at a tcmperature of about 4OO0C, or just below
the temperature of appreciable thermal etching. Upon raising the voltage
progrcssive dulling of the tip was cvidcnt by a dccrease in current. The
vncuum system was cleared of chlorine and thc tip was flashed t o a tempera-
172 KENNETH R. SHOULDERS

ture sufficient for cleaning; the original emission pattern was then observed
to be free of chlorides.
Mueller has sharpened tungsten tips in oxygen [25] by simply heating
them. This would seem to be the opposite effect to what can be accom-
plished with low heat and electrons.
The mechanism for self-formation is not kriowi, but the experimental
coiiditions suggest some form of solid state electrolytic plating of cathode
material from thc chloride or salt formed at the cathode surface. This
electroplating would riccessarily usr the emitted electron current to activate
the process and possibly to niaiiitain charge neutrality in the salt. Since a
strong field exists across thc salt, migration of material ~ o u l dfollow thc
field lines and not hc proiw to diftuse lstcrally. Under these conditions it
may be possible t o Luild up the tips that are t,oo sharp, and thereby reduce
emission. The dec.ompositioii of a volatile metal-carrying compound such as
molybdenum or tuiigsten chloridc or tungsten carbonyl under the action
of emitted electrons would rausc a similar effect. An example of this is
shown for the decomposition of tin chloride by Powell et al. p!6] and the
author has reduced small quantities of molybdenum chloride by electron
bombardment. None of thew reactions has been carried out on field ernis-
sion tips; however, these will be investigated during the course of the
project.
G. Vacuum Encapsulation
Vacuum encapsulation mcthods are similar to t he surface smoothing
methods that must be used betwcrn laycrs of components of either vacuum
or solid state type. If an array of one-microii-cubed comporients and t,heir
associated transmission lincs arc deposited on a surface, this constitutes
the production of a rough surfare that must be smoothed before proceeding
to the next layer. In present film methods using masks, this effect is not
evident because the edges are so diffusc and the components so wide that
a gradual thickness transition is produced. Doping methods of producing
integrated wires that do not rise above the surfacc are not considered
rcalistic in this size range because of the rscwxlingly high loss of the con-
ductors. If the surface is not filled or smoothed before proceeding to thc
next layer, a “pinhole effect” is produced, dielectrics are thinned a t the
steep boundaries, and the possibility of dielectric breakdown is increased.
One method of vacuum encapsulation resolves itself to the equivaleiit
problem of drawing a taut film across the top of an open cavity in a vacuum
chamber. To implement this in a way that does not interfere with the
component operation, or introduce undesirable impurities, several steps arc
needed. These steps consist of the deposition of a low melting poiiit ma-
terial, the fusing of this material to give a smooth surface, thc dcpositio~l
MICROELECTRONICS 173

of a thin film of rrfractory material, the rcinoval of the low melting ma-
terial by evaporation, a n d finnlly thc siritwing of thc refractory materi:tl
to the basc niatcrial in high v:~(~uuni.
The first technique devisrd to test thrsc methods was to strctah a thiu
collodion film, in air, across the rough surface of an evaporated aluminum
oxide film, dusted with alumina particles, to hc smoothed in much the same
way that a phosphor is covrrrd before evaporating a n aluminizing layer.
This film was then covered with LZ drposit of rvaporated silicon monoxide
or aluminum oxide, as is often done in electron microscope specimen
preparation. Hrating the sandwich to high temperatures drives out the
collodion without lifting the diclrctric film, and a t sufficiently high temper-
atures in vacuum the silicon monoxide film call be sintered to the underlying
film of aluminum oxide. The film sandwich is then tested in an electron
microscope or an optical microscope and moire effects or optical interference
tietween the f wo surfacrs near a bulge or anomaly indicate the separation of
the surfaces t o form a cavity. Thrrc is no way of testing the degree of
vacuum scalcd in the enclosurrs. Occasionally the top film ruptured and no
covering was produced; this was assumcd to be due to the strain, produced
hy very large particles of alumina, that wcre put on the surface to act as
support for the original collodion film.
An all-vacuum process was next testrd by the author to fiiid a substi-
tute for the collodion film that had t o bc applied a t atmosphrric pressure.
This test consisted of depositing a layer of myristic acid by evaporation,
followed by quick heating to the n-rlting point and then rapid freezing to
produce a smooth surfacc formed by surfacc tension. This laycr of mate-
rial was covcred by evaporation, nith :m agglomcrated laycr of sodium
chloride to produce isolated 100 A cubrs of niatrrial. A film of silicon
monoxide, 50 A thick, was thrn applicd t o cover the surface. Upon gentle
heating the rnyristjc acid drposit was driven out from under the silicon
monoxide, presumably by passing through the vents provided by the
sodium chloride crystals. Upon heating to high temprrature the sodium
chloride was driven out and the covering film sintercd to the base film.
A thin evaporated layer of aluminuin oxide coming from a low grazing
angle to the surface was used to close thr small holes produced by the
sodium chloride without penetrating to the basc layer, and then a thick
layer was deposited normal to the surfacr to increase the strength. Electron
microscope examination revraled that enclosures had been formed around
any hole or anomaly on thc surfacr that the original myristic acid film had
rovered, its surface tension being sufficient to hridge these cavitics.
These same surface tension methods coupled with evaporated deposits
can be used to support a diaphragm in the center of a cavity, similar to
those needed for producing mechanical effects like electrostatic relays or
174 KENNETH R. SHOULDERS

iriwhaiiiv:d filters. This must, 1)c donc in a multilnycr f:Lshion hy c.ovcriiig


the top of onc cavit,y with a film, constxuctiiig another cavity on the t q )
of this by micromachining, and finally closing this cavity by another film.
Similar encapsulation techniques have been investigated by Sugata et al.
[27] for the observation of specimens in gas layers in an electron microscope.
This technique seeks to encapsulate a specimen at atmospheric pressure
between two thin films. This is the inverse of our problem, but there are
some similar features.
The encapsulation methods investigated thus far have sought to test
the method of encapsulation but not necessarily to optimize the selection
of materials. The materials selection may be guided by the following con-
siderations :
(1) The most difficult problems arise in choosing the fill material which
is to flow on the surface and fill in voids by surface tension action. This
material must be able to wet the surface when liquid and freeze without
crystallizing into a rough surface. The decomposition products of this
material must be volatile and nonreactive with the electronic com-
ponent’s materials. The vapor pressure of the material a t the melting
point should be low enough to prevent rapid loss of material, but high
enough (just below the melting point) to be removed by sublimation,
since melting tends to distort the thin covering film. Organic materials
tend to satisfy most of the requirements, but are prone to contaminate
by production of metal carbides. Glasses of the sulfur-arsenic system are
also interesting. A wide range of materials are available for selection
and further tests are simple to conduct. Myristic acid and 1-octadecanol
partially satisfy the requirements.
(2) A suitable hole-producing material is one that agglomerates on the
surface, and can be removed by heating without reacting unduly with the
component or encapsulating film. Ionic materials and salts with a strong
tendency toward crystallization are the best class. Ammonium chloride
has shown favorable results for this part of the process.
(3) The thin film that is used as a supporting membrane must be able
to be evaporated to the surface without, agglomeration or surface mobility
because it must accurately shadow the tiny hole-producing aggregates on
the surface. This material must also be able to sinter to the base material
after the removal of the fill material, and be able to recrystallize to a
taut film without rupturing. A wide range of metals or dielectrics can
fulfill these requirements, but, in general, they are low-vapor-pressure
refractory materials that have chemical affinity for the substrate. Alumi-
num oxide is one of the best materials used thus far.
(4) The final encapsulating film can be almost any material that can
be evaporated and is stable enough to use in the final system. This layer
MICROELECTRONICS 175
can be backed up with a reactively deposited coating which is pinhole
free and stable. Aluminum oxide is also a good material for this part of
the process.
The lifetime of the components on a substrate will largely depend upon
thc effectiveness of encapsulation of the outer layers of material. It is
expected that a multilayer coating will be employed and that reactive
deposition methods will be used. Tests have been carried out in the past
by the author to help determine the materials and methods bcst suited for
encapsulation. In the absence of an adequate method for testing the degree
of vacuum in a micron-sized enclosure, corrosion methods were substituted.
When a thin metal surface is prepared in an ultrahigh vacuum and is
exposed to various gases, such as hydrogen and oxygen, the resistivity
changes by over two orders of magnitude if the film is thin enough to have
very little bulk electrical conductivity. A inonolayer of gas adsorption is
all that is needed to change the surface scatter of the conduction electrons.
The encapsulation tests to be described are based upon the possibility
of a similar change in resistivity if a foreign gas permeates the covering
laycrs.
A 100 A thick film of molybdenum was deposited on a sapphire sub-
strate that had been clcaned by heating to above 1200°C in vacuum. This
film was covered with an aluminum oxide film approximately 2000 A thick,
followed by molybdenum and silica films each of the same thickness. The
depositions were carried out a t around 9OO"C, as described in Section VIII,
C on Material Deposition. The films were judged stable a t 800°C by pro-
longed heating in vacuum and measurement of the resistance of the first
molybdenum film. The sandwich was removed from the vacuum system and
tested a t temperatures up to 600°C in various corrosive media such as
molten salt baths, and gaseous atmospheres such as carbon tetrachloride,
hydrogen, phosgene, and water vapor. Tests in air up to 800°C were also
conducted. None of the tests caused a properly encapsulated sample to
change resistance. Many experiments failed, however, due to either im-
proper choice of materials or processing methods. The greatest point of
weakness in all systems tested was a t the terminals, where dissimilar
materials and gross joining techniques were used. These tests have not
been correlated in any analytical way with the effectiveness of vacuum
encapsulation, but it is believed that there is a high probability of producing
good encapsulation by these methods; however, the only complete test
will be the performance of a micron-sized vacuum device.
H. Component Lifetime
Present field emissioii cathodes operated at lo7 anip/cni' have lifetimes
of 12,000 hours [ZS]. The deterioration mcchaiiisms are inevitably traced
176 KENNETH R. SHOULDERS

to gases being adsorbed on the tip and changing the work function or
being ionized by the emitted electrons and then sputtering the cathode.
These gaseous molecules come from adsorption sites on the container walls;
they migrate through the container, or are driven out of impure construc-
tion materials by heating effects or electron bombardment. By reducing
the quantity of these migratory materials the lifetime of tunnel effect
devices could be extended in an almost linear fashion proportional to their
reduction. By employing ultrahigh-vacuum deposition methods, the mate-
rials can be cleaned up by a factor of over 1000.
The use of dielectric materials in close proximity to the electron beam
will introduce the possibility of electron activated decomposition of the
dielectric and attendant contamination, but tests thus far have not revealed
any difficulty. “The Research on Microminiature Field Emission Tubes”
[15a] has as one of its specific goals the investigation of the compatibility of
dielectrics and field emission cathodes that are in close proximity.
One desirable effect in reducing the size of the envelope is the reduction
of surface area and the adsorbed contaminants that are contained on it.
If the cathode is considered a sink for contaminants and the surface of the
envelope a source, then the improvenient in lifetime is proportional to the
reduction in envelope surface area; in our case this is a factor of about
over large glass envelopes. Diffusion effects through the encapsulation
material, outgassing of the construction materials, and decomposition would
limit the lifetime long before this limit was reached. A strong ion pumping
action is expected in a one-micron-sized tunnel effect device because of the
high electron current density throughout the volume of the device even in
the quiescent state, where the current density is around amp/cm2. Dur-
ing the switching cycle or active state the temperature and the current
density may reach high peak values that serve to desorb gas from active
surfaces and drive foreign material back into the encapsulation and allow
it to continue diffusing throughout the system. A small amount of diffusing
niatcrial is inevitable, but, it should be kept in the encapsulation material
instead of being allowed to concentrate on the active surfaces.
Young [29] has recently shown that certain metals containiiig oxygen
can be made to liherate oxygen under the action of electron bombardment
without heating. l‘ungsten and molybdenum liberated gases readily, while
titanium seemed less troublehome. This rcsult ran be predicted from the
stability of the oxides. Gross field emission devices use anodes having this
decomposition effect and would be expected to show shortened lifetime.
Clean materials would solve this problem, :tnd vacuuni handling techniques
produre tlic. c*leniicbhtrn,ztcrials.
If the materials that compose a coiiipoiicnt wcre perfectly stable and 110
K ~ W material were :idded then the compoiicnt would have an infinite life-
MICROELECTRONICS 177

time. The binding energies of materials and thr opwating tcmprratur~s


determine the stability of the component. Vacuum tunnel effect componcnt,s
need only a single type of metal and dielectric, and these materials can be
chosen to have maximum binding energy without having to compromise
an electrical property. These components are able to operate at high tem-
perature, but if the lifetime of the component is the prime concern, then
they may be operated a t 10x1- temperatures; in this case, however, the data
procewing rate of the entire inachiiie will be reduced because fewer com-
ponents can be permitted to switch per unit of time since dissipation heating
is maximum during switching.
All active electronic components are apparently disturbed to a similar
degree by foreign materials. The smaller components will show a higher
sensitivity to a fixed number of foreign atoms simply because these atoms
represent a larger percentage of the active region. If a component is con-
sidered to be a certain volume of material embedded in a finite lattice of
encapsulating material, then some of the difficoltics in stability will arise
from the constant flux of foreign material dif'fusing through the volume of
the component, affecting the active elcctroiiic surfaces. If no sinks for
this foreign material are allon.ed to causc accumulation, then a vacuum
device and a solid device would have equivalent stability. Micron-sized
vacuum tunnel effect components appear to avoid establishment of im-
purity sinks hecawe of the high electron current densities and the attendant
ion pumping action of the device. Sinks for foreign material can be provided
in a solid system by having material concentration gradients or internal
surfaces. Both solid state devices and vacuum devices can be influenced to
an equal extent by these traps, but the vacuum device does not have sur-
faces other than the principal electronically active oiics to cause difficulty.
It, is important to reduce thermal gradicwts and other strain producing
mechanisms a t the external surfarcs of tlic bystem in order t o reduce dif-
fusion into the system by hf rchs corrosion mechanisms. Similarly, external
electric fields should I,c avoided in order to reduce electrolytic action.
With small area enclosures the amount of material that is evaporated
from the various electrodes and distributed to the dielcctric supports must
be very small in order to prevent a continuous conducting film being
formed on the surface. A coating of 50 A thick would cause great difficulty
in operation; however, the electrical characteristics of the device would bc
impaired Ixcause of the loss of mctal from the clectrodcs before the above
twndition was reached. Extremely high temperatures or high sputtering
rates nould 1 e needed to move much nietal to the dielectric surface, butj
the dielectric could be transported through surface niigration to the metal
electrodes a t temperatures as low as 1300°C; this is another reason for
including an iiiitially small, aiid hopefully saturated, aniount of dielectric
178 KENNETH R. SHOULDERS

with the cathode mctals, as discussed in the section on multiple cathode


format ion.
Mueller has recenlly shown [IG] that the sputtering of field emission tips
by gas atoms produced dislocations in the tips which caused an increase
in surface migration, and therefore the chiseling action described by Dyke
[22]. Individual atoms were observed in the field ion microscope and dis-
locations could be seen at the surface. Data on material migration effects
both in the bulk and at the surface has bcen obtained by field emission
microscopy. Surfaces have becn formed that are atomically clean with
accurately measured radii for even these submicroscopic surfaces. All of
these direct observation methods are available to tunnel effect component
designers who have the job of optimizing the electrical and mechanical
stability problems. Such powerful tools help assure the reliability of tun-
nel effect components.
The smallest electronic component presently known is the field emission
device. Even though the envelopes are large at present the cathodes have
tjhe same area of 1O-lo cm that we intend t>ouse eventually. If it is assumed
that the reliability of electronic components varies directly with the active
area, for a given amount of coritamination wandering into the active area,
then the present large sized vacuum tubes and semiconductor devices would
have to show about 10l2hours of operation to be equivalent in stability to
present field emission cathodes.
Conventional electronic devices that are reduced in size by using thc
same relatively unclean techniques employed for the large species would be
expected to have a very short lifetime, and microelectronic construction
methods therefore require techniques involving a high order of cleanli-
ness. With a degree of cleanliness that seems attainable with state-of-the-
art methods, several hundred years of component stability would seem
reasonable.

1. Solid State Tunnel Effect Devices


Solid state tunnel effect devices were investigated a t least as early as
1935 when De Boer [30] made diodes by evaporating successive layers of
metal and dielectric in such a way that the cathode was rough and yielded
field emission electrons when a voltage was applied to the sandwich. The
current in the reverse direction followed the field emission equation very
well, but the current in the forward direction obeyed a V3I2law, as if caused
by space charge effects. This space charge was probably due to a large
number of traps that set up a negative space charge. De Boer obtained
about 1ma of current at 0.05 volt and 25 ma a t 0.15 volt using a potassium
cathode, a calcium fluoride dielectric, and a silver anode.
MICROELECTRONICS 179

In Russia, Volokobinskii [31, 321 has iioted tunnel effects in solid sys-
trills composed of metals and dielectrics; Malter [8] effects* are thought
to be based upon field emission electrons being drawn from a metal cathode
through a pure dielectric layer and into a vacuum.
Methods of using solid state systems of metals and dielectrics for the
construction of field emission triode switching components have been pro-
posed by the author and summarized by Highleyman [33]. These methods
involve the use of refractory metal cathode areas with raised anomalies to
assist tunnel emission and to define the emitting area. Grid structures
consist of either thin metal films with appropriate electron transmission and
absorption characteristics, or thicker metal films with physical holes
aligned with the cathode anomalies to prevent excessive grid currents. The
anode is located adjacent to the grid and all electrodes are immersed in
and separated by solid dielectric, such as alumina made by film deposition
methods.
Recently, Mead [34] has shown an analysis and some experimental
results for a pure metal and dielectric type of tunnel effect triode made by
alternate layers of aluminum and oxidized aluminum. Mead’s conclusion
was that semiconductors are not necessary; that a triode tunnel device
would replace a tunnel diode; and that the devices must be made by very
refined processes. These remarks are substantially in agreement with our
findings.
Some tests were conducted in 1956 by the author on field emission into
solid dielectrics by employing a point projection field emission microscope
wit,h evaporated coatings of aluminum oxide on the tip of either tungsten
or molybdenum. By using this method the active area of emission could
be accurately defined and current density measurements made. Films from
a few monolayers thick to several thousand angstrom units thick were
deposited on tips with radii from 200 A to 1000 A and the current-voltage
plots were made both before and after the dielectric deposition. It was
noted with some surprise that the field required for the appearance of
emission was the same both before and after the deposition. The only real
diffcrence the addition of heavy dielectric layers made was to limit the
current density to around lo3amp/cm?. At this point the tip exploded and
ruined the experiment. Thin layers below 100 A thickness did not cover
the tip uniformly and heavy emission current could be drawn from around
the crystals of alumina. Heavy coatings seemed to have an instability in
the emission pattern that might be construed to be traps changing their
space charge effect, although the same effect would have been caused by
surface charges from electrons or ions. The emission stability was much
* See p. 182.
180 KENNETH R. SHOULDERS

more tempcraturc-dcpcndcnt than for thc metal-vacuum field emission casc.


Although the solid state turincl device could probably be developed int.o
something useful, it has largely been replaced by the vacuum tunnel effect
device for our purposes because of the following unfavorable characteristics :
it has higher temperature sensitivity (probably due to trap effects); lower
input impedance due to electron scatter in the lattice; and less device
uniformity due to dependence on crystalline properties in the dielectric
lattice. I n addition, self-forming methods arc difficult to apply. On the
favorable side the solid state device can be made to operate a t lower
voltages than vacuum devices; it probably has a much wider power range
and lower quiescent power than semiconductor devices; and it may have
a lower surface migration of materials, as compared with the vacuum device.
However, boundary diffusion may be troublesome.

V. Accessory Components

A. Secondary Emission Devices


There are two priiicipal uses for secondary electron emission in the
microelectronic system under consideration. Amplification of low level
photocurrents can be greatly facilitated by electron multipliers, and grids
of tunnel effect devices can be driven positive upon receipt of a burst of
negative electrons if the secondary electron emission ratio is greater than
one. A thin-film transmission-type electron multiplier similar to the one
described by Sternglass [35] is represented in Fig. 5 . For small signal

PHOTO SURFACE
ENCAPSULATION

FIG.5 . Thin-film transmission-type multiplier phototube.

amplification, such as photocurrent multiplication, this type of device


may have considerable application; however, for large voltage swings the
thin diaphragms may resonate mechanically a t frequencies within the
pass-band. The spacings that would be employed in this device would be
around 2000 A and the film thickness would be about 200 A. A maximum
diameter of two microns would seem permissible if the films were taut.
MICROELECTRONICS 181

The voltage between electrodes would be approximately 100 volts to


obtain a yield of four for a niolybdenum-alumina secondary emission
surface operating at a field intensity of nearly lo7 volt/cm. Five stages of
multiplication would give a current gain of 5000 with a transit time spread
low enough to allow gain up to lo5 Mc. T5nch dynode in a large array of
multipliers could be operated from a common power supply source.
For large signal applications a inore sturdy design is called for. The
design shown for the dynodc iii Fig. ci is similar to the design of Weiss [36]
and is urcd herc as a secondary emission amplifier. When the dynode is
struck by high velocity electrons, mow electroils leave the electrode than
arrive; thus the electrodc is driven positive and clampcd near anode
potential. Skellct t [37] describes various ways of usiiig secondary emission
to achieve circuit functions with a devicc similar to this. The purpose of
this particular circuit is to drive the grid of the top triode, in the series-

ANODE
SECONDARY
EMISSION
CWTING DYNDDE- OUTPUT

GRID

CATHODE

GROUND

FIG.6. Srcorid:iry emissiou nmpliF,er couplcd n i t h a turinel effect vacuiiiii triode.

connected triodes, positive without haviiig to suffer degeneration due to


cathode follower action. This will be described in more detail in Section VI,
on iiitcrcoiinect ions.
Secondary emission surfaccs are iiorrnally associated with instability;
however, close inspection reveals that the surfaces tested could be predicted
to be unstable because they are made from thermally unstable materials
such as alkali halides [38], or electrically unstable materials such as mag-
nesium oxide [39]. Even materials such as aluminum oxide, which is in a
stable class of oxides, frcquently have uiistable hydroxides included in
them because they are produced by electrolytic processes. Aluminum
oxide must be fired to over 900°C to produce a stable alpha phase crystal
structure. Impurities must be reduced to the same level that is found in
remiconductor materials if stability is t o he achieved. Once stable and
purr materials have been obtained, and eiicapsulation methods have been
perfected to maintain this coriditioii, sccoiidary emission may be used for
technical application. h i y system c*lcan cwough to accornmodate field
182 KENNETH R. SHOULDERS

emission cathodes will be suitable for the use of secondary emission effects.
Pure metal secondary emission surfaces have yields up to around two
secondary electrons per primary. The time delay from these surfaces is so
short that it cannot be measured and the current density is limited only
by space charge effects and heating of the material to the evaporation
point. The temperature sensitivity of the effect is negligible and a normal
yield may be obtained from a material even after it is melted [40]. Sec-
ondary emission is a fundamental process similar to field emission in some
respects. One interpretation of the process states that a high local field is
produced in a material by the ejection of a bound electron by a primary
electron and that the high field produced by the emission of the electron
can act t o accelerate a conduction electron sufficiently to escape the surface.
Because this process is extremely rapid-faster than the relaxation time
of electrons in metals-local fields can exist momentarily. Secondary
emission is a lossy process on an energy basis in that the total emitted
electron energy rarely exceeds 1% of the primary energy.
When dielectrics are mixed with metals in various geometries, the
properties of the surface can have many interesting aspects. The Malter
effect [8] and the magnesium oxide self-sustained secondary emission
cathode [9] are examples. I n both of these systems a primary bcam of
electrons striking a complex metal-dielectric surface causes secondary
yields of over 10,000. The cause of this high yield can be traced to field
emission caused by a positive charge on a dielectric particle located near
to the cathode surface. The positive charge is caused by secondary electron
emission from the dielectric. The positive charge is not neutralized rapidly
through dielectric leakage or through electron capture because it is placed
out of the electron path in much the same way as the grid in a vacuum
tunnel effect amplifier. For smaller amounts of dielectric than is needed to
produce the Malter effect the yield of the surface falls and smoothly
approaches the value of pure metal surfaces.
The time constant for secondary emission is very long for the complex
surfaces, going t o infinity for the self-sustained secondary emission cathode.
For the simple geometries used in the Malter effect the time constant is in
the region of a few seconds for gains over 10,000,and falls to the submicro-
second region for yields of about 50. Only a small fraction of the surface is
used for emission, yet t3hecharging current for the eff'ect is spread out over
the entire surface. For optimum geometries employing specific cathode
areas and adjacent grid structures similar to tunnel effect amplifiers and
having specific charging paths, the current gain would be related to the
number of clcrtrons that escaped past the grid before one was caught;
this would be in the vicinity of lo6.The time constant would be related to
the grid-cathode capacity and the size of the charging beam current. It
MICROELECTRONICS 183
i~oul d11c :~rouiicllo-'" src for a oiic-mic~ron-siz(I(1
tlc\.iw :uitl :L I00 pmnp
beam current. This beam aould l w ohtaiiicd from n 11rnr1)yfidcl emissioii
cathode, and controlled by another grid. I11 this light, secondary emission
seems very closely related to field emission. Tcchnologically, both processes
perform best in the prcsencc of high fields, are operated a t similar voltages
-approximately 50 volts-and must 1lai.c clean processing techniques
and ultrahigh vacuum.

B. Light Detectors
For the fast detection of low levcl light pulses the thin film transmission
typc of multiplier phototube shown in Fig. 5 could be employed. The
operation of the electron multiplier is described in Section V,A, on Sec-
ondary Emission Devices. I n this geometry the photocathode is contained
on the optically transparent encapsulating window. For operation a t high
temperatures, stable materials would have to be used; this precludes the
use of normal photocathodes. Metal-dielectric complexes such as molyb-
denum and alumina would be useful again, but they would be suitable
only for the 4000 A blue-light region. Using an electron multiplier having
a gain of 5000, as described earlier, and a two-stage tunncl cffcct tetrode
amplifier having a gain of lo4with a 100 Mc bandwidth, the over-all gain
would be sufficient to detect a light intensity of ft-c falling on a one
micron area and to amplify the signal to the voltage level used for the
switching components.
The principal uses for the light detector arc to allow optical coupling of
up t o lo4 channels between substrates or modules containing lo9 compo-
nents; to provide a method of reading microdocument storage data; to
obtain optical information from outside the machine; and to provide
coupling between internal electronic devices operating a t widely different
voltages. Two different-sized optical detectors would be aeedcd for these
functions. A 0.2-micron-diameter detector would be used for the micro-
documcnt reading, and a one-micron-diameter detector ~rouldIIC used for
thc other operations in order to have drtectors the samr size as active
components. Many one-micron devirrs could be arrayed in parallel when
used as intermodule detertors. Having lo4 paths of information would
require detectors with dimensions not exceeding 0.01 inch; in any practical
case, the detcctors would have dimensions of 0.004 inch by 0.004 inch,
which would require about 100 one-micron-sized detectors operating in
parallel. The lo4 paths of information have been selected as a maximum
because of the necessary substrate thickness of 0.01 inch, which places a n
upper limit on resolution due to light scattering in the absence of a lens.
When data is fed from the outside world into the machine through a lens,
184 K E N N E T H R. SHOULDERS

the iiiput tnoh:iic- c*oultl coiitniii iilioiit, 10* o n e - n ~ i r ~ o i ~ -(Icfwt


s i ~ ~o~r h~ l: L I ~
I\ ould thus requirc t hr best lens availal-ilc.
For the rcading of mirrodacunicnts t hc 0.2-niivron-tlciwt ors will liuvc
t o be followed by 0.2-micron-diamctcr amplifiers, or have the larger
micron-sized amplifiers stacked several layers deep with connecting wires
fanned out, t o each detector. If a single external illumination source is
provided for microdocument rcading, and a scanned output is desired,
then one of the intermediate dynodes of the electron multiplier ran bc
gated to provide the blanking of that particular channel without intro-
ducing spurious signals. By appropriate wiring the microdocument optical
detecting elements can be connected to light generators on a greatly
enlarged viewing screen on the opposite side of the plate and thus provide
the effect of optical magnification. A magnification in the order of 1000
could be achieved and still have lo4 bits in a field. The over-all effect
would be the same as an image-intensifying microscope.
Taft and Apker [41] and Sokolskaya [42] have reported on a type of
optical detector using field emission from a cadmium sulfide tip. The field
can be raised a t the tip until emission occurs even though not illuminated,
but if the field is lowered to a point just below extinction, emission is not
obtained until light is directed onto the tip. The maximum sensitivity is
found in the peak of the characteristic absorption band of the material
used. By the use of photoconducting materials in very high fields the
photoelectric emission threshold is found to be extended to very long
infrared wavelengths. To employ this effect in infrared detecting devices,
the lattice must be kept cool in order to lower the noise figure; however,
this apparently has no effect upon the emission mechanism.
C. Light Generators
Phosphors that havc not been particularly optimized for cfficient opera-
t ion frequently have time constants in the lo-* sec region when stimulated
with electrons. This stimulation can be achieved by emitting from n
mctallic tip dircctly into the phosphor lattice or by first accelerating an
electron and permitting it to cnter the lattice. The mechanism for direct
currcnt elcctroluminescence has been described by Zalm [lo] as being
produced by field emission from irregular edges of phosphor crystals coated
with a slightly conducting layer. Luminescence in aluminum oxide, which
has been observcd during anodization by Van Gee1 [GI, is considered to
be electroluminewence. To verify the possibility of light emission from
aluminum oxide stimulated by field cniit ted elcctrons, the author coated
a tungsten field emission t,ip with evaporated aluminum oxide and emission
current was drawn through the coating. A faint blue light was observed
from the region of the tip. This work was done in an exploratory manner
MICROELECTRONICS 185

and no effort was made to measure the efficiency of the process nor thc
spectral distribution of the light. Elinson [44] has shown the luminescence
of one form of aluminum oxide. Aluminum oxide is being stressed here
because i t represents one class of stable phosphors. Various phosphor
materials, such as zinc sulfide and zinc oxide, have been made by film
methods, but these do not seem stable enough for our requirements.
An alternate method of stimulating a phosphor is to accelerate electrons
from a field emission tip into a phosphor coated with a very thin metallic
layer so as t o prevent surface charge. By using smooth film phosphors and
small areas, a metallic coating much thinner than the usual aluminized
layers can be obtained without an excessive voltage drop in the metallic
layer. Low voltages and high current densities would be desirable so that
compatibility with field emission sources could be achieved. One hundred
volts a t several thousand amperes per square centimeter is expected. The
maximum power loading of the phosphor would be very high because of
the good thermal contact with nearby electrodes.
Large arrays of parallel-operated one-micron-sized light generators
would be needed to present output data and to couple between modulcs.
Approximately 100 elements in an array would bc nceded.
If the light source was scaled down to around 0.2-micron in diametcr
and placed near a light detector, but out of sight of it, then the light source
could be used t o illuminate an individual bit of microdocument data. The
reflectance of the stored data would serve to couple the source and the
detector. Diffraction effects would not be pronounced in this suhmavc-
lcngth range because large aperture anglcs are postulated.
The brightness from microscopic luminescence sources is not known in
detail, but various emissions from silicon junctions, silicon carbide resistors,
anodic films, and ficld emission sources indicate that although the intensity
is escecdingly high the area is also very small, so as t,o limit the total light.
By employing construction processes that produce a large number of active
areas, the total light output could be raised to useful levels.
D. Microdocument Storage
ITsiiig a micromachining process having 250 h rcsolution to record
pcrmanerit data, l 0 l pbits of information could be isolated on a one-square-
inch arca. The material stored on this plate could be read at a later date
by a normal electron microscopy system, but this entails the use of cum-
bersome, expensive equipment. Optical rcading methods using conven-
t ional light microscopy would be ineffective because of the diffraction
limits of light, although dark-field methods would scatter light into the
microscope from particles below the wavelength of light.
I3y using individual light detcctors having cross scctiorial arcas propor-
186 KENNETH R. SHOULDERS

tional to the particle size to be rcsolvcd, thc data printed on the one-square-
inch area could be read provided the data was held in close contact with
the detectors. By reading at a resolution of 2500 A and writing with the
limit of 250 A provided by the micromachining process, 100 levels of light
as seen by the integrating light detector could be discerned, thus yielding
close to 7 X 1Olo bits of data on a one-square-inch plate. It is not expected
that the full range of 100 light levels would be available to a designer
because of fluctuations in illuminating intensity, instability, and non-
uniformity in detectors, effects of variable spacing between surfaces
causing interference effects, and lack of analogue circuitry in microelec-
tronic systems. Ten levels would seem to be the maximum value attainable
in practice, and even this would require special techniques. A maximum
storage density of 3.3 x 1O1O bits/in.2 would result.
The illumination of the entire array could be accomplished by an external
source of light flooding the area or by individual light sources located in
thc same area as the detector. This latter method would give a convenient
way of locally exciting the data and allow simultaneous or sequential access
to the data without having to gate the photo detectors.
Aside from the problems of forming the light generation and detecting
dcvices, which are discussed in Sections V, B and V, C, the largest problcms
in this storage system would be in achieving and maintaining smooth and
clean surfaces with uniform antireflection properties. Standard microscope
slides are smooth enough for our purposes, and they are often flat to within
10 fringes of light. With adequate antireflection coatings on both the
optical detector surface and the micromachined surface containing the
stored information, the difference in spacing will primarily result in adja-
cent channel cross-talk. Without antireflection surfaces a waveguide action
between the surfaces will carry the scattered light to great distances and
increase the cross-talk. It is expected that the light detectors will be within
a few thousand angstrom units of the outside surface of the machine. This
distance is primarily determined by the encapsulation requirements and
antireflection coatings. The recording medium would be a simple metal
film properly covered with encapsulating and antireflection materials. The
minimum spacing between the data and the detector would be about
2500 A; the maximum spacing would be set by the flatness of the recording
plate and would be around 10,000 A in absence of dust specks. The optical
detector surface should be considered to be a delicate surface even if hard
materials like alumina are used for covering layers. There is a relatively
high probability of punching through the thin windows if a dust particle
is pressed or rolled on the surface by the recording medium.
The two methods of using this data storage system would be to mechan-
ically scan the data in front, of a relatively small viewing area of lo6 ele-
MICROELECTRONICS 187
ments in which the data could be t,aken from the storage plate in both
serial and parallel fashion, or to locate the plate in a fixed position and
scan the data out in any series-parallel fashion from an array of 1010
detectors. The latter method would be preferred because there would be
less abrading action to the surfaces and absence of a mechanical scanning
mechanism.
Recording methods using electron-beam-activated micromachining
techniques are presently developed to a degree to permit attainment of
250 A resolution on glass plates or thin transparent films of support mate-
rial. Encapsulation and antireflection coating methods are also developed
to a high degree. The data converters necessary to take printed information
from a book or other source and convert it to a complicated electron image
are not available at present; however, no basic research would be required
to attain this.
Electron optical systems are able to expose complete retinal fields of
iiiformation containing over lo8 bits per field [44a], with a current density
sufficient for activating the electron beam machining process in 1/100 sec.
This 10'O bit/sec data recording rate cannot be matched by present scan-
ning devices. A scanning rate of about lo4pages/sec would be required. If
lo4 pages/sec could be obtained by using microfilm methods to illuminate
a metallic photocathode with a 4000 ft-c light source, then a 10 ma/cmz
electron source would result; this would allow the micromachining process
to proceed a t one-tenth full speed. A preferred method would be to make
the first copy as a metallic image on a thin substrate a t reduced speed and
t.hen use this master in a transmission-type electron optical system, with
further demagnification, to produce copies a t full speed.
Each square-inch plate would require up to lo4 exposures of the lo* bit
fields t o produce the desired 10l2 bits of stored information. Using 0.1
amp/cmZ current density in t,he electron beam, about two minutes would
be required to expose the plate. This two minute recording time is in accord
with the time needed t o mechanically scan the lo4 areas of the recording
plate in front of the electron lens. The details of the exposing time require-
ments and the number of bits per field will be discussed in Sections X and
XI, on Resist Production and Electron Optics.
I n addition to the time for exposing, time for deposition of base metal,
etching, and antireflection coating would be added to the total time. Since
these are batch processes, where many plates can be handled a t one time,
they would not significantly increase the total time by more than a factor
of two; this would give a total time of about four minutes to store 1OI2 bits
of information.
One-square-inch plates have been selected because of their ease of
processing and their ease of manipulation in a dust-free environment,. The
1 aa KENNETH R. SHOULDERS

storage of a large number of these plates would seem economical even if


special containers or casettes had to be provided to keep them free of dust.
Mechanical positioning devices accurate to 0.001 inch can be easily pro-
vided for such rigid plates, and this accuracy can position lo6 individual
fields in front of the viewing area of the microelectronic system. Exact
registration with some desired data cannot be expected with simple me-
chanical means; therefore, electronic data processing methods must be
coupled with mechanical methods to locate the details needed once a field
of data is presented to the machine.
E. Electrostatic Relays
Electrostatic relays employing a one-micron-diameter diaphragm, under
small tension, a few hundred angstrom units thick, would have a funda-
mental resonance above the 10 Mc region. With spacings of lo00 A between
this conductive flexible diaphragm and a fixed plate, a field strength of
3 X lo6 volt/cm could be achieved with 30 volts. At a field strength of
3 X loe volt/cm the maximum stress would be 12,000 lbs/in.* and the
diaphragm would be extended 1800 A. A small area electrical contact and
lcad wire could he carried with the diaphragm and relay action obtained.
More favorable geometries, such as unstretched diaphragms and cantilever
beams, could be used to help lower the operating voltage and to provide
memory action of the relay due to the adhesion forces of the contacts.
Actuator plates on both sides of the diaphragm would be needed to restore
the diaphragm to the alternate contact.
By employing a separate electrically irisulatrd contact on the relay,
normal relay action could be obtained. The contact area of electrostatic
relays of such simple geometry must be smaller than the actuating area or
they must be operated a t lower voltage to prevent the contact voltage
from exerting a strong controlling action on the diaphragm and overriding
the action of the input signal.
Mechanical contacts made in high vacuum and never exposed to air
would be free of the contamination problems found in ordinary relays;
however, theFe contacts would have to be especially prepared to prevent,
sticking. Hard contacts, such as tungsten carbide, or cermets such as
tungsten and alumina may provide contacts with minimum sticking action.
These materials are easy t o handle hy film techniques and would not
increase the fabrication difficulty.
Electrostatic relays would be useful in controlling very low level signals,
in the distribution of power to various electronic devices, and in certain
memory functions that could use mechanical devices as slow as 0.1 psec to
drive a large number of electronic devices. In addition, optical reflection
effects based upon mechanical motion and optical interference would be
MICROELECTRONICS 189
11scfu1f(ir outputJ equipment, in which incident light oil oile surfam of t 110
substrate could h r modified t o produce various colors : t i i ( I iiitcnsitirs i n a
desirrd pnttcrii d l r d for by the clcctrical informatioil i i i t he macahiiir.
F. Electromechanical Filters
If a circular diaphragm of molybdenum has a radius of oiie micron, is
2000 A thick, and is spaced 3000 A from an exciting electrodr, then the
fundamcntal resonant frequency is 670 Mc and the electromechanical
coupling coefficient is 6 X for a ficld strength of lo7 volt/cm. If the
diaphragm is reduced t o 200 A, the resonant frequency is 67 h1c and the
coupling coefficient rises quickly t o O.G, which is considered to be very
strong coupling. I n order to lower the operating frequency of these small
mechanical filters, the fundamental resonance of a reed supported at one
end may be used. For a molybdenum reed two microns long and 200 ,4
thick, the resonant frequency is 4 Mc.
The frequency dependence on temperature, which is caused by a change
in the elastic modulus of the materials used, could be compensated by the
use of bimetal elements for the exciting electrode, provided the coupling
coefficient is high enough to allow the electrical capacity of the circuit to
approach in value the effective capacity of the electromechanical element.
The outstanding mechanical properties of thin fibers and diaphragms
have long been noted. Part of this strength comes from the lack of crystal-
lographic slip that is found in bulk materials. This characteristic would
seem to impart stability to devices made from thin films. If metallic creep
in molybdenum films became evident, then part of the metal in each ele-
mcnt could be replaced by aluminum oxide, which has similar elastic
properties but greater hardness. Just enough metal is iieedcd to make a11
electrically conductive vibrating member.
These electrostatically driven electromechanical eleinent s appear to
provide very convenient accessory components for vacuum tunnel effect
devices, since they could be made from the same materials by the same
processes and operate a t the same voltage and field strengths. A simple
connection from the anode of a tunriel effect component to thc driving or
exciting element of the filtcr is adequate to introduce the signal, although
this requires a load resistor of several megohms to operate in the hundred
megacycle region. Direct electron beam excitation can be used without
load resistors if secondary emission is employed. An electron beam that is
deflected across an alternately low and high secondary electron emission
area of the filter element or thc driving element can cause the voltage on
the electrode t o assume any value between the full anode voltage and the
cathode. Experimental observations in the electron microscope have shown
a similar effect. When a material like silica or alumina is produced in film
190 KENNETH R. SHOULDERS

form 011 a screen wirc, and intcntionally brokcn by mcchanical means, the
breaks usually produce cantilever beam siaucturcs that protrudc out) hit o
thc scrccn opcnirig and arc attached to the scrccii cdgc. Whcn this sample
is observed in the electron microscopc under nonuniform illumination
conditions, the image of the scrcen is seen t o be vibrating and the ampli-
tude can be controlled by the illumination shape and intensity. This forced
oscillation is evidently caused by some method of alternately charging
and discharging the film by secondary electron emission. TWOtypes of
oscillation are evident in the microscope image: one is a relaxation effect
which seems to produce square waves, since two distinct images are
observed; the other is essentially sinusoidal and is assumed to be an
oscillation a t the resonant frequency of the cantilever beam. An electron
multiplier could be inserted in front of the phosphor screen of the electron
microscope and the output fed to an oscilloscope to determine the wave-
form and frequency of the oscillation.
The point projection electron microscope and micromanipulator used
on the program for “Research on Microminiature Field Emission Tubes”
[15a] is ideally suited for obtaining data on micron-sized electrically oper-
atcd mechanical filters. Data has recently been obtained on the low frc-
quency resonances (audio spectrum) of the various members by exciting
the system with alternating current instead of direct current. Had rf been
introduced, and the projected image of a mechanically resonant structure
been displayed on the fluorescent screen, the bandwidth and other features
of the structure could have been investigated.
It is assumed that fabrication methods for large arrays of electromechan-
ical components would alternately test and correct the structures until the
assigned frequencies are obtained. The test could be implemented by
direct excitation from the tunnel effect components or from the electron
microscope feature of the micromachining process.

VI. Component Interconnection

A. Vacuum Tunnel Effect Amplifiers


A tunnel effect amplifier may be considered as a normal vacuum tube
having a positive grid that draws low current. This positive grid allows the
direct connection of anode and grids, thus dispensing with various coupling
networks and transformers. When direct coupling of triodes is used, and
the control grid is driven more positive than the anode, grid current results.
Tetrodes would not have an appreciable control grid current under the
same conditions, but the screen grid would draw current unless used as a
low voltage suppressor grid. I n spite of direct coupling features most of
MICROELECTRONICS 191

the circuitry in this microelectronics system should be arranged for opera-


tion on a pulse basis in order to prevent excessive energy dissipation and
heating. Stable load resistors are difficult to fabricate in this size range
because the high resistivity materials needed have poor temperature
coefficients of resistivity. Dynamic resistors in the form of vacuum tunnel
effect triodes connected as diodes could serve as load resistors. Their tem-
perature characteristics would bc very low and mat,ched to those of the
active elements. It is believed that by the use of self-forming processes it
would be possible to tailor the diode characteristics of triodes t o fit the
active element characteristics. The steep voltage-current characteristics
of the tunnel diode would make a very nonlinear resistor, but this would
not seem to be excessively troublesome in switching circuits.
For driving a transmission line or setting the voltage on a storage capac-
itor the series tuhe arrangement shown in Fig. 7 could be used. A pulse

K==?l- ANODE

CATHODE

FIG.7. Series connected tunnel effect vacuum triodes.

into the upper tube grid would cause conduction and the output point
between the two tubes would be driven to anode potential. Conduction of
the lower tube sets the output value to cathode potential. The time con-
stant for both of these operations depends upon the conduction current
and the external capacity, and would be in the neighborhood of 10-lo sec
for normal operation.
With the series tube connection shown in Fig. 7, the top tube is acting
as a cathode follower and voltage degeneration results when the input
signal is derived relative to ground potential. To provide gain in this stage
without the use of iiiverting amplifiers and load resistors, the secondary
emission amplifier circuit shown in Fig. 6 would be employed. When elec-
trons are emitted from the cathode by either raising the grid voltage or
lowering the cathode voltage they are accelerated t o the dynode; this
rauses more electrons to be emitted than are received and the dynode is
clamped t o the anode potential. There is no mechanism shown in Fig. G
for discharging the grid. Figure 8 shows a method of discharging the grid
192 KENNETH R. SHOULDERS

ANODE

DYNODE

GRID

INPUT

CATWODE

SECONDARY EMISSION
AKPLIFIER
i SERIES CONNECTED
TRIOOES
I NEGA-WE RESISTANCE
MEMORY

FIG.8. Assembly of multilayer tunnel effect coinpoiirnts to give an active memory


with low quiesccnt power consumption.

when the lower series triode conducts. Part of the electrons from the lower
cathode are bypassed to the grid through the anode of the lower tube,
thus discharging the grid when needed, namely, upon conduction of the
lower tube. Figure 9 shows a single metal layer type of component used
for the same function as Fig. 8. Skellett [37] and Bruining [45] describe
various methods of employing secondary electron emission to obtain cir-
cuit functions normally difficult t o achieve without the use of secondary
emission. It is expected that the current density of the secondary emission
process is similar to the currcnt density of the primary electron beam, thus
yielding switching time constants in the same region as a vacuum tunnel
effect device. Space charge effects can be neglected when high field intensi-
ties are used.
A relatively low-noise negative grid, Class A amplifier could be formed
from the various basic elements of the vacuum tunnel effect device by
providing a space charge smoothed emission source that is followed by a
normal negative grid triode. The emission source for the triode would be
provided by a field emission cathode and anode. The anode would have a

'/////I/
CATHODE CATHODE

/ / / / / / / /, /-
/
lop we*

F ~ G9.. Assembly of sinylc-luJrr tuiiiiel effect coitipoiiciits to give uii active memory
with low quiescent power consuniption.
MICROELECTRONICS 193
Iiolc in it similar t o Q positive control grid, and some of the emitted elec-
trons would pass through the hole into the retarding field region of the
negative grid triode that followed. The space charge smoothing that re-
sulted in the retarding and drift region would smooth the current fluctua-
tions and reduce the effective noise temperature of the emission source
below the temperature of the emitter. If a room temperature emitter were
used, a useful noise improrrmrnt ovcr conventional negative grid therm-
ionic tubcs could result.
B. Memory Devices
It seems practical t o achieve memory effects by employing vacuum tun-
nel effect devires to compensate for the leakage current of storage capaci-
tors. The distributed capacity of active elements can be employed as
memories provided the active elements have a negative resist3ancecom-

ANODE
I
I
.’ DYNODE 8 MEMORY
! ELECTRODE

---; CATHODE

FIG.10. Negative resistance memory device composed of tunnel effect vacuum triode
constant current generator and sccondary emission dynode.

parable to the positive leakage resistance of the dielectric. The dynatron


action of secondary emission devices can be used for a memory, as can a
flip-flop action that operates a t current values equivalent to dielectric
lrakage.
The dynatron or negative resistance type of memory device is shown in
Fig. 10. This is essentially a tetrode with a secondary emitting screen grid.
The cathode is required t o emit a very low electron current somewhat
greater than the leakage currents of the memory electrode or screen grid.
This low current is provided by the control grid being connected to a supply
voltage through a resistance formed by the dielectric leakage resistance.
When the control grid voltage tries to rise the increased emission current is
partly intercepted by the grid and any further rise is degenerated. The
screen grid is clamped to either anode or cathode potential, depending upon
where it has been previously set, by the negative resistance or dynatron
action of sccondary emission. The power consumed for this holding action
194 KENNETH R. SHOULDERS

would be roughly 10 timcs the leakage dissipation of thc dielectric; this


would make a large array of such memory devices possible without exccs-
sive power consumption. The array would resemble a capacitor of equiv-
alent area and thickness. If power were removed for a short time-up to
several hours at room temperature-there would be no loss of stored data.
Upon heating the entire array of devices the leakage current would increase
as well as the conduction current from the active devices; however, they

I CROSS-OVER I I
ANODE I

ANODE

GRID GRID

CATHODE
OUTPUT
ANODE I ANODE

GRID I GRID 2

CATHaoE

'
Sidm wiw
SERIES CONNECTED TRIODES TRIODE-DIOOE

FIG.11. Flip-flop memory device composed of croes-connected tunnel effect variium


triodes using active anode load resistors.

would increase a t approximately the same rate and prevent loss of stored
data. Figures 8 and 9 show a series tube setting circuit, negative resistance
memory, and secondary emission amplifier combination.
A flip-flop type of memory could be employed in the same fashion as the
negative resistance memory but would not require secondary emission.
Figure 11 shows an arrangement in which a series tubc ronnection is sup-
plemented with a diode-triode connection to obtain low-power flip-flop
action. During the set,ting of thc memory the series tubes forcefully dis-
MICROELECTRONICS 195

rhargc t hc st oiqq. capacity in approximately 10-lo sec. Following this


wtting c~yclethe currents fall t o very low values and the effective plate
h a d resistances are in the region of one-tenth of the dielectric resistance
values. Vacuum tunnel cffcct devices would be very good for this type of
operation because of their cxtremcly wide range of current swing for a small
voltage change on the grid. During the holding part of the memory cycle,
the upper diode and triode of Fig. 11 act as load resistors. The lower triodes
have their grid and plate leads cross-coupled in typical flip-flop fashion and
regenerate any charge loss on thc rncmory capacitor.
It would be possible t o have a syinmetrical flip-flop in which the diode
was substituted for a triode, and eomplcmcntary inputs as well as outputs
were provided. The flip-flop circuit can be connected to output amplifiers
of the series tube type when isolation is desired. This type of memory cir-
cuit can supply virtually no energy to extcrnal circuits and would normally
be followed by low 1.1 amplifiers that remain quiescent until power is drawn
from them by thc external load.

C. Electromechanical Components
Electrornechariical components are designed to operate at the full anode
potential of vacuum tunnel effect devices and may be coupled directly to
them. When low level signals are to be processed, the various stages must
be isolated by coupling capacitors in the usual manner to prevent drift of
dc characteristics from saturating the amplifiers. Most filtering require-
ments could be satisfied by using many active elements and electro-
mechanical components in series-parallcl cornhination.
D. Steerable Electron Guide
A pcriodically focused elcctrostatic electron guide seeins compatible with
this microelectronic system. Such a guide would be used to replace some of
the fixed wiring in the system so as to give greater system flexibility. This
electron guide system has the potentiality of greatly decreasing the power
required to perform a particular computation by using combinational logic;
in this case the beam must thread its way through a complex maze of logic
states before giving up its energy to an electrode. Such a n electron guide
system can also cross beams in the same plane without interference, thus
reducing the wiring problem in a single plane. Ultimately, certain beam-
beam interactions seem suitable for the processing of information without
having to charge and discharge the energy storage structures in a data
processing machine. This is because a superconducting-like action is avail-
able through persistent current loops that can be set up and controlled by
other beams.
An interesting form of periodically focused electrostatic guide has been
196 KENNETH R. SHOULDERS

used by Cook et al. [46] to form high pcrveance beams for traveling wave
tubes. The analysis of the stability criterion of such a “slalom” bcam has
been given by Cook [47]. His data indicates that a beam guide structure
having a spatial period of several microns and operated a t 100 volts could
easily contain a beam with a currciit density of lo4amp/cm3, which is ade-
quate for 10-lo sec switching time operation. The velocity of this beam is
a little greater than one hundrcdth the velocity of light; thus propagation
across a one-inch system would occur in about 5 X sec.
The form of guide most suited to our purposes would consist of a uniform
array of positive electrodes contained between planes of conductors operat-
ing a t cathode potential. An clcctron bcam would be injected into the struc-
ture with a ccrtain range of angles and velocitics so as to obtain a stable
orbit or path through the array. Thc injection would be done with field
emission sources followed by a simple grid structure to rcducc the emission
angle to a useful value. These launching structures would be located
throughout the array a t intervals of a few microns, in the same fashion as
the positive electrodes. I n order to guide the bcam, it is necessary to altcr
the potential on thc positive electrodes with t,he voltagc swinging betwccn
anode potential and cathode potcntial, Beams having the same velocity but
launched a t different angles follow diffcrcnt paths and may be effected in
various ways by the stcering clectrodc. Bcams launched at a high angle
relative to the direction of travel are most easily turiicd by the steering
electrode; beams launched a t low angles and crossing very ncar to the
positive electrodes are difficult to turn.
Collection of the electrons must be accomplished by inserting an elec-
trode in the electron path or by disturbing the elcctron path in the vicinity
of the collection point so as to allow collection by the positive guide elec-
trode. The collection points would have to be as numerous as the launching
positions. In addition, it would seem reasonable to include several other
functions, such as memory for the steering functions, and memory and
gating elements for the logic functions. This cntire group of components
would form a low complexity module that has internal communication via
wires and distant communication via electron guides. The entire array of
modules would operate a t a single potential of around 100 volts, even
though the electron velocity periodically falls to lower values when turning.
By using free electron beams isolated from the lattice and having a
suitable interaction space, very low noise amplifiers similar to the para-
metric amplifiers of Crumly [48]and Udelson [48a] could be obtained, in
spite of high lattice temperature. This electron beam parametric amplifier
would have a decided advantage over solid state types employing tuned
circuits because of the low Q of microminiature tuned circuits.
The construction of free electron guides would primarily involve provid-
MICROELECTRONICS 197
iiigIdlow structures between plane clectrodes supportcd pcriodically by
mctallic elcctrodcs. Thc construction process worild thus omit wircs and
provide vacuum cavities in thcir stcad.
The understanding of the principle of opcration or the application of
steerable electron guides is far from complete; they are mentioned here
only to show some of the potciitialitics of free electron systems.

E. Plasma System
I t is the author’s opinion that all organization of the sort that is interest-
ing to data processing does not usefully ccase at a temperature equivalent
to the melting point of matter. Conceptually, it may be feasible to consider
a gaseous-like array of very small particles, such as ions, organized in quasi-
static structures, through which slalom-focused electron beams thread their
way. Some of these beams could scrvc as casily alterable system intercon-
nections. Othcrs, circulating in persistent current loops, would serve as
memory elements; control of these bcams and cnergy transfer would be
accomplishcd by bcam-beam interaction.
Some preliminary steps [49] have bccn takcn by showing the possibility
of confining charged particles in quasistatic positions in an enclosed space
by varying electric fields imposed esternally. This clcctrodynamic suspen-
sion system could provide the means for the organized structure consisting
of charged particles so disposed in space as to guide the slalom electron
beams carrying information.
One of the most interesting features of a plasma-like machine is the
triviality of the microminiaturization problem. Due to the extremely elastic
behavior of the entire system, the organization could be accomplished at
convenient sizes and then scaled down by a change in some parameter such
as the confinement field frequency. This type of machine would show a high
degree of three dimensional communicating ability-very much unlike our
present layered structures. The extreme plasticity of the machine’s struc-
ture would assist the organization of data for optimum machine usage.
All useful electronic effects would be available to such an electronic
organism. It appears possible to generate and receive information from
the acoustical end of the spectrum up into the X-ray spectrum, and to
process information a t rates that would seem phenomenal by present
standards.

VII. Substrate Preparation

The deposition of film-type microelectronic components requires a rigid


supporting structure that is capable of bcing processed at high tempera-
198 KENNETH R. SHOULDERS

turcs and aMc to have ruggedly bonded lead wircs attachccl to it. Wc have
clectrd t,o use rcfractory transparent dielectric substrates such as sapphire.
These substrate plates are approximatlcy 1inch square and 0.01 inch thick.
The present cost of one-inch Eapphirc windows, which represent a good
starting point for our substrates, is ten dollars, when bought in small
quantities. The cost of preparing the substrate for final use could make
the raw material cost quite tolerable.
A high thermal conductivity, rigid refractory material such as beryllia
would be more suitable to our application, but as yet there is no trans-
parent material available a t reasonable cost.
A. Mechanical Forming
The ovcr-all dimensions such as thickness, parallelism, squareness, and
flatness can be obtained by ordinary commercial grinding techniques to
dimensional tolerances substantially better than 0.001 inch. The maximum
convenient size for a substmtc of 0.010 inch thickness is about 1 square
inch.
The most difficult operation is the mechanical polishing of surfaces to
the degree required for microelectronic components. A surface smoothness
approaching the 300 A resolution of the construction process would bc
desirable; however, it is difficult to obtain over the entire area of the sub-
strate. Glass surfaces that have not been weathered have an average
smoothness greater than 100 A but these surfaces are usually produced
by fire polishing. Fire polishing has the undesirable property of fusing
various dust particles into the surface where they become rough spots and
chemical anomalies that can later damage the film components. Mechan-
ical polishing of glasses frequently produces sleeks, pick-out cusps, and a
host of mechanical difficulties that are a result of melting the surface by
friction from the polishing medium. Ehrenberg [50] and Koehler [51] dis-
cuss some of these problems in relation to producing ultrasmooth sur-
faces for X-ray reflection.
Polishing of hard, high-temperature materials like sapphire usually pro-
duces errors in the form of minute fractures in the surface instead of the
melting effects seen in glass. Sapphire can be polished by commercial tech-
niques so that it shows few flaws greater than 1000 A in depth, although
some of the scratches produced extend for quite some distance. It does not
seem worthwhile to attempt t o remove all of the mechanical irregularities
down to a smoothness of 300 A by mechanical polishing alone; however,
this process is a great asset in producing surfaces flat to less than one fringe
of light and with a consistent smoothness of around 1000 A, having very
few anomalies protruding above the surface. As will be shown later, the
MICROELECTRONICS 199
pits are less troublesome than the spikes when attempting to further smooth
the surface.
B. Substrate Cleaning
There are two slightly related problems in substrate cleaning, namely, to
remove the specks of dust and debris that adhere to the surface and to re-
move the material that is contained in the substrate just below the surface
and distributed throughout it as gas. If these problems are not handled
separately, then, surface specks can be driven into the bulk by heating and
greatly complicate their removal. The aim is to remove most of the dust
particles, then heat the substrate to very high temperatures in vacuum to
drive out the remaining material that can be removed at the firing tem-
pera ture .
A high-vacuum cleaning method, which seems adequate for removing
surface dust and other anomalies that have not been fused into the surface,
has been previously investigated by the author. This method was developed
after it was found that, even if a surface could be cleaned by very laborious
techniques in air, the surface usually became dirty again during the pump-
down of the vacuum system. A vacuum system used in everyday service
is far from the clean environment visualized because there are many tiny
metallic and dielectric particles as a result of previous depositions; these
particles are moved around in the system under the influence of convection
and electrical forces, some depositing on the substrate. These particles can
be stabilized by welding them to the chamber. This is done by baking the
vacuum system at high tempernturcs, while operating all of the high volt,-
age electrical circuits, and depositing several thousand angstroms of mate-
rial on the walls of the vacuum chamber.
To remove foreign material from the surface down to a particle size of
300 A, a method employing explosive reevaporation from the surface has
been tested and found satisfactory. This method consists of evaporating a
highly volatile and decomposable material like ammonium chloride onto
the surface t o a thickness of several thousand angstrom units. This mate-
rial is pulse-heated by an electron flood bcam of about 100 amp/cm2 at
20 kv between a tungsten filament and an anode ring of tungsten that is
located near the substrate. After this treatment it has been found that the
surface is free of foreign material that has not been fused into the surface
by prior heating or polishing. An explanation that can be offered for the
cleaning action is that the explosive vaporization of ammonium chloride
carries off adhering particles by mechanical action after having discharged
material adhering by Coulomb forces. The electron beam ionizes a great
many of the gas molecules at the surface to assist in neutralizing charged
200 KENNETH R. SHOULDERS
debris long enough to be removed from the surface. The ions formed do
not have sufllcient energy to sputter the surface to any measurable extent
if a short current pulse is used because they are formed in the low voltage
region close to the surface.
After removing adhering particles from the surface, the substrate can be
heated to around 1700°C in vacuum to remove many of the absorbed and
adsorbed gases produced during the mechanical polishing of the surface.

Fro. 12. High-vacuum electron-bonibiLrdmerit-heatrd furnace.

The effectiveness of heating as a method of cleaning is discussed by


Hagstrum [52].
A vacuum furnace suitable for this heating, as well as for ceramic firing
and metallizing, is shown in Fig. 12. The entire assembly is installed in a
vacuum bell jar and pumped down t o the mm Hg region. The material
t o be fired can be loaded into the molybdenum box shown in the center of
the water-cooled housing, and a small molybdenum door is fitted onto the
box to prevent direct electron bombardment of the material being fired.
MICROELECTRONICS 201
The anode box of molybdenum is heated by electron bombardment from
the filament that is coiled around the box and suspended from the water
cooled housing. A temperature of 2000°C can be attained by using an accel-
erating voltage of 5 kv a t 0.5 amp. The temperature is monitored by a
tungsten-molybdenum thermocouple inserted in the anode. To prevent in-
sulating the thermocouple meter the anode is operated at ground potential
and the water-cooled housing and the filament are operated at high nega-
tive voltage. To do this the water-cooling lines must be insulated by 10 feet
of plastic tubing; the filament current is supplied by a 10 amp isolation
transformer with a 115 volt output. This furnace can be put on automatic
regulation by using the standard emission regulators described in Section
VIII, A and using the thermocouple output to feed a Philbrick USA-3
amplifier.
After this heat treatment the surface is no longer smooth; it shows signs
of thermal etching, has peculiar extrusions of material from inside the sub-
strate, and has many unexplained steps and ridges. A subsequent mechan-
ical polishing that is carried out with extremely fine diamond powder and
water, using another sapphire plate as a lap, will remove most of the large
anomalies. This process should be carried out with extreme care and only
the minimum of material removed.
When this substrate is once again clcancd by the above process in high
vacuum and heatcd to around 1600°C the surface will be found to be
smoothcr than 800 A, with only an occasional particle sticking out of the
surface and a very few fractures deeper than 1000 A. It is an extremely
tedious job to check by microscopy a surfacc that has any appreciable area,
although methods will be describcd lntcr for doing so.
C. Substrate Smoothing
A substrate smoothing method, which involves drawing a taut film across
the substrate surface, and sintcring it onto the surface by heating, has been
previously investigated by the author. This process, which is essentially
the same one used to form vacuum cavities, was discussed in Section IV, G
on tunnel effcct components. The process essentially amounts to depositing
a material that can be easily liquified, such as myristic acid; rapidly heat-
ing a i d coolirig the material to produce a smooth surface; and evaporating
a thin layer of material over the myristic acid t o provide a refractory sur-
face to receive a heavier deposit later. The myristic acid is then driven out
and the thin film is sintered to the subtrate. When completed, a heavy film
is deposited over the thin film to provide mechanical strength. The entire
process produces a surface that is smoother than 300 A; this smoothness is
controlled by the crystallization of the smoothing material and the heavy
film covering it.
202 KENNETH R. SHOULDERS

If this process were optimized, the advantages of a smooth fire-polished


glassy surface could be retained along with the advantages of stability and
cleanliness of refractory materials such as sapphire. There has been no
work done on determining the limits of smoothness attainable by vacuum-
fire-polishing sapphire or similar crystalline materials with an intense
electron beam; however, there is some evidence, from results on flame-
polished samples in air, that smoothness could be obtained. The difficulty
that might be expected would be the production of thermal etch pits and
ridges.
Even though a fire polishing process may be developed for the substrate
proper, it will not serve to smooth between layers of components because
of the damage to the components. If low temperature materials are used
and retained between layers to allow fire polishing, the stability of the en-
tire system would suffer and high bake-out temperatures for cleaning and
outgassing could not be reached.
D. Terminals
Sapphire is a very good material to use for a substrate because stable,
rugged terminals can be attached to it. Molybdenum metallizing can be
applied to sapphire and then coated with nickel or gold-nickel alloy for
the attachment of nickel connecting wires or other, more corrosion-
resistant alloys. Sapphire has very high strength and an expansion co-
efficient near that of the metallized molybdenum coating.
Satisfactory terminals have been produced in the past on sapphire by
notching the edge of the substrate with a slot 0.02 inch wide and deep;
coating this with a mixture of 90% -325 mesh molybdenum powder and
10% zirconium oxide; and firing at 1850°C in a vacuum furnace. This oper-
ation is carried out before the substrate goes into the final grinding opera-
tion, so that the terminals are ground flat along with the substrate. When
all processing of components is completed on the substrate, nickel or gold-
nickel alloy can be used to vacuum-braze the connecting wires onto the
terminals at temperatures between 970°C to 1500"C, depending upon the
brazing material selected. In addition to the connecting wire termination,
the thin film wires of the components must be terminated with a heavy
vacuum-deposited film of molybdenum that acts as a buffer between the
fired-on molybdenum terminal and the thin film. If this is not done there
is an occasional open-circuit produced at the junction after high tempera-
ture cycling, probably as a result of some corrosion process and ineffective-
ness of encapsulation at the junction of the heavy molybdenum alloy
terminal and the thin a m .
Terminals produced by these methods were used in the encapsulation
tests described in Section VIII, C, where repeated cycles between low
MICROELECTRONICS 203
1 cmpcratures and temperatures around 800°C mere made in very corrosive
onvironments. The terminal scrmrtl to he the most inadequate link in the
process and failure was causcd hy sonic corrosion mechanism working its
way under the encapsulation in the region of the molybdenum terminal.
By siliconizing the termiiial and lead wire, a protective covering over the
entire assembly could be obtained. Molybdenum wires treated in tetraethyl
orthosilicate vapor a t around 800°C can be operated for extended periods
above 1200°C in air without dificulty [53]. The protective layer is appar-
ently a thin coating of quartz, bonded to the molybdenum through a
molybdenum disilicide phase.
E. Substrate Testing Methods
Two classes of checking methods seem in order: one, to help the investi-
gator converge upon a solution to surface-smoothing and speck removal;
the other, to simply test the surface before proceeding to the next layer of
components. Electron microscopy can serve for the first method, and the
deposition of a very thin film capacitor can serve for the second.
If a surface is cleaned properly and coated with a release agent, such as
carbon, by vacuum evaporation, then coated at ail acute angle with a
shadowing material like chromium, which is subsequently stripped from
the surface for examination in an electron microscope [54], variations in
the surface characteristics smaller than 50 A can be determined. The shape
of the offending anomalies can help determine the source of trouble, and
occasionally a particle is picked up by thc replica techniquc and electron
diffraction can help determine its origin. Replica techniques are useful
when commercial tranPmissioii microscopes must be used and direct sur-
face examination cannot be employed. Later, we will incorporate a scan-
ning probe electron microscope in our equipment and be able to examine
surfaces directly; however, this is a very tedious process when large areas
must be examined. An automatic process could probably be developed,
but as yet nothing has been done toward achieving this goal. The testing
method would involve searching for any light or dark area that appeared
while the surface is scanned electronically and moved mechanically.
One test method that has been used in the past to determine the smooth-
ness of large areas is the deposition of a capacitor having a thin dielectric.
I n this test, alternate layers of molybdenum and aluminum oxide are de-
posited to a thickness of around 100 A by rcactive deposition methods, as
described in Section VIII, C on material deposition. The most sensible test
for a surface is whether or not it is smooth enough to build microelectronic
devices, and the thin film capacitor represents a useful test. Capacitors
having about 100 A dielectric thickness and one square inch area have
been produced by careful technique. This test method incidentally revealed
2Q4 KENNETH R. SHOULDERS

that evaporators frequently spatter out particles a few hundred angstrom


units diameter which puncture dielectrics and roughen the surface ; there-
fore, reactive deposition processes were substituted.
These capacitors, which are discussed in more detail in Section VIII, C,
have shown up to 1000 mfd/in?, as judged by time constant measurements.
A high series resistor was used to watch for the onset of tunnel emission,
which must not become excessive.

VIII. Material Deposition

Two deposition methods are used in this microelectronic construction


process-thermal evaporation and reactive deposition. Both methods are
carried out in a high vacuum system, and both need very similar equip-
ments to perform deposition. Both require heaters for the source materials,
monitors for determining evaporation rates, and substrate heaters. Thermal
evaporation methods use a source that is much hotter than the substrate,
whereas reactive deposition usually USCS two sources that are cooler than
the substrate, as well as a substrate that is hot enough to rcact the two
materials or decompose them. As examples, molybdenum can be evaporated
by having a source at approximately 2600°C and a substrate surface at
400°C; reactive deposition uses a molybdenum chloride source operating
near 400",a hydrogen source at room temperature, and a substrate tem-
perature as low as 900°C or as high as 1500°C. The reason for preferring
reactive deposition is that by using a very hot substrate, clean, properly
crystallized, and stable materials result. The substrate temperature can be
much higher for reactive deposition than thermal evaporation because the
reaction by-product evaporates from the surface, taking any excess energy
with it. This permits the deposition of the desired material without re-
evaporation experienced in thermal evaporation deposition. Deposition of
compounds such as oxides, nitrides, carbides, borides, sulfides, and silicides
can be done by reactive deposition without decomposition [55], whereas
the deposition of many compounds is difficult or impossible with the ther-
mal evaporation process. A very great advantage is obtained with reactive
deposition in that pinhole free and dense deposits are usually obtained.
This is because there is a high degree of surface mobility that prevents
shadowing of any rough spots on the surface; there thus results a complete
dielectric covering of surfaces and a strain-free crystalline structure that
is not prone to break out tiny pieces, an effect frequently found in evapo-
rated deposits. The high substrate temperature also immediately volatilizes
any spattered pieces from the evaporator that arrive at the substrate. These
MICROELECTRONICS 205
picccs wonld norinally constitute specks on thc surfare of rv:tporatrd dn-
posits and cause pinholes.
Thermal evaporation methods will not bc uscd for cnd-product maherials
in the final component phase of this work, but only for temporary deposits
where the substrate must be kept cold, such as in the smoothing operation
between layers; for the production of resists; and for the first film of the
vacuum encapsulation process. Due to their simplicity, they will also be
used in interim studies, where the finest films are not required.
A. Thermal Evaporation
Two types of material sources are used in this project. Low temperature,
nonreactive materials are handled by radiation-heating crucibles, contain-
ing the various materials, with resistance wire heaters. The heater wires are
usually molybdenum or tungsten. High temperature and reactive materials
are heated by direct clectron bombardment. For large samples and high
evaporation rates, a water-cooled hearth is used and the evaporating mate-
rial is bombarded with high energy electrons. Metals and dielectrics can be
handled by this method provided the electron velocity is greater than the
one-to-one point on the secondary electron emission characteristic, thus
causing the dielectrics to charge positively. Small samples can be either
directly bombarded and serve as their own support, or they can be con-
tained in refractory metal baskets or ceramic crucibles. Bombarding of
tungsten or molybdenum baskets is preferred to resistance heating because
there is no burnout caused by alloying and thinning of the heater wire; in
addition, there is no shorting problem between turns.
Figure 13 shows a small multiple source evaporator for simple experi-
ments; Fig. 14 is a drawing of the same evaporator. A mechanical manipu-
lator moves the various sources and their shields under an electron-emitting
filament. A switch makes contact with the appropriate anode and high
positive voltage is supplied. The voltage ranges from 200 volts for mate-
rials like aluminum chloride, having a high vapor pressure, to 3000 volts '

for a material like tungsten. The emission source is a .010-inch-diameter


tungsten filament, which normally runs at about 7 amps, to obtain emission
currents of about 100 ma, the highest value used for this small evaporator.
An auxiliary electrode, called the ion collector, is placed above the filament
and operated at 30 volts negative with respect to the ground and filament.
This ion collector collects a fraction of the ions present, as a result of the
bombardment of the evaporating material, and serves to indicate the evap-
oration rate. The ion current is amplified and fed into the emission con-
troller, as shown in Fig. 15, to cause automatic regulation of the evapora-
tion rate. The desired evaporation rate is selected on the range switch and
206 KENNETH R. SHOULDERS

FIQ.13. Apparatus used for electron-beam-activated micromachining showing vac-


uum station, adapter spool, multiple-source electron beam heated evaporator, flood
electron gun, shutter and substrate heater.

SUBSTRATE HEATER

I tNIPULATOR
RES

FIG.14. Drawing of apparatus used for electron-beam-activated micromachining


shown in Fig. 13.
* R-IWA
T
-300 -
POWER SUPPLY

-
-
-L

10 MEG TOTAL- LOG TAPER


EUPORATWN RATE SWITCH

I ION COLLECTOR

I
I
51
El
7 I

FIG.15. Schematic diagram of evaporat,ion rat,e regulat,or used on multiple-source electron-beam-heated evaporator shown in
Fig. 14.
208 KENNETH R. SHOULDERS

can be repeated to about 30% of previous values. The variations come from
changes in geometry and changes in the gauge sensitivity as a result of
change in the bombarding current.
For the evaporation of larger quantities of refractory material, the dual
electron bombardment evaporator, shown in Figs. 16 and 17, is used. This
evaporator uses a water-cooled anode operated at voltages between 1000

Fro. 16. Dual source, electron-beam-heated evaporator for 1/2-inch diameter samples
of refractory and reactive materials employing a water-cooled hearth for material
support-shown with upper shield removed.

and 7500 volts. The emission current is supplied by a 0.012-inch-diameter


tungsten filament that can supply a maximum of 0.5 amp emission a t ap-
proximately 10 amp heater current. For low voltage operation, a 0.01-
inch-diameter tungsten grid wire structure having the same diameter as
the filament structure-about 0.80 inch-is used to assist emission. This
grid is held between 200 to 300 volts positive and serves to control the
electron emission. An ion collector wire located above the top shield is run
MICROELECTRONICS 209
at 30 volts negative and used to indicate the evaporation rate. The regu-
lators can be connected between the ion collector and the control grid to
regulate the evaporation rate. For evaporation of 0.50-inch-diameter Sam-
ples, the input power is about 200 watts for nickel-iron alloys, 600 watts
for molybdenum and aluminum oxide, and 1200 watts for tungsten and
tantalum.
The maximum evaporation rate is limited by the onset of a glow dis-
charge caused by the presence of the high pressure molecular beam.
For a 0.5-inch-diameter source the maximum deposition rate is about
2000 A/min at a distance of 10 in. During normal operation of this evapo-
rator the melted and evaporating materials do not stick to the cooled anode,
although occasionally materials like aluminum and silver do stick; an in-
creased power input is then needed to continue evaporation because of
greater heat transfer to the anode.
A shield system is provided t o prevent large quantities of evaporating

EVAPORATING MATERIAL 7

FILAMENT k; /[, r F l L A M E N T INSULATOR

UPPER SHIELD

ANODE
I 4.; ; I J, LOWER SHIELD
INSULATOR

\-ANODE tlUM

Pic. 17. Drawing of water-coolctl elect ron-beam-heated evaporator shown in Fig. 16.

materials from adhering to the filament and changing its operating char-
acteristics. Another shield between the filament and the substrate prevents
most filament materials from reaching the substrate either from thermal
evaporation or from reaction products like tungsten oxide, which is formed
when aluminum oxide partly decomposes upon evaporation. The shield is
not completely effective; occasionally, filament material reaches the high
pressure evaporation zone and is scattered to the substrate.
Another source of impurities is the sputtering of atoms from the con-
struction materials near cathode potential, but this effect diminishes as a
thin film of evaporating material is built up on the structures, allowing
sputtering of only the desired material.
Low temperature materials, particularly those used in reactive deposi-
tion and molccular beam etching, are evaporated from sources similar to
the one shown in Fig. 18. A crucible of glass, alumina, or metal is centered
in one of the heater coils shown and heated by radiation. The maximum
temperature that can be reached conveniently by this method is about
210 KENNETH R. SHOULDERS

FIG.18. Dual evaporators and ion gauge rvitporation rate monitors for low tempera-
ture materials.

9oO°C, but this is adequate for any materials used in reactive deposition
or molecular beam etching.
The evaporation rate from this sourcc is monitored by a simple ion gauge
located in a position to see only one of the sources. The ion gauge cross
scction is shown in Fig. 19. This gauge is operated at 300 volts anode volt-
age and 1 ma. The ion collector is operated 20 volts negative with respect
to the cathode and ground. Under these conditions the gauge sensitivity
for air is around 10 puttmps of ion current per micron of pressure. The cir-
ION COLLECTOR--\ [FILAMENT

ANODE

COVER

MOLfCULAR
BEAM
FIG.19. Cross sectional drawing of triode type ion gauge evaporation rate monitor.
MICROELECTRONICS 21 1
(wit shown in Fig. 20 is used to regulate the emission current, amplify the
ion current,, and regulate the evaporation rate.
By careful attention to geometrical positioning, this type of evaporation
I ate controller has produced films that have optical densities consistent
to 2yc.The film thickness should have a corresponding consistency. The
principal rawe of variation is the movement of the gauge relative to the
fourre. A n inverse square law of evaporating pressure vs. distance is seen
by the gauge and this markedly affects the film thickness obtained. Cali-

-
-
George A Philbrick
3~ Researches b c

22 sv
-
- .I M

t 300 -300

FIG.20. Scheniatic diagram of ion gauge emission controller and evaporation rate
regulator.

bration of such a gauge and evaporator is normally carried out by evapo-


rating a known weight charge of material to completion and observing the
time required. Repeated runs of the same weight have shown that the re-
sults are repeatable to within 2% of any previous experiment and better
than 1% of recent experiments.
The ion gauge shown in exploded view in Fig. 21 is a ccramic-metal type
tlcsigned for service in the ultrahigh-vacuum system where high bakcout
temperatures are used. This design will eventually become the ionizer for
an rf mass spectrometer that will be used l o monitor evaporation rate to
212 KENNETH R. SHOULDERS

and from the substrate. This gauge uses a control grid to control the emis-
sion, an anode operating at around 300 volts to draw emission into the
ionizing chamber, an ionizing chamber that can have its potential varied
between 10 volt,s and 300 volts, and a small diameter ion collector wire
operating up to -20 volts. Typical operating currents are: first anode,
2 ma; ion chamber, 4 ma. The ion chamber has a separate collector a t the
far end from the electron source that operates at about 1ma. This electrode
is used to indicate the ionizing current and is connected to the current
regu1at)ingamplifier. The output of this amplifier connects to the control
grid and maintains constant ionizing current. A 0.003-inch-diameter wire

FIG.21. Ceramic-metal type ion gauge evaporation rate monitor designed for high
temperature service in ultrahigh vacuum.

is inserted into the ionizing chamber to give an indication of the gas or


molecular beam pressure there. The sensitivity of this gauge operated under
the above conditions is 20 ramp per micron of pressure for air.
The gauge is constructed of high alumina and fired in vacuum at 1900°C.
The metallizing is a 0.0005-inch-thick coating of - 325 mesh molybdenum
powder mixed with 10% zirconium oxide and fired at 1900°C. The various
terminal posts and rods consist of molybdenum wire that has been ce-
mented in by a 90% alumina and 10% zirconium oxide mix that is also
fired in vacuum at 1900°C. The dimensional stability of these parts is ex-
cellent, even at 900°C bakeout temperatures.
Both types of ion gauges may be used to monitor the evaporation from
any type of source. When these gauges are used with high powered electron
MICROELECTRONICS 213

bombardment evaporators the leads have to be shielded from stray elec-


trons and ions; in addition, deflection plates are placed at their molecular
beam entrance in order to prevent ions and electrons from entering directly
and changing the gauge calibrations.
These gauges must be operated in a vacuum of’ better than iiim Hg
to reduce the effects of background gas 011 the gauge reading; however, they
have been operated at pressures as high as lop4 mni Hg by using a second
gauge t o monitor the background gas pressure oiily and then subtracting
the two gauge readings externally. A 3% balance over a pressure range of
100 t o 1 has been obtained in the past.
B. Substrate Heater
A substrate heater that is particularly adapted to reactive deposition is
represented in the sectional drawing of Fig. 22 and shown disassembled in

FILAMENT SUPPORT

CATHODE MOUNT AND

MOLYBDENUM UNTING HOLE AND

SUBSTRATE HOLDER

b-lcm4

FIG.22. Ceraiiiic-metal elrctroii I)omlmrtliiiriit siibstrtitr h a t e r for 1500°C service.

Fig. 23. This heater is designed to raise 0.70-inch-square substrates to


1500°C without introducing reaction by-products or introducing impurities,
as some metallic heaters do. The construction material is alumina with
molybdenum coating on the inside of the cups. High temperature vacuum
firing methods are used throughout (as in the ionization gauge described
in Section VIII, A), thus preventing volatile impurities from spoiling the
films being produced.
Heating is accomplished by electron bombardment of the molybdenum
coating on the inside of the anode cup. The emission source is a 0.010-inch-
diameter tungsten filament wire that emits up to 0.10 amp. A circular piece
of molybdenum is used in the center of the filament to give an annular elec-
tron beam on the anode t o improve the heating uniformity. Regulation of
the heat is obtained by n standard emission controller, as used on the ion
gauge evslporatioii rate regulators. The regulators can be fed from a high
gain ampl%er,’such as the Philbrick USA-3 that is used to amplify the out-
put of a thermocouple. The thermocouple may be either placed near the
214 KENNETH R. SHOULDERS

substrate and operated by radiation coupling or by evaporating molyb-


denum-tungsten thermocouples onto the substrate.
Using 1000 volts at 50 ma the heater reaches 800°C; 3000 volts and
100 ma gives 1700°C. The maximum temperature is limited by the soften-
ing point of the aluminum oxide anode, which is about 1700°C. This type
of heater, having no voltage gradient across the hot ceramic, can attain
higher temperatures than the resistance wire type because of the absence
of electrolysis in the ceramic due to the presence of an electric field. Broad

FIQ.23. Photograph of disassembled substrate heater shown in Fig. 22.


area metallic sheet heaters can reach high temperatures, but they usually
have exposed hot metal parts that can cause undesirable chemical reactions
during etching or deposition.
The small substrate heater shown in Fig. 24 is used for carrying out ex-
periments on electron microscope specimen screens. This heater is heated
by a 0.015-inch-diameter tungsten filament and can reach about 1000°C at
16 amp. The principal construction material is alumina. The substrate
heater is used in the demonst,rntioii of electron-beam-activated micro-
machining described in Section XIV. It is shown installed in the vacuum
system in Figs. 13 and 14.
MICROELECTRONICS 215

-THERMOCOUPLE
HOLE

HEATER .-
,-RETAINER
SPRlNQ

C. Reactive Deposition
Reactive deposition is characterized by low pressure rnolccular beam
sources that are in line of sight of the substrate. The commercial process
called vapor plating [55] is normally carried out at high pressures in a con-
tainer; here there is a st,rongpossibility of reaction with the walls and hence
contamination of the specimen being deposited. Some work in vapor plat-
ing has been directed toward epitaxial growth of semiconductors and other
electronic end-products [56], but the majority of the work is for the pro-
duction of thin corrosion-proof coatings on high temperature devices like
rocket nozzles and exhaust manifolds.
The two large classes of reactive deposition arc pyrolysis and combina-
tional reactions. The first class is illustrated by the deposition of silica from
the decomposition of tetraethylorthosilicatc on a hot surface and the depo-
sition of tungsten from the dccomposition of tungsten hexacarbonyl. Most
low temperature rcactions involve thc decomposition of organic compounds
and the side reactions can contaminate the deposit more readily than in
cases where inorganic sources are used. High temperature reactions of the
same type are known as thermal decomposition reactions, and with these
material can be deposited from the halides directly without undue fear of
contamination. The deposition temperatures by this method are frequently
too high t o be useful, in that the substrate will not withstand the tempera-
ture. The second class of reactive depositions are produced by evaporating
two materials to a hot surface simultaneously and reacting them. Molyb-
denum is produced by the reduction of molybdenum chloride with hydrogen
or a reactive metal such as zinc, aluminum, or magnesium. I n this reaction,
the volatile halide is carried away from the hot substrate and deposits on
216 KENNETH R. SHOULDERS
t,hc wall of thc equipment or is pumped away. Aluminum osidc is dcpositctl
by the reaction of aluminum chloride and watcr vapor or othcr oxidizers
such as ammonium nitrate. The deposition temperaturc for this second
class of reactions is conveniently in the range of the maximum allowed by
our substrates. The highest temperature that the substrate can tolerate is
desirable because of the tendency to form clean stable deposits at high
temperatures.
1. MATERIAL SOURCES

The only end-product deposition method considered useful for this proj-
ect is the oxidation and reduction of metal halides. Thus the principal
problem in a source is obtaining pure metal halides. This may be done by
filling small glass ampoules with material after vacuum distillation, and
then breaking the ampoules after they have been transferred to the depo-
sition chamber and are ready for use. These ampoules must be baked mildly
in the deposition chamber before they are opened in order to drive off ad-
sorbed gas, but they must not be put into the high temperature zone of the
ultrahigh-vacuum system because it is baked out far above the softening
point of glass. A vacuum lock is needed to make the transfer. This method
is good for some special purposes but does not have the versatility of the
method discussed below.
Materials such as iodides, bromides, chlorides, and fluorides can be pro-
duced in situ by reaction of the metal that is to be transported to the sub-
strate with one of the halogens. The metal is heated in a small-diameter
tubing of alumina, quartz, or even the same metal, provided it is pure
enough. A halide is heated in the lower portion of the tubing to its decom-
position temperature and a low pressure gas results. Platinum chloride
makes a good regenerative source for chlorine. This gas passes up the tube
toward the hot metal and reacts with it to produce a volatile halide that
goes to the substrate as a molecular beam. If the parent material is intro-
duced as a clean vacuum-refined metal, and the halogen source is handled
so as not to produce any volatile halides or metals, then a pure metal halide
for deposition purposes results. All halogen sources should be line-of-sight
baffled from the parent metal to be reacted and should contain a cold re-
gion for the purpose of stopping and condensing any of the decomposition
products that are not halogens. A universal source of this type can be de-
signed to fit practically any deposition apparatus.
Alloys have been found particularly easy to handle by this method. The
alloy is inserted in the heated tube and the halide passes over it to produce
the correct ratio of halides corresponding to the alloy composition after a
short time has elapsed to obtain equilibrium. The alloy sample is held a t a
temperature high enough to react all components and volatilize all of them.
MICROELECTRONICS 217

If one coniponcrit is slow to react, it soon becomes prcdominant on the sur-


face, as a result of the rcmoval of thc othcr compoiiciits, but thc corrcct
ratio is ultimately obtained. If there is bulk diffusion of the sample, then
an improper alloy is obtained, bcrause the reaction surface is constantly
saturated with this mobile element. Whether or not the proper alloy is ob-
tained a t the substrate surface is largely a function of the ratio of the re-
action efficiencies of the various components of the alloy a t the substrate
and not a function of the source material. A test was conducted by the
author on a molybdenum-tungsten alloy containing 80% tungsten; a
chemical analysis showed that this was approximatley the content of the
film obtained.
The control of the evaporation rate from these sources is obtained by
adjusting the temperature on the halogen generator. A feedback loop from
the halogen heater to the ionization gauge monitor regulates the evapora-
tion rate to any desired value. The heater on the metal source rcmains fixed.
It is desirable t o generate halogen gascs and metal halides in situ in order
to overcome the difficulties of introducing thc pure gases into the ultrahigh-
vacuum chamber through automatically regulated mechanical valves. Most
metal chlorides are deliquescent,, absorb inoisturc rapidly, and cannot be
handled in air. This method of generating them in the vacuum chamber
has been found to relieve the problem. Many sourccs for halogen and other
gases are available. Oxygen is obtained from silver oxide, hydrogen from
heating zirconium or uranium hydride, fluorine from cobalt fluoride 111,
chlorine from platinum chloride or molybdenum triehloride. All of these
sources can produce very pure gas if properly handled. Compounds such
as ammonium chloride may occasionally be used to replace halogen sources
without danger of side reactions. Metal chlorides such as lead and thallium
chloride can also be used because there is very little possibility of the metal
component remaining a t the substrate as a compound or in the free state,
due to the high temperatures used during deposition.
2. MOLYBDENUM AND ALUMINUM OXIDE DEPOSITION

Molybdenum and aluminum oxide have been successfully deposited


by the author in various shapes and on various surfaces to test some of
their properties. These materials were taken as representative of a class
that would be used in tunnel effect devices, namely, a refractory metal
and a dielectric. The materials were deposited on field emission microscope
tips to determine cleanliness; thcy were also made into sandwiches to test
encapsulation and to test pin-hole effects, dielcctric breakdown strength,
and electrolysis effects.
Molybdenum was deposited on clean, smooth, sapphire substrates by re-
acting molybdenum chloride with hydrogen a t 1200°C. The substrate was
218 KENNETH R. SHOULDERS

hratcd by direct clcctxon bombardmcnt and was not uniform in tcmpri-a-


ture by more than 200°C. Electron bombardment also tends to cnhanw
the deposition [26] but the amount was not determined for this case. Tho
molybdenum chloride was obtained by direct chlorination of molybdenum
with chlorine gas, as described earlier. The hydrogen was obtained by
heating zirconium hydride to around 900°C. An excess of hydrogen, by a
factor of two, was used over the theorectical amount that is needed to carry
out the reaction. A molecular beam pressure of around mm Hg a t the
surface was computed. The deposition time ran nearly one-half a minute
to produce a 200 A-thick film, as judged by optical transmission, which
indicates a low deposition efficiency. Separate tests were also run on thin
film aluminum oxide substrates so that direct electron microscope exami-
nation could be undertaken. Because of crystal growth, these reactively
deposited samples showed a rougher surface than is produced by evapora-
tion; the roughness was approximately 50 A or 25% of the crystal size.
The crystal size was in the same order as the film thickness. For heavy
deposits that must be smooth, alloying with materials to reduce the crystal
size could be undertaken. Small crystal size is also desirable from the stand-
point of micromachiniiig, as will bc discussed latcr in the section on molec-
ular beam etching.
Aluminum oxide was iicxt deposited to a thickness of 200 A by reacting
aluminum chloride with water vapor on the 1200°C substrate previously
coated with molybdenum. Aluminum chloride was obtained by direct
chlorination of aluminum a t around 400°C; watm vapor was admitted to
the system by a simple valvc. One difficulty is encountered with this sys-
tem: the alumiiium chloride gauge becomes coated with aluminum oxide
and produces erroneous readings. This was later avoided by using solid
oxidizers that cannot enter the aluminum chloride gauge because of the
shielding between the gauges. Deposition temperatures as low as 300°C
appear to produce aluminum oxide films, but previous experience with un-
stable forms of aluminum oxide dictated temperatures above 900"C, the
recrystallization temperature where stable alpha alumina is formed.
During this deposit, a water-cooled mask was used to prevent deposition
on the molybdenum terminal of the final metal layer. This masking was
not very defined due to the high surface mobility and reevaporation from
the substrate and mask.
Electron microscope examination of the alumina film produced by this
method did not show any of the dust-speck shadowing effects that can be
found in thermally evaporated films. The film appeared continuous, dense,
and about as rough as the molybdenum deposits. No examinations were
undertaken on combination molybdenum and aluminum oxide films be-
cause it was believed that the high density of the molybdenum would
MICROELECTRONICS 219

obscure the alumina detail, as in the case of evaporated films that have
been tested.
A second layer of 200 A thick molybdenum was deposited through a
water-cooled mask so that the lower electrode was not coated. This second
layer was connected to a terminal which formed the capacitor between it
and the lower electrode.
A layer of aluminum oxide approximately 2000 A thick was next de-
posited over the entire assembly, then a 2000 A molybdenum layer, and
finally a silica layer formed by decomposing tetraethylorthosilicate at
900°C. These three layers formed the encapsulation for the assembly. The
tests for encapsulation effectiveness have been described in Section IV, G
on tunnel effect component encapsulation.
3. ELECTRICAL TESTS

The electrical tests for the above assembly have been designed to show
signs of instability in the materials. These tests amounted to heating the
assembly by passing a current through the thin base metal and observing
any change in the resistance with time. It was assumed that any migrating
material, material diffusing through the encapsulation, electrolytic action,
or recrystallization would result in a shift in resistance of the metallic film.
When a test piece had been properly made, heating at 800°C for as long
as 20 hours in various corrosive media did not show any change in resist-
ance in excess of the 2% experimental accuracy. Tests for a period longer
than 20 hours were not performed because the few samples that werc
produced were destroyed in the capacitor tests to be described. Poorly
processed test pieces would show an almost instantaneous shift of charac-
teristics upon heating. These fault,s wcre usually traced to an inadequate
terminal encapsulation.
Dielectric tests were performed to determine the niaximuni field strength
attainable and to investigate any field enhanced migration that might be
a result of foreign materials or decomposition of the dielectric. A resistivity
of about 1OI6 ohm/cm was measured at room temperature; however, the
actual value may ham been higher because of the increased effective area
of the rough surface. The only method of measuring the dielectric constant
was to use the ZtC charging time of the capacitor and then use the area and
thickness to compute the dielectric constant. The capacity was around
100 mfd/cm2 for an estimated thickness of 200 A. The calculated value of
dielectric constant was abnormally high and it was concluded that the
surface roughness obscured the real dielectric constant. The data on the
dielectric constant was secondary to the results sought on stability.
At 800°C the resistivity of the dielectric was about 1Olo ohm/cm. This
resistivity measurement could be repeated after many temperature cycles
220 KENNETH R. SHOULDERS
between room temperature and 800°C. A few cycles were made between
liquid nitrogen temperature and room temperature with no observed effect.
By raising the voltage to about 20 and producing a fieId of lo7 volt/cm
in the material, strong indications of tunnel emission could be observed.
The voltage that produced this emission varied by as much as a factor of
five between the several samples that were available. To find the point
that emission occurred, the voltage was raised very slowly, giving the
charging current of the capacitor time to subside. Increments of only a few
millivolts were used and the maximum current change was only a fraction
of a milliampere because of the sudden onset of tunnel emission. When the
emission point is found it can be distinguished from ion current in a quali-
tative way by changing the temperature a small amount. The tunnel emis-
sion is normally able to sustain a more or less constant current with small
increases in temperature, whereas ionic conduction increases more rapidly.
Tunnel emission that is affected in some way by traps would also be ex-
pected to show a strong temperature dependence, but the experience gained
in these tests allowed at least a few examples to be seen where the conduc-
tion current was primarily due to tunnel emission currents.
The test for dielectric stability that seems most significant is the stability
of the leakage current when the field is just under the value for tunnel emis-
sion to occur. The voltage for tunnel emission is found to be lower as the
temperature is increased, and a reduction of voltage by 20% a t 800°C is
considered to be normal for the samples used. If this voltage variation is
taken into account, then the temperature may be cycled repeatedly with
no apparcnt change in operating condition. When a normal capacitor or a
poorly made film sample is left for some time at high field strength there is
a gradual increase in current until an irreversible breakdown occurs. This
current increase is accompanied by an instability or noise, which is assumed
to be some form of material migration that precedes and causes actual
breakdown. The most certain test for a good metal-dielectric system is a
stable tunnel emission current. In several examples this current has been
several milliamperes before breakdown occurred. Occasionally the break-
down is violent enough to clear the area around the emission site and allow
further testing-without encapsulation. These tests were tried with evapo-
rated dielectrics and anodically formed dielectrics; however, even though
some results could be obtained near room temperature with anodically
formed dielectrics, the high temperature results were completely negative.
Evaporated materials yielded so few samples for testing, due to pinhole
effects, that they were given up. Large area, 200 A thick dielectrics are
difficult to evaporate.
The dielectric tests were attempting to show that the theoretical break-
down strength of a little over lo8 volt/cm could be achieved, but tunnel
MICROELECTRONICS 22 1
emission currents limit the applied field to around lo7 volt/cm. If sclf-
formation processes, described in Section IV, F, had been used t o smooth
the surface it may have been possible to reach higher values. Powers [4]
has shown the breakdown strength for glasses such as aluminosilicate to
be as great as 2 X lo8volt/cm; very smooth glassy surfaces were available
and a special low emission cathode of silver iodide was used.
4. FIELD EMISSION MICROSCOPE TESTS
In order to confirm the above limits and to test for purity of the deposi-
tion processes, a limited amount of work was carried out on field emission
microscope tips, where many things can be directly seen and related to
tunnel effect component work.
Aluminum oxide was deposited on tungsten tips and measurements were
made as described in Section IV, I on solid state tunnel effect components.
The general conclusion directly confirmed the above finding-namely, that
tunnel emission occurs a t the same applied voltage with or without a di-
electric layer of alumina, and that this emission current brings on the
breakdown. The maximum current density that could be supported by
thc alumina on the tungsten tip was about 103 amp/cm2.
Molybdenum was deposited by reactive deposition on tips of tungsten
and molybdenum. The tip was also etched slightly with chlorine. When
the tip was tested for cleanliness by viewing the emission pattern in a n
ultrahigh-vacuum system, no effect that could be attributed to impurities
was notcd. The tip had grown a prcdictable amount due to the deposition.
The tip was never heated higher than 150O0C, in order to simulate the con-
dit ions that would exist in actual componeiit construction on a sapphire
substrate. The best method available to see the effects of interstitial im-
purities would be the use of ficld ion microscopy. Mueller [IG] has shown
single atom interstitial impurities of oxygen in platinum. This method
suffers slightly for poorly bound impurities in that the high fields of
lo8 volt/cm used in field ion microscopy tend to desorb the impurities.
This is of little concern, however, since our heating process would also
drive these matcrials off.
D. Single Crystal Growth
The apparatus for depositing single crystal films on amorphous or micro-
polycrystalline substrates is available with the various material sources
and substrate heaters; however, adequate information is not available a t
the present time on how to use this apparatus to produce the desired result.
Small area films of single crystal silicon have been grown inadvertently
during an etching process in which a polycrystalline film of silicon was
being removed from a silica substrate by chlorine. A decomposition of
222 KENNETH R. SHOULDERS

the silicon chloride apparently resulted, and single crystal sheets about
0.03 X 0.005 inches were formed; these sheets had a thickness that varied
from several hundred angstroms to several thousand angstroms in a step-
wise fashion. The existence of the single crystal over the entire area of the
deposit was confirmed by the selected area electron diffraction attachment
of the electron microscope. The substrate was amorphous silica.
Attempts to produce single crystal films of material on micropolycrys-
talline substrates would involve using reactive deposition methods near
the equilibrium temperature where either deposition or etching could occur
and then sweeping a thermal gradient across the substrate by electron
bombardment so as to cause the growth to commence at one side and pro-
ceed across the surface. Epitaxial methods on single crystal substrates
would not need a sweeping thermal gradient.
At this point in the art of depositing films of material it is not clear
whether micropolycrystalline films or single crystal films will be the most
likely to produce the fewest troublesome imperfections across their thin
dimension, imperfections that would cause migration, electrical breakdown,
and etching difficulties. A single flaw between the surfaces in a single crystal
film would be disastrous, whereas a micropolycrystalline film with several
aligned crystallite boundaries in series could produce an equivalent effect.
By admixing materials and using stratified structures the grain boundary
diffusion could be retarded, but there is not enough experimental evidence
to compare this case to the practical single crystal case. To the author’s
knowledge, all single crystal thin films that have been produced thus far
have shown strong variations in the thickness dimension; however, it is too
early to accept these indi~nt~ions conclusively.

E. Instrumentation Methods
Instrumentation is needed for the determination of film thickness as the
deposit is being formed so that process control can be achieved. I n addition,
instruments are needed to monitor the chemicals being used in the deposi-
tion and etching process and to aiialyze thc impurities contained in samples.
The two instruments best suit,ed to the above requirements are an X-ray
fluorescence spectrometer and a mass spectrometer.
X-ray fluorescence methods have been shown to be capable of analyzing
grams of material to an accuracy of 1%in an area as small as one
micron [57]. These methods are applicable to all elements, provided that
absorption of the emitted X-rays by gas or detector windows is prevented.
The vacuum chamber is an ideal operating environment for such equip-
ment. X-ray methods are independent of the temperature of the sample
being measured and of the crystal structure because nuclear processes are
MICROELECTRONICS 223

iiivolvcd. These propcrties make the process applicablc to the detcrmina-


t ion of film thickness during deposition at elcvatcd tcmperaturcs.
Future cquipmcnt will incorporate a simplc clcctron gun focused to a
small spot on the substrate during deposition, and an appropriate X-ray
detector such as an electron multiplier coupled with an analyzer crystal to
be used as an X-ray filter. The electron multiplier will be followed with a
counter, integrators, and analog control equipment for regulating the film
thickness. By proper electron beam current monitoring and standardization
techniques involving periodic deflection of the beam to a st,andard sample,
a film thickncss determination repeataldc t o 0.1% could be achieved.
Thickness control is useful for both dcposition and etching operations.
The equipment must operate in the vicinity of the deposition apparatus,
and one of the prime design rcquirernents is the prevention of contamina-
tion of the electron gun and detector surfaces. By using molecular beams
of solids instead of gaseous materials most of the contamination could be
eliminated by simple shielding; howcver, the substrate being deposited
upon emits a small quantity of material as a result of reaction inefficiencies
and these materials tend to deposit on both the electron lens and the X-ray
detector. Periodic testing of thc surface through mechanical shutters when
the molecular beams are shut off would offer oiic solution, but not an en-
tirely dcsirable one.
A quadrupole mass spectrometer incorporating some features described
by Paul [58] and by Brubaker [59] will he constructed and used to monitor
both evaporation rate from the sources to the substrate and reevaporation
from the substrate. In addition, the spectrometer can be used for destruc-
tive analysis of the various deposited films by either etching them off or
sputtering them off and looking for the quantity and type of material con-
tained in the film. This instrument will greatly aid in the understanding
of the free radical type of surface chemistry that predominates in this low
pressure range.
The spectrometer consists of an ionization unit and an analyzer unit.
The ionizer will resemble the one illustrated in Fig. 21 and described in
Section VIII, A. The aiialyzer is simply four cylindrical conductors operat-
ing a t correctly chosen amplitudes of dc and rf frequencies. In operation
the rf is swept across a range of frequencies in synchronism with the hori-
zontal axis of a monitor oscilloscope. The vertical axis of the oscilloscope
is fed from the selected ions that traverse the analyzer unit and a spectrum
of atomic mass units versus their quantity is observed. The unit is equally
applicable for solids or gases, and is intended to replace the present ioniza-
tion-gauge evaporation-rate monitors. A stability in the region of 1% is
expected for this instrument and a sensitivity adequate to detect a frac-
tional monolayer on the surface appears available.
224 KENNETH R. SHOULDERS

IX. Material Etching

Since selective deposition cannot be carried out by reactive deposition


methods to the high resolution required in our microelectronic work, we
combine high-resolution selective-resist production with a gross etching
process to give the desired micromachining action. The etching will be
done in the samc vacuum system used for deposition in order to maintain
high purity and good control over the process. There are three somewhat
similar methods that are compatible with our requirements: molecular
beam etching, atomic beam etching, and etching by sputtering. Molecular
beam etching is the most commonly used and will process 90% of the
materials that must be etched. Atomic beam etching is used when the
reactions at the surface must be produced at a low temperature; sputtering
is used when the surface material must be removed without any heating.

A. Molecular Beam Etching


1. GENERAL METHOD

When a heated surface in vacuum has a molecular beam of material


directed upon it there is possibility of reaction and etching. The etching
is produced by volatile species being formed and evaporating from the
surface. The most readily volatile class of simple compounds are the,halides
formed by reacting a metal with halogens. An example of this is the etching
of molybdenum with chlorine gas in which molybdenum chloride is formed
and evaporated from the surface. A temperature in excess of 500°C is
needed to supply the activation energy for the reaction and to volatilize
the chloride. In general it will be found that the more active halogens like
chlorine and fluorine react more easily but produce less volatile halides,
while the less active iodine and bromine are more difficult to react but
produce highly volatile compounds. This has a tendency to keep the mini-
mum operating temperature constant for the different halogens. The
choice among halogens is largely based upon other considerations, such
as compatibility with the resist and the underlying layer that will be
reached upon completion of etching, as well as the availability of the pure
halogen.
Sources of molecular etchants can be divided into two classes-solids
and gases. The gaseous sources are most easily obtained by admitting
bottled gases into the vacuum system through a valve; however, this is a
cumbersome method for controlling the gas pressure at the surface, and
it is difficult to secure a clean source of gas. As mentioned in Section VIII,
C on Material Deposition, halogens can be obtained by the thermal de-
MICROELECTRONICS 225
composit ion of various materials such as molybdcnurn trichloride, platinum
chloride, and cobalt fluoridc. Thesc sourccs can bc vcry clcan if prccautions
arc taken to prevent solid products such as ~nctalsand lowcr chlorides
from being carricd along with the gas. The prcssurc of thc gas can be con-
venirntly controlled by adjusting the heat on the source, and regulation
can be achieved by ion gauge monitoring and fecdback to the heater with
the equipment shown in Figs. 18 and 20. One difficulty with gaseous ctching
sources is that they must bc continuously pumped from the system to pro-
duce molccular beam conditions. Evcn with fast pumps, the number of
collisions a t the surfacc by molcculcs arriving a t anglcs other than normal
to the surfacc is high. This can produce a11undcrcutting action of the resist.
Matcrials that begin as solids from thc sourccs and can be deposited as
solids a t room temperature are cffectivcly pumping thcmsclvcs a t a very
high rate and can produce truc molccular bcams. The arrival angle at thc
surface is always vcry near thc normal anglc and any uiidercutting of thc
m i s t would bc caused by other cffccts. An extremely wide range of com-
pounds arc available that will producc ctching cffccts. The choice is largely
dependent upon the side reactions produccd from thc compound. For
hydrogen fluoride sourccs, materials like ammonium fluoride and am-
monium bifluoride havc been found dcsirablc because their side products
are gaseous and do not foiin any stable nitridcs or hydrides with molyb-
denum, one of thc principal materials under invcstigation here. These
hydrogen fluoride sources are good for the removal of silica resist layers.
Almost any solid compound of a metal and a halogen can be considered for
the production of the halogen provided the compound reacts a t the etching
temperature used and that the side reactions produce volatile products.
Examples of materials that have been used include aluminum chloride,
ammonium chloride, lcad chloride, thallium chloridc, potassium acid
fluoridc, potassium tantalum fluoridc, ammonium fluoride, and ammonium
bifuoride. By using solids and molecular beam techniques, reactions with
the vessel can be prevented that could result in transport of foreign mate-
rials to the surface. The source material purity largely governs the final
purity of the etched deposit. Solid sources also prevent unwanted etchants
from entering the various instruments in the system, such as X-ray thick-
ness monitor, ion gauges, and the electron lens.
Molecular beam etching can be produced a t lower than normal tempera-
tures by supplying the activation energy for the reaction by electron bom-
bardment during the etching. Current densities in the order of 0.1 amp/cm2
must be used to provide high reaction rates in the order of one hundred
monolayers per second. The difficulty with this process is that good uni-
formity of the electron bombardment is hard to obtain, compared to that
obtained by heating the surface uniformly. Even if reactions can be ob-
226 KENNETH R. SHOULDERS

tained on the surface the process will not always be good for etching be-
cause the reaction products arc not volatile. Volatility can usually be
increased by forming a higher halide or by forming a complex compound.
Platinum chloride is an example of a low volatility compound that can be
converted into a highly volatile compound by reacting with carbon mon-
oxide to form the halide carbonyl. Other organic compounds, such as metal
acetonates, can be formed that have high volatility. A risk is involved in
using these organic rcactioris in that t,hey may form unwanted stable
metal carbides.
Metals that have heen microetched with chlorine gas include tungsten,
molybdenum, tantalum, nickel, iron, aluminum, and silicon. Silicon dioxide
has been etched with ammonium bifluoride and potassium acid fluoride,
and aluminum oxide has been etched with phosgene and potassium tan-
talum fluoride. There appears to be a gas or a compound available to etch
any known material and fairly simple chemical selection rules can be used
to determine the proper ctcharit and etching tcmpcrature.
2. PURITY TESTS

Molecular beam etching using chloriiie gas has becri carried out in the
past by the author on a tungsten field emission microscope tip to determine
whether or not any residue resulted when conditions simulating the final
process were used. An cmittcr tip of approximately 1000 A radius was
exposed to a chloride gas pressure of around mm Hg for two minutes
a t about 600°C in the absence of an electric field. When the vacuum
chamber was returned to ultrahigh-vacuum conditions and the tip was
heated momentarily to 1500°C the emission pattern observed resembled
the original pattern. The conclusion was that the tungsten was not con-
taminated by chlorine under these conditions. Admitting chlorine to the
system a t a very low pressure the work function would immediately rise,
indicating that a clean condition had initially existed.
Aluminum oxide has been deposited on a 1000 A tungsten field emission
tip by thermal evaporation to a thickness of around 400 A and then heated
to 1500°C for stabi1il;ation. A low current could be drawn through this
dielectric layer without destroying it and some of the characteristic appear-
ance described by Mueller [20] was observed during the early deposition
phase. The tip was heated to around 400°C and etched with phosgene gas
at a pressure of mm Hg for four minutes. When the vacuum system
was returned to ultrahigh-vacuum condition and the tip was heated to
1500"C, the tungsten pattern reappeared, indicating that the aluminum
oxide had been removed without altering the tungsten pattern or radius
in any visible way. It was assumed that carbon formed from the phosgene
decomposition would have resulted in an enhanced emission around the
MICROELECTRONICS 227

:11dlonwcd eniission on thc 334 plmies, :ts shown by


01 1 a i d 112 p1aiic.s
Mueller [GO]. This \\ah iiot evidcnt.
Tests werc carried out using duniinuni cliloritlc to etch tuiigstcn tips in
the accidental prescnce of oxygeii or water vapor-which is normal for a
mni IIg vacuum system-and the aluminuni oxide pattern appeared.
This could bc explained by the reaction of thc aluminum chloride and
n.ater vapor 011 the hot tip.

3. DEEI' ETCHING

If 100yo reaction efficiency could be obtained, the molecular beam etch-


ing process would produce straight sides on thc etched samples and give
very high ratios of depth to width. In practice, the surface migration of
the etchant and compounds formed between the etchant and the film
material set limits to the depth-to-width ratio. Materials have been
tktchcd that show ratios as high as 10 to 1. In this experiment the etched
shape was a hole about 300 A in dinnictcr and 3000 A deep in a film of
evaporated molybdenum. Possibly deeper holes could have been etched;
however, the film thickness was only 3000 A. It is not known whether a
pillar 300 A in diameter and 3000 A high could also be obtained by the
same process.
Etching is sometimes accompanied by a decomposition of the compounds
formed after they have migrated some distance from the site of formation.
In some extreme cascs with silicon films being etched in chlorine, the
silicon chloride decomposed so as to form a finger-like growth of single
crystal silicon. The crystals were several thousandths of an inch long and
were not uniform in thickness. This decomposition process could con-
ceivably be controlled to nullify thc effect of undercutting.
With low-efficiency etching therc is a preferential attack on various
faces of certain crystals, as can be sccn most readily with the field emission
microscope. This effect would tend to produce an uneven etch on films
composed of randomly oriented crystals, being most pronounced for films
having large crystals extending through the thickness dimension of the
deposit,. Ry proper alloying of the materials, the crystal size could be
minimized and the cffrct reduced. Another method of controlling the dif-
ferent etching rates a t the various faccs is to adsorb materials on the
sensitive faces that retard the etching. Optimization of any particular
system of chemistry could be carried out on the field emission microscope
and the process could then bc applied without modification to the niicro-
machining process. Conversely, by simultaneously depositing a non-
migratory catalyzing material, the etching process may proceed more
rapidly in thc thickness dircction than through the lateral direction; the
effect would thus give straightcr sides to the etched shape.
228 KENNETH R. SHOULDERS

B. Atomic Beam Etching


Atomic beams of dissociated moleculcs have larger reaction energies
than molecular species and can bring about reactions at much lower tem-
peratures. Wise and King [61] have shown the room temperature reaction
and etching of carbon, silicon, germanium, and tin with atomic hydrogen.
The hydrides of these materials are volatile at room temperature so that
etching can proceed without interference from a surface layer. Atomic
beam etching can offerno improvement over molecular beam etching unless
the products formed are volatile a t the etching temperature. Reactions
known as “Paneth reactions’’ [62] have long been used to identify methyl
free radicals, which are an atomic species. These reactions involve passing
a methyl radical vapor over lead at room temperature. The lead is reacted
to form a methyl-lead compound which moves down the tube, decomposes,
and plates a lead mirror on the walls of the apparatus. The fact that the
species produced is unstable after reaction does not alter the utility of the
etching process. I n either molecular beam or atomic beam etching the
active materials are kept away from other gases, and from the walls of our
processing chamber, and thus have no opportunity to give up their energy
or decompose.
Atomic species are usually produced by an rf discharge in a low pressure
gas. The simplest method of accomplishing this in our apparatus is to use
an rf field across the end of a quartz tubing having a small hole in the end
and a gas pressure inside the tubing in the range of 100 microns. The exit
atomic beam pressure should not be over 20 microns so as to produce the
necessary mm Hg pressure a t the surface being etched. Simpler
sources are available for some materials, such as hydrogen, which can be
obtained by heating zirconium hydride. This molecular beam is then
directed onto a tungsten plate operating a t 17OO0C, thereafter reevapo-
rating to the surface to be etched with hydrogen atoms. In a similar
fashion chlorine and oxygen atoms can be formed by reaction with hot,
surfaces. For example, Langmuir [63] noted that tungsten deposits on the
walls of an incandescent lamp were removed when the filament was heated
to the dissociation temperature of chlorine, which was contained in the
bulb a t a low pressure. He attributed the removal of the dark tungsten
deposit from the walls to the formation of tungsten chloride. In other
experiments involving two tungsten filaments, one running a t high tem-
peratures and the other a t low, the low temperature filament was etched
away on the side facing the hot filament and the hot filament gained weight
from the thermal decomposition of the chloride so produced. The use of
atomic species can markedly increase etching efficiency and yield large
depth-to-width ratios.
MICROELECTRONICS 229

C. Ion Beam Sputtering


Material can be removed by physical or chemical sputtering [64] in a
vacuum system operating a t a pressure of around 100 microns. The sput-
tering gases can be either inert or made chemically active to enhance the
removal rate. The principal disadvantage to sputtering is the possibility
of destroying electrical circuits by dielectric breakdown. The charge
accumulated on the surface of a sputtered material can easily produce
fields greater than the breakdown gradient of the underlying dielcctric.
An additional disadvantage of sputtering at high removal rates useful for
the micromachining process is the tendency to alter the electrical prop-
erties of material through damage to the crystal lattice, and by driving
the sputtering atoms into the lattice. RrIost of these effects can be annealed
out, as shown by Farnsworth [65].
The principal advantage of sputtering is the possibility of obtaining
high ratios of depth to width of the etched sample, because of the high
energy and high efficiency of material removal for the impinging atoms.
Wehner [66] has given examples of the sputtering and etching of a silver
surface, with fine abrasive particles imbedded in the surface, which left
many long pillars of silver after etching. In a discussion with the author,
Wehner stated that the etching angle was in the vicinity of one degree.
The abrasive particles were probably aluminum nxide, which has a very
low sputtering rate and makes a good resist.
D. Depth Control
Molecular bcarii etching tests on molybdenum have been performed by
the author in which a 3000 A-thick film of niolybdenum on an aluminum
oxide film xas etched in chlorine until a mean thickness of 300 A was
rcached. The variation in thickness across the Pample surface was checked
in an electron microscope by observing the electron scatter produced by
the sample and found to be less than 100 A. Evidently polycrystalliiie
samples such as evaporated molybdenum can be etched by time-tempera-
ture methods to a repeatable thickness and to a uniformity greater than
2%. T o carry out uniform etching the temperature should be sufficiently
higher than the niininium value required, so that variations in temperature
across the surface of the sample will not cause greatly different reaction
rates. The etching rate is then controlled by the rate of arrival of the
molecular beam on the surface, which is in turn controlled by the halogen
evaporation rate regulator to nn accuracy of 1% in the optimum caw.
The over-all accuracy of depth control that could be expected, and has
been shown experimentally for an open-ended type process, is in the order
of 5% under controlled conditions. This value should be increased to
230 KENNETH R. SHOULDERS

better than 1% for average operating conditions involving closed feedback


loops using 3000 A thick films. This implies a permissible variation of less
than 30 A from all sources.
Closed loop processes involving an X-ray fluorescent probe to monitor
the film thickness ~7ouldgreatly facilitate the control of etching depth.
This method is described briefly in Section VIII, E on Material Deposition.
The electron probe that excites the X-rays would bombard several areas
on the substrate not associated with components in order to check for
etching depth and uniformity. A mass spectrometer placed so as to observe
the reaction products coming from the surface can detect the conipletion
of etching for a particular material by showing the appearance of a new
species of compound and the disappearance of the material being etched.
There would be very little indication of the uniformity of the process over
the surface except for the sudden disappearance of a particular compound.
Perfectly uniform etching would produce a sudden change in thc materials
coming from the surface.
When absolute control over etching penetration is required, thc lower
layers of materials can be made chemically resistant to the molecular beam
etchant. A buffer layer of very thin material can be used between layers
of films; when this material is reached the etching process slops uiitil a
very short etch is used to remove the buffer laycr. In this fashion the
control over depth could be regulated to within approximately one-tenth
the thickness of the buffer layer, or around 10 A.

X. Resist Production

Selective etching of a material can be produced by first selectively


coating the surface with a chemically resistant laycr of material, and then
etching away the unprotected areas. The thickness of this layer rarely
exceeds 50 A and can be produced by a variety of methods. The simplest
method is to evaporate a material like silica or alumina through a mask to
the surface; however, this method suffers in both resolution and ease of
manipulation for the large quantities of information that must be passed
on to the surface. Optical systems could be used to expose light-sensitive
resists but these methods also lack resolution and the number of hits of
information per optical field is very limited at reduced size.
The method that seems best suited to the micromachining process is the
production of a resist layer b y electron beam methods. The principal re-
quirement for this method is that a chemical change be brought about b y
the action of electroils on a material without undue side reactions being
MICROELECTRONICS 23 1

c:uiwtl l)y light, X-rays, heat, stray low velocity wcondary clcctrons, or
1tackscat t crcd elcctrons. Dense mntcrials ctpnblc of absorbing thc energy
of an elrctroii beam arc necd(tl so that the exposure tiiiie can be as short
as the mechanical wanning time recluircd to pass the substrate under thc
lens and produce many exposures or frames on one substrate. No lens or
electrical scanning system is capable of producing the 1011bits of informa-
tion needed 011 the surface without mechanical scanning. Additional
requirements are that the resist producing materials do not contaminate
the electron lens and that the materials he deposited on the substrate by
vacuum methods.

A. Evaporated Resists
Expcrimental work can make very good use of evaporated rcsist layers
because their thickness, as well as their chemical composition, can be
accurately determined. It has been found that silica and alumina can be
used to protect a very wide range of materials. Nearly all metals that can
be etched in chlorine can be protected by silica and the silica later removed
by hydrogen fluoride. If there is danger of contamination from silica then
alumina can be used andjater removed by phosgene or tantalum potassium
fluoride. Alumina can serve as a resist for etching silica, and silica is a n
effective resist for alumina, because phosgene does not attack silica. These
evaporated resists, which are applied through masks, are not good for
component construction requiring high resolution; however, they are very
good for studying high-resolution etching processes.
The most effective mask for etching studies is one that has a known size
and shape and is located very near the surface. These conditions are
satisfied by depositing polystyrene latex spheres on the surface to be
evaporated upon. These spheres, which are used to calibrate the niagnifica-
tion of electron microscopes, come in a variety of sizes. They range from
one micron in diameter down to 880 A, and are known in size to better
than 1%. Deposition is accomplished by simple spraying of a solution from
a nebulizer. When a resist is evaporated at an angle other than normal to
the surface, the polystyrene spheres cast a shadow of known size and
shapc. Any etching process following this now has a standard resist for
dimensions and chemical constitution. The resist has been shown to have
a definition in excess of 100 A. If a standard mask such as a screen mesh
located some distance from the surface is also used during the resist
deposition then penumbra regions will exist where the resist thickness is
changing between maximum and minimum thickness. This variety of
effects on one surface greatly accelerates the optimization of the etching
232 KENNETH R. SHOULDERS

process for a particular material and shows the various effects that can be
cxpectcd due to having a resist, layer that is too thick or too thin.
8. Chemical Decomposition Resists
When electrons bombard certain materials there is a possibility of the
material decomposing and producing a solid product that remains on the
surface near the point of decomposition. Under certain conditions this
material can be used for a resist either directly or through chemical con-
version. Haefer [67] has shown the high resolution decomposition of
hydrocarbons, silane, and borane by electrons to produce carbon, silicon,
and boron. The same reactions have been investigated by the author with
the intention of using the decomposition products as an etching resist.
Silane was admitted to a vacuum system at a pressure of mm Hg and
a thin film electron microscope specimen screen was bombarded with
1000-volt electrons at around 1 ma/cmz for several seconds. Upon exami-
nation in the electron microscope, high resolution deposits had been
formed from the various surface structures, and they could not be etched
away in chlorine. It was assumed that silicon had been produced by the
electron decomposition of silane, and that this silicon had oxidized to silica
during the transfer through air to the electron microscope. Since the silane
had been in gas form, the electron flood gun was also coated with silica;
this caused undesirable charging effects and instability of the beam. At
the low pressure of mm Hg the only highly probable reaction site for
the silane decomposition process was in the condensed phase of the
adsorbed gas a t the surface being bombarded. Material formed in the
vapor phase would be scattered widely to all surfaces.
Compounds containing oxygen can be decomposed by electron bom-
bardment, thus circumventing the oxidation step of the previous method.
Tetraethylorthosilicate is one compound that has shown reasonable results
for the micromachining of molybdenum [68]. The decomposition of this
compound probably goes through a free radical polymerization phase
immediately after bombardment; however, this high polymer decomposes
upon heating to etching temperature, leaving silica as the principal residue.
The production of silica by this method has shown a resolution in excess
of 100 A. When used as a resist for the etching of molybdenum the resolu-
tion is also in excess of 100 A. The process conditions used to produce this
resist are to admit tetraethylorthosilicate into the vacuum system at a
pressure of lo-* mm Hg and to bombard the substrate with 1000-volt
electrons at 1 ma/cm2 for about three seconds to produce a film of resist
that is 20 A thick. After exposing, the silicate vapor is turned off and the
substrate is heated to the etching temperature of about 600°C. The quan-
MICROELECTRONICS 233

t um yield of the process is over one, presumably because of the high gain
of the polymerization mechanism. Since the silicate is in vapor form
t,hroughout the vacuum system and adsorbs to the lens parts, silica is
produced and instability results, as in the case of silane.
To prevent decomposable material from reaching the lens surfaces, a
solid may be evaporated to the surface of the material to be etched. One
material that has been found useful is triphenylsilanol. This is a solid a t
room temperature that can be evaporated to a surface to produce a thin
film. The remaining material that does not go to the surface deposits on
the walls of the vacuum unit without reaching the electron lens. When a
film of triphenylsilanol is bombarded with an electron beam of 1 ma/cmz
for approximately one second, part of the deposit is polymerized. Inspec-
tion of the deposit immediately after exposure does not reveal any change,
but when the sample is heated to 200°C the unexposed material evaporates
and the exposure pattern can be seen as a deposit of material. The deposit
is largely silica, with traces of organic tars that can be driven out a t high
temperatures. This resist is the one that has been used in the demonstration
of electron beam micromachining of silicon and molybdenum, described in
Section XIV; i t is very simple to use and it forms a protective coating on
silicon for the transfer in air between the deposition chamber and the
electron microscope used for exposing.
A great many oxygen-containing organic compounds of silicon that have
low enough vapor pressure and can be evaporated without decomposition
can substitute for triphenylsilanol. In general, the higher molecular weight
materials have the lowest vapor pressure and are the most desirable.
A thin film of metal such as aluminum can be evaporated over the uii-
exposed resist layer to help confine the vapors, prevent the conversion of
the material by low velocit,y stray electrons, prevent surface charging,
and help to increase the sensitivity of the reaction by adsorption of the
primary beam; this has been shown by Sternglass [35] for transmission
type electron multipliers. After exposure, the thin metal film can be re-
moved by etching without disturbing the resist or underlying material.
Most of the polymerization type reactions and a great many of the
simple decomposition reactions caused by electrons can be classed as
contamination-prone reactions, because they contain carbon or silicon,
both of which form fairly stable compounds with metals used in electronic
devices. Unless this contamination is strictly controlled, a source for
device nonuniformity is present. Tests carried out by the author on field
emission microscope tips did not reveal any sign of contamination, but
judgment should be withheld until final components involving metal-
dielectric combinations are tested.
234 KENNETH R. SHOULDERS

C. Multilayer Resist Production Methods


In order to achieve the highest efficiency resist production, multiple
layer processes may be employed in which a current gain is obtained in the
layers. The highest yield of resist atoms possible, triggered by a single
electron for a 300 A resolution, is in the order of los; in this case, every
atom in the 300 A cube is converted by a chain process initiated by the
single electron. The highest yield that has been obtained experimentally is
around lo4.These high gain processes also have the smallest heating effects
because of the low input energy required.
A multiple layer process was tested by the author in which successive
layers of 100 A-thick aluminum, 200 A-thick lead chloride, 300 A-thick
lead sulfide, and 200 A-thick aluminum were deposited. The first aluminum
layer was to be eventually converted into a resist; the lead chloride served
to electrolytically corrode the first, aluminum layer; the lead sulfide acted
as an electron-sensitive phot,oconductor ; and the final aluminum was a n
electrode. In operation, this sandwich has about three volts applied between
the aluminum plates while a 3 kv electron beam penetrated the layers.
A local conduction path was set up in the lead sulfide by the high velocity
beam and the lead chloride was put under strong field. The resulting elec-
trolysis caused preferential chemical attack of the first aluminum layer,
which was corroded into aluminum chloride. Upon heating the entire
sandwich, the top three layers peeled off, leaving the selectively etched
aluminum; this could be oxidized or fluorinated and used for a resist. This
process had a quantum yield of about lo4.In spite of high yield the process
is not suited to resist production, primarily because there is a constant
leakage or “dark current” in the lead sulfide; this causes a background fog
that seems difficult to control. The resolution of this process was not
investigated, but it could not have been greater than 300 A because of the
electron scatter produced in the thick layers of material. This process may
be applicable to methods that expose the entire field a t once, but our
process of micromachining requires over 1000 separate exposures on the
same substrate, which makes the leakage current problem more difficult
by a factor of 1000. All reactions investigated thus far that are enhanced
by an external field common to all areas show the above leakage effect to
various degrees. There are some reactions involving tunnel emission that
look promising, but no definitive experiment has been performed. These
high field reactions have the ability to confine the reaction products to the
area of initiation because of the migration of material along the straight
field lines of the parallel plate geometry. Space charge dispersion effects
would probably be negligible a t the low current densities used.
A simpler class of reactions that is potentially more nsrful to oiir
MICROELECTRONICS 235
proc~ssis reprcscnted by anodic or corrosion reactions; hcrc a film of
metal such as aluminum is covcrcd with a film of oxidizing material like
molybdenum trioxide, mangancsc dioxidc, or silver trioxide. Molybdenum
trioxide is known to yield an oxygcn atom upon being bombarded with
clectrons and converts from the yellow form to the blue oxide. Some of
these decompositions have heen shown by Fischer [69] and Camp [70].
The oxidation of the aluminum or other base material would proceed until
the oxygcn was depleted or until the field across the oxide fell to the point
where tunnel electron emission [ll] or bombardment-induced conductivity
[71,72] could no longer be sustained. Brief tests by the author, using
aluminum and molybdenum trioxide, gave indications of being useful for
resist purposes, but have not been completely verified. It was found that
the molybdenum oxide residue could be removed by simple etching in
chlorine, apparently by forming an oxychloride. The difficulty experienced,
which was not overcome at the time, wts the removal of a thin layer of
background fog produced by thcrmal oxidation of the aluminum. If this
fog can be etched back without removing an excessive amount of the
sclectively oxidized portions of resist, this could be a clean and useful
process. In the above process an overlay of molybdenum metal would be
beneficial to cause electron multiplication, to prevent loss of oxygen and
to cause reduction of surface charging effects.
D. Compatibility with Electron Optical System
I n the type of electron optical system uscd, the samplc will be immersed
in the field of the lens instead of being shielded by an aperture, in order to
overcome part of the spherical aberration caused by using apertures, This
will require that the substrate be flat and that the surface of the resist
being exposed not charge and distort the electrical field of the lens. A
metallized covering over the resist will satisfy this requirement. I n addi-
tion, the resist material should not outgas or emit materials that would
contaminate the lens. The same metal covering also reduces this problem.
The resist-producing materials usually require only tens of volts of
electron velocity to activate them, but it is difficult to operate a high
resolution lens at lower velocities than 5000 volts because of space charge
problems and stray fields. Fortunately, a resist material can be exposed a t
any velocity above the minimum value, although at high velocities there
is a compromise in resolution because of back-scattered electrons and
increased heating effects. These effects have not yet occurred in practice.
The optimum velocity is determined by the complete absorption of the
beam energy in the resist material; however, this velocity is found to be
very low for thin films and high resolution, being only about 300 volts for
100 A resolution. A compromise velocity would seem to be about 1500
236 K E N N E T H R. SHOULDERS

volts, although it may have to be as high as 5000 volts to avoid stray fields.
High velocities have the additional disadvantage of producing X-rays
and backscattcred electrons that can expose the resist and produce fog;
for X-rays, however, this is a minor effect, becausc about one X-ray
photon is produced for lo4electrons and the absorption of the resist layer
for X-rays is fairly low.
Effective aperturing of the clcctron lens will have to be used to prevent
exposure of more than one field a t a time. This is necessary in order that
reflected primary electrons and scattering from apertures further up the
lens system will not accumulate to troublesome levels during the exposure
of 1000 fields of information.
Any tendency toward an arc-over should be detected and suppressed
before it happens; otherwise the field being exposed by the lens will be
ruined. Arc-over suppression is discussed in Section XI, A, on the Electron
Optical System.
Obtaining registration between adjacent fields and alternate layers will
require observation of the resist surface by the mirror microscope or the
scanning microscope feature of the electron optical system. The mirror
microscope has essentially zero velocity electrons a t the surface; the
scanning probe can only be as low as about 100 volts. A metallic covering
over the resist will prevent electron penetration and exposure of the resist
within certain limits of electron velocity.

XI. Electron Optical System

The present electron optical system development that is being pursued


will provide the following modes of operation with only external electrical
switching being required to go from mode to mode:
(1) Exposure of a sensitiaed substrate by a scanning probe with an
electron velocit,y between 500 volts and 30 kv a t a current density of
around 100 amp/cm2, and resolution of 200 A, with provisions for con-
version to a retinal image using a field emission source.
(2) Scanning electron microscopy with a resolution limit of around
200 A having lo6 bits per field and a scanning time variable between 60
fields per second and one field in one minute.
(3) Scanning X-ray fluorescence probe capable of detecting l O - I 4
grams of material and having a one micron resolution. The long wave-
length detectability would extend through beryllium.
(4) Electron mirror microscopy capable of measuring voltage differ-
ences to 0.2volt for a resolution of 500 A and having the capability of
measuring time-varying voltages with greater than 1000 Mc bandwidth.
MICROELECTRONICS 237

( 5 ) Field emission and thermioiiic emission microscopy with a resolu-


tion of better than 500 A, capable of studying the uniformity of multiple
field emission cathode arrays operating under ultrahigh-vacuum
conditions.
When uridertakiiig the design of such a versatile instrument it is neccs-
sary to compromise operating characteristics in some of the modes in
order to gain performance in others. The resist-exposing mode has been
optimized in the electron optical system described here and the X-ray
feature has been deemphasized. Higher resolution transmission microscopy
methods have been supplanted by front surface methods because tho
thickness of most, of our samples is too great for transmission microscopy.
In order to obtain the same quality image from one field to another, thc.
substrate must be flat, thick, and rigid. These requirements prevcnt
transmission microscopy even if very thin films are used for components.
An electrostatic imaging system was selected over a magnetic system
because of the smaller distortion and image rotation effects, the insensi-
tivity to voltage variations, and the abiIity to retain higher dimensional
stability through vacuum bakeout. A spherical electron optical system
was chosen over a cylindrical system because of the ease of fabrication
and the mechanical stability during bakeout. All outputs from the various
modes of operation have been converted to electrical form because of tho
difficulty of providing for optical paths in the system and the instability
of phosphors at, the higher bakeout temperatures.
A. Micromachining Mode
The primary function of the electron optical system is to expose images
on the substrate that can later be converted into machined shapes by
appropriate etching. I t is .desirable to ultimately use gross images for
exposing the resist producing material ; however, for simple operations,
involving only a few thousand components and their interconnections,
scanning methods will be employed because they are simpler in that thcy
do not require a pattern generator in the lens system. Simple external
equipment can be obtained commercially for generating television-like
signals to feed the deflectors of the electron optical system. Von Ardcnnc
[44a] has shown that, by using sufficiently small deflection angles and
highly corrected lenses, a scanning oscillograph can be made that has over
109 bits of information per field. The largest number of bits per field that
ronveiit ional television generators are capable of achieving is approxi-
mately lo6. Elcctroii microscopes in general have over lo8 bits prr field,
so that any information that, can bc scanned into the system will bc repro-
duced in the imaging system, provided that the aperture angles of the
system remain somewhat less than one degree.
238 KENNETH R. SHOULDERS

1. OVER-ALL DESCRIPTION

The electron optical system that is being constructed for this micro-
machining operation is shown in Fig. 25. Simple discs and cylinders of
quartz are used to produce the functions of lens electrodes deflectors, and
spacers. These quartz pieces are metallized with both highly conducting
molybdenum and high resistivity material to provide the necessary con-
ductive surface to form an electron lens. The principal components of the
system are an electron gun, condensing lens, deflectors, intermediate lens,
objrctive lens, and the necessary apertures. I n addition, there is an electron
multiplier, a micromanipulator, and a stigmator built into the objective
lens, as shown in Fig, 26. The group of parts shown in Fig. 25 and Fig. 26
is contained within a ceramic tubing that provides mechanical support
and electrical contact to the various electrodes through the sockets pro-
vided, as shown in Fig. 27. The entire assembly is covered with a magnetic
shield that has a removable top for the insertion and removal of substrates.
A molten metal seal type of varve is provided on the top of the lens en-
closure to allow sealing the lens from the vacuum system that surrounds
it during certain bakeout operations that may contaminate the lens ele-
ments or the substrate that is in the enclosure. A socket actuating mech-
anism, shown a t the bottom of the lens in Fig. 27, serves to disengage the
contact springs during the bakeout cycle and for removal of the lens parts.
All parts of the lens are made with sufficient dimensional accuracy so that
no alignment is necessary after installation, although slight electrical
adjustments are possible with the deflectors.
I n operation, the various lens components would be used as shown in
Fig. 28(a). The crossover of the electron gun could be expected to be in the
region of 0.005-inch diameter and would have to be demagnified 5000
times to reach 1 pin. diameter, or 250 A. I n order to reduce aberrations,
the objective lens must be operated a t the highest demagnification and
shortest focal length possible, while the intermediate and condenser lens
operate a t progressively less demagnification. The operation and design
of a three-lens electrostatic eIectron microscope similar to this one has
been described by Bachman and Ram0 [73]; the reader should refer t o
this reference for design details such as lens shape, aperture position and
size, dimensional accuracy requirements, and stray field consideration.
Each of the electron lenses is the three element unipotential type com-
monly found in electron microscopy. The most critical lens is the objective
lens, shown in Fig. 26, which determines the over-all resolution of the
system. This lens iriust be made with dimensional tolerances of about 20
pin. on each part in order to reduce the astigmatism to a value low enough
to achieve 200 A resolution. The principal concern is t~ form very round
i r
[ Z F E [SCREEN
SPACER APERTURE
APERTURE
I

h)
w
Y)

INTERMEDIATE LENS

‘-ELECTRODE
SPACER

I+(;. 25. I.cns voiifigwation for elertron optiral s y s t c w .


-
M u m MANIPULATOR RING

SUBSTRATE HOL ELECTRON MULTIPLIER

MICRO MANIPULATOR ANOOf


ELECTRON MULTIPLIER LEA

MICRO YbUlWLATOR GRID

LENS ELECTRODES OBJECTIVE LENS SOCKET

h) STIGMATOR SURFAC

P APERTURE CONTACT MICRO YbMPULATOR GRID

APERTURE CONTACT SPRING

ELECTROOE SPKERS

LENS SUPPORT OUTER SWPORT TUBE

SPRING RETAINER

FIG.26. Objective lens assembly for electron optird system.


i
OBJECTWE
LENS SOCKET

I
I

h)

LEL&CTRO. QUN Lcmo I


-SUBSTRATE
A M CONDEIISER LENS MFLECTOR

FIG.27. Lcns enclosurc and support structure for dectron optical system.
242 KENNETH R. SHOULDERS
holes in the lens electrodes that are concentric with the adjacent electrodes
so that the fields are uniform to a high degree. Provisions have been made
for the incorporation of an electrostatic astigmatism corrector in the
objective lens, a s shown in Fig. 26. This stigmator would consist of six
metallic stripes of molybdenum deposited on the surface of the first lens
electrode followed by a high resistance coating of material to prevent
charging by the electron beam. The electrodes would be connected through
the socket contacts to an external voltage source that could correct for
residual asymmetry in the electric fields of the lens.
The objective lenses in normal electrostatic ,instruments are apertured

ELECTRON GUN

CONDENSER LENS

STORAGE SCREEN
AN0 PPERTURE

DEFLECTOR n I

INTERMEOlATE LENS

DEFLECTOR # 2
DEFLECTOR I 3

4PLRTWlE
OBJECTIVE LENS
ELECTFION MULTIPLIER
SUBSTRATE
MlCROPROeE’ MICROPROBE MIRROR MIRROR
DEFLECTION MICROSCOPE MICROSCOPE
(0) Ibl IC) RE4D-OUT
(dl

FIQ.28. Ray diagram for various modes of operation for the electrou optical system.

on both sides so that the specimen or substrate can be located out of the
field; however, Liebmann [74] has shown that the apertures cause a n
increase in spherical aberration that is very undesirable. Newberry [75]
has immersed the specimen or target of an X-ray projection microscope in
the field of the lens and avoided the exit aperture, thus giving an increased
performance. This ttype of operation is possible with our application and
will be used to help improve the lens performance. The entrance aperture
is located as far as possible from the high field region of the lens in order
to reduce the effect of the aperture. With this immersed type of operation
the final lens electrodes, formed by the electron multiplier discs, are oper-
ated near the substrate potential, while the center lens electrode is operated
MICROELECTRONICS 243
near cathode potential a i d is used to focus the electrons on the substrate
by varying the voltage slightly.
2. OBJECTIVE L E K S DESIGN

The cscellence of the objective lcns is determined by its focal length,


which is in turn deterniiiied by the field strength of the lens. The largest
aberration term that limits the performance of a lens is spherical aberra-
tion, which can be reduced by reducing the focal length. When the limit
in focal length is attained the maximum aperture angle to the lens can be
determined, knowing the resolution desired, and the efficiency of the lens
is determined. The lens shown in Fig. 26 is designed for a minimum focal
length of 4 mm, using the 0.040-inch-thick electrodes shown; however,
provisions have been made to operate with conical shaped lens elements
having closer spacings and higher fields to obtain a focal length as short a s
2 nim, while still retaining the center electrode near cathode potential.
All of the electrodes of the lens system arc interchangeable and the hole
size can be conveniently altered. A focal lcngth of 4 nim is considered
adequate for our purposes; a t this focal length, a spot of 200 A diameter
can be focused having a current densit,y of about, 100 amp/cm2.
Electrostatic lens systems have shown excellent results in the past in the
hands of experienced operators, but all commercial attempts so far have
been unsuccessful because of contamination problems. Our utilization of
ultrahigh vacuum makes the electrostatic lens performance high because
the field strength of the lens can be increased about one order of magnitude
past the nornially allowed valucs of lo5 volt/cm. In order to operate in the
region of lo6 volt/cm, the surfaces of thc lcns exposed to the high field
must be very smooth, have high nork function, and be free of dielectric
films that could cause Malter effect eniissioii arid the ensuing arc-over that
this form of field emission produccs. Tests have been carried out by the
author on molybdenum-coated quartz lens elements in which the field was
increased to lo8 volt/cm without breakdonn, provided the surfaces were
cleaned by high temperature processing in vacuum. The ceramic base
material used in thesr lcns coiifiguralions havc lowcr thermal conductivity
than metal electrodes and they arc more prow to be destroyed by a n elec-
t rical discharge. The discharge rcnioves a port ion of the metallizing,
requiring refinishing of the c~lcctrodes.Elaborate protection methods seem
in order to protect both the lens elements and the substrate during expos-
ing. These methods could consist of slowly raising the voltage while
nionitoring the current to the various electrodrs in a n effort to sense the
onset of field eniissioii, which invariably preccdcs the discharge. If field
emission is detected, it can usually be rcmoved by exposing the source to
a very low chlorine prwsure. This operation would have to be followed by
244 KENNETH R. SHOULDERS
another bakeout. Coiisidering that the above cycle would not have to be
done more than once a day, or whenever the lens system was opened to air
and contaminated by dust, this half-hour procedure may be worthwhile
if ultimate performance is required.
3. PATTERN QE7XERATION

The deflection of the microprobe would be acconiplished as shown in


Fig. 28(b); the aperture is used as a fulcrum point in order to prevent a
severe limitation of the field of view by the aperture. The deflectors are
quartz cylinders that have four equally spaced metallized stripes on the
inside with a high resistance uniform coating applied over-all. This type
of deflection system produces strong coupling between t.he deflection
plates and gives nonuniform deflecting fields, but these effects can be
removed by fairly simple external circuitry. The deflection angles are
normally less than one degree and linear deflection amplifiers are not diffi-
cult to secure. Only about lo6bits per field will be obtained with the scan-
ning type of data input. The 100 amp/cm2 probe would be distributed
over lo6 200 A diameter spots having a field size of 20 X 20 microns for
aii average current density of amp/cm2. An exposure time of about
10 sec would be required under these conditions. The deflection signals
can be derived from a commercial high definition flying spot scanner
apparatus, the video output feeding the grid of the electron gun. Ordinary
drawings are adequate for the information source.
Had a gross image of los bits of information been used, the exposure
time would have been decreased by lo6or the current density requirement
reduced by the same factor.
4. MICROMANIPULATOR

The micromanipulator shown in Fig. 26 is designed to move various


portions of the substrate into the field of view of the lens by using a n
electrically operated, thermal, bimetal motor. The micromanipulator
anode is made from a bimetal of molybdenum and nickel and is heated by
electron bombardment from a triode gun assembly machined into the
ceramic contact support structure. By operating four diametrically opposed
thermal motors and one locking device, the substrate can be progressively
stepped to any position allowed by the limits of the system. The smallest
increment of motion would be about 100 A and the longest continuous
motion would be about 0.01 inches. Forty of the 0.01-inch steps would be
needed to cross the 0.4-inch substrate shown in Fig. 26. After arriving a t
any chosen position, the substrate is prevented from further movement
by the friction locking of the system. All bimetal motors are disengaged
MICROELECTRONICS 245
from thc lockcd subbtratc, so that their drift does not disturb thc sctting.
The timc constants of the thcrinal motors are sufficient to allow crossing
from one side of the substrate to the other in approximately onc niinutc.
In addition to the micromanipulator, thc substratc can bc positioned
quickly to within 0.01 inch of any chosen position by an external mechan-
ical manipulator that is used to exchange substrates and remove them to
the deposition and etching positions in the apparatus. The vacuum seal
in the top of the electron optical system and the magnetic shield cap shown
in Fig. 27 must be removed during the use of this external manipulator.
5. MAGNETIC SHIELDIYG

The electron vclocity of an electrostatic lens system can be varied


without affecting the focus or rotating the image, provided all voltages to
t!he various lens elements are varied proportionally. The electron velocity
that seems most likely to be used for resist exposing is in the 3000-volt
region. Higher velocities result in uiiwanted heating and back-scattered
electron effects, and lower velocities are subject to stray magnetic field
disturbances. If the triple shielding shown in Fig. 27 is as effective as
planned, and if there is no deterioration of the shielding with successive
vacuum bakeouts, then t8he voltage could be reduced to the 500-volt
region without destroying the 200 A resolution or causing drift and distor-
tion of the images by stray magnetic fields.
6. REGISTRATION

The problem of obtainiiig registration between adjacent fields and


between adjacent layers can be divided into two problems; namely, locating
the area that must be fitted, and then providing identical frame size and
shape for the two fields that must be registered. The first problem can be
ultimately handled by using precise optical interference locating methods.
With thcse methods, a one-inch substrate can be positioned to within
one-hundredth of a wavelength of light, or about 50 A. For the present,
however, simpler methods, giving poorer results, will be used by taking
advantage of the electron microscope and X-ray feature of the elect,rori
lens. These methods will be discussed in a later section. The most difficultj
part of the registration problem is to obtain two images a t different times
that have the same distortion and size. A drift in external circuitry or the
mechanical featurcs of the lens will result in many divcrsc effects which
are difficult to cornpensatc.
A commcrcial electron niicroscope has sufficient stabilit,y to expose an
image showing a resolution of better than 8 A in a n exposure time of up to
one minute without the image being blurred by drift of either external
246 KENNETH R. SHOULDERS

clectrical circuits or i i i t c n d mcchaiiics. The same i1ii:ige c:m be exposcd


a t some later time on the same photographic plate and it will be found
Ihat the drift is usually lcss than 50 A over a pcriod of two days, provided
the instrument is left in operating condition and had been properly sta-
bilized before the first exposure. The beam current must also be turned off
during this period or the contamination that results from the poor vacuum
and the many rubber scals will contaminate the apertures severely and
distort the image badly. When the instrument is shut down completely
and then turned on at some later time and allowed to stabilize the drift
can be very great, in some cases amounting to over 5000 A. The most
difficult problem in stability is apparently caused by the many mechanical
joints in the massive lens column. We have endeavored to design a sturdy
mechanical system that is not massive by incorporating rigid quartz and
ceramic pieces in an assembly that has high dimensional tolerances so as
to prevent inadvertent motion of critical parts. In addition, the thermal
expansion and material creep for these quartz lens elements is much lower
than for metal elements.
By using highly stable mechanical structures to prevent mechanical
motion, and ultrahigh vacuum to prevent contamination and the attendant
charging effects, and by being very careful to provide slightly conductive
surfaces on all dielectrics exposed to the electron beam, it is hoped that we
will achieve a long-time stability of better than 500 A in both distortion
and drift of field so that this part of the registration problem can be made
approximately equal to the resolution of locating the field to be registered
upon.
B. Scanning Electron Microscope
A scanning elcctron microscope can be made by using the lens configura-
tion shown in Figs. 28(a) and 28(b) in conjunction with an external
monitor and sweep generator similar to a television monitor. The output
from the electron multiplier would feed the brightness axis of the monitor
and the sweeps of the monitor and the microscope would be synchronized.
Comlett and Duncumb [76] and Everhart et at. [77] have shown their results
using scanning microscope methods. One important conclusion is that not
only geometrical properties of the surface appear, but that differences in
materials can be distinguished, as can the electrical characteristics of
devices. The specific samples shown by Everhart were back-biased p-n
junctions of germanium and p-n-p junctions of gallium phosphide. A de-
cided change in image contrast resulted by altering the potentials applied
to the junctions: base regions of less than 0.2 micron could be seen and
variations of this width were apparent for various positions along the
junction, a difficult thing to determine by any other nondestructive method.
MICROELECTRONICS 247

1. I1EGISTHATION
TLc principal w e for the scanning electron microscope in the niicro-
~nachiningprocess would be to determine the location of the registration
inarks on the underlying layers of inaterial that have beeii previously
machined. These indicating marks will be covered by a smoothing layer,
a deposited film to be machined, and a resist layer, but the pattern of the
underlying film would not be completely obscured because of the sensitivity
of the xanning microscope to slight surface angle changes such as those
produced during a surface smoothing operation. A vacuum cavity has
been teen t o cause a slight depression at the surface, amounting to as ~nucli
as 400 A for a one micron diameter cavity. The scanning niicroscope would
in effect see a relief image of the underlying layer and registration could
tie cfectcd by electrical servo-ing of the beam without exposing the resist,
provided low elect ron velocities were used that could not penetrate the
oiwlying nietal film. When registrat ion was secured, the beam velocity
could be increased for the exposure without greatly altering the registration.
2. SZ'HF.4CE INSPECTIOS

The scanning electron microscope can serve as an inspection tool for the
cleanliness and smoothness of the subst rates. Slight imperfections on the
surface would be seen as either dark or light areas in which the average
secondary eniission value was altered by the shape of the anomaly. External
clipping circuits could be adjusted so as to indicate a fault on the surface
as t k x surface was scanned both electrically and mechanically. When an
asperity was found, the operator could determine the best action to be
taken .
The contrast-producing mechanism for this type of niicroscopy is
partly due to having anisotropic electron collection and partly due to
celecting the proper velocity of the secondary electrons emitted from the
surface. To perform these operations, the electron multiplier input poten-
tial must be adjustable, and some method of determining the polar angle
of emission of the electron from the surface must be provided.
3. ELEC'TROS MT'LTIPLIER

The electron multiplier shown in the ohjective lens in Fig. 26 and in


cspanded form in Fig. 29 would seem to fulfill our need. There is a require-
ment €or a completely symmetrical field around the input dynode of the
multiplier because it forms part of the lens structure, but once the electrons
Iiave entered the region qf the fourth dynode axially unsymmetrical fields
can 1;c considered. In order to provide for some degree of anisotropy for
clcctroii collection, four anodes will l x provided and the one giving the
I I

h)
.s
OD

PRIYARV
ELECTRONS
FLY

FIG.29. Electron miiltiplier and X-ray detector.


MICROELECTRONICS 249
greatest contrast will bc selectcd for the prcsentation on the monitor. The
symmetrical rings or dynodes opcrating at the same potential will tend to
spoil the angular resolvability of the emit tcd electrons, but enough may
remain for our purposes.
The collection potential for the sccondary clectrons can he varied be-
tween several hundred volts positive with respect to the substrate target
and several hundred volts more negative than the cathode potential. As
shown by Evcrhart et al. [77], the contrast of various specimens depends
upon which range of secondary electron velocities are selected to be used
on the viewing monitor, the high-energy elastic primaries giving a different
contrast than the low-energy secondaries.
The electron multiplier will be made from quartz lens discs that have
been ground so as to produce concentric grooves with the shape shown in
Fig. 29, although a geometry using only smooth parallel plates has been
postulated and may prove satisfactory. These blanks are metallized with a
high resistivity coating to provide the voltage divider action needed for
the various dynodes. The high resistivity coating that has been tested for
this purpose is a cermet of tantalum-molybdenum and aluminum oxide,
applied by evaporation and then heated to above 1000°C in vacuum. The
stability of this coating is good over a long period of time and is not partic-
ularly affected by repeated temperature cycles up to 9OO"C, the vacuum
bakeout temperature. The temperature coefficient of resistivity of this
material is high, but in our application this is not troublesome because of
the constant opcrating temperature. The temperature in the neighborhood
of the lens must be maintained nearly constant for the stable operation of
the electron lens. A sccondary emission coating of silica, tantalum, and
beryllium, as described by Mendenhall [78] seems suited to our applica-
tion, since high temperature cycling tests by the author and repeated
exposure to air have failed to show appreciable change in operating char-
acteristics. These coatings would be evaporated onto the electron multiplier
surface using the shadowing effect of the dynodes that were machined into
the quartz discs. The secondary emission coating is thus broken up into
concentric bands with resistance material connecting them. I n order to
provide a constant voltage drop between dynodes, the resistance material
must be made thinner on the rings having the greatest diameter and area.
By application of 100 volts per dynode the gain of the multiplier should be
sufficient to detect single electrons in the input and produce a one-tenth
volt output for a one-megacycle bandwidth.
C. Scanning X-Ray Fluorescence Probe
Cosslett and Duncumb [76] and Duncumb [79] have shown a scanning
electron microscope and scanning X-ray fluorescence probe combined into
250 KENNETH R. SHOULDERS

one instrumcnt that allows the examination of a solid surface by micro-


scopy, and the chemical analysis of the same surface by X-ray methods.
The instrument we are constructing should serve a similar purpose, but
the X-ray feature can be broken down into two modes of operation that
are primarily a function of the X-ray detectors used. For high geometric
resolution work that would not have high resolution for discriminating
between chemical elements, a proportional pulse height detector would be
used by biasing the electron multiplier to electron cutoff in the input and
making it sensitive to X-rays. The pulse height output from the multiplier
would give an indication as to the wavelength of the incoming X-ray
photon and consequently the chemical element involved. For a more
definite chemical analysis the substrate would have to be raised from the
lens enclosure to a position that would allow the collection of X-rays on
a crystal spectrometer and X-ray detector. This latter mode is not being
planned for the immediate future although provisions have been made to
incorporate it at a later date.
1. X-RAY DETECTOR

An electron multiplier can be made to serve as an X-ray or a high energy


particle detector with some wavelength discriminating ability. Bay [80]
has shown some of the limits of this method. One of the biggest problems
is that monochromatic radiation does not produce uniform output pulses
because the electron multiplier gain varies from pulse to pulse, resulting
from the electrons taking different paths through the multiplier. For
single electron or photon inputs, a statistical distribution of pulse heights
occurs. By providing the proper type of detector surface on the first dynode
of the multiplier it is hoped to achieve enough discrimination between
adjacent atomic numbers to allow detection of 10% of one material in the
other by averaging the various pulse heights over many counts. The
quantum efficiency of tantalum multiplier surfaces has been shown by
Allen [81] to be abo6t one electron per 500 photons in the energy range
between 0.2 A and 1.0 A, with the highest efficiency for the long wave-
length photon. The limit of detectability for long wavelength photons is
known to extend to the visible light region for electron multipliers, provided
that no absorbing material is introduced between the source and the
detector. Since we are concerned only with a nonabsorbing vacuum path,
as shown in Fig. 29, the wavelength limit is essentially negligible. By using
the X-ray absorption filtering action of various films of material on the
detector surface and choosing the optimum electron velocity to excite the
desired characteristic radiation, the multiplier type of detector may be
adequate for routine chemical analysis of the materials at the surface, but
the more desirable method would certainly be the use of a crystal spec-
MICROELECTRONICS 251

trometer. When proper operation of an X-ray fluorescence probe is attained


a quantitative analysis on 10-13 grams of material is possible with a n
accuracy of 1% [57].
2. USE O F X-RAY PROBE

The principal use for the X-ray rnicroprobe in the micromachining


process, aside from the film thickness determinations, is in checking for
registration with very deep layers of material. This can be done b y first
locating the general area with scanning electron microscopy and then
raising the velocity to around 30 kv and penetrating the films in one
selected spot that is expected to show the buried registration mark. This
will expose the resist, but if an unused area is selected there will be no
difficulty. The error signal developed by this scanning probe could be
used to restandardize the top layer being exposed in t,he event that there
has been a gradual shift of previous layers.
D. Mirror Microscope
A mirror microscope can be formed by using the lens configuration
shown in Fig. 28(r). The substrate is illuminated with a flood electron
beam from the electron gun. The substrate is held a t a potential slightly
negative with respect to the cathode and electrons arc reflected from the
surface, imaged through the objective and intermediate lens, and strike
the storage mreen a t high velocity. The storage screen had previously
been charged by a scanning electron beam that traversed the No. 1 de-
flector twice and was mirrored from the intermediate lens, as shown in
Fig. 28(cl). The scanning beam is syiichroiiized with an external monitor
scope and the signal currents derived from charging the screen are used to
modulate the brightness axis. When the storage screen is fully charged by
scanning, no output image results; however, the high velocity electrons
mirrored from the substrate cause bombardment-induced conductivity in
the screen dielectric, and the screen is selectively discharged and a pattern
can be scanned out to the monitor. The process of bombardment-induced
conductivity has been described by Pensnk [71] and Ansbacher [72] and
has been shown to bc effective for duminum oxide, thr dielectric to be
used on this storage wrreri. An undrrlyirig signal elrrtrodc of molybdeiium
will be used.
1. STATIC OBSEIlVATIOPiS

The performance of the mirror microscope for some applications has


heen described by Bartz et nl. [82] and Mayer [83]. This instrument is
particularly useful for front surface microscopy in which the electrons do
not stxikc the surface. In particular, the instrument has been used to
252 KENNETH R. SHOULDERS

measure resistivity, contact potential, voltage variations across a surface,


and magnetic field distribution. Our principal use will be in the determina-
tion of the electrical characteristics of finished devices. If a single compo-
nent is centered in the field of view of the microscope, the voltage on the
various electrodes can be determined to an accuracy of about 0.2 volt by
biasing the entire component near the cathode potential for the mirror
microscope. The velocity distribution of the emitted electrons from the
microscope cathode prevents more accurate determination of voltage
without undue complexity.
2. DYNAMIC OBSERVATIONS

If the entire field of view is ceiitered on a single electrode of the compo-


nent under investigation, and this field is imaged to a spot on the storage
screen while the No. 1 deflectors are fed with a sweep signal that is syn-
chronized with the input signal to the component, a micro-oscilloscope
would result which allows time varying voltage waveforms of the compo-
nent to be shown as an intensity modulation on the external monitor.
The bandwidth of this method would be limited by the brightness obtain-
able on the screen and the transit time of the electrons near the mirror
surface. The brightness is governed by the current density a t the surface
and the gain of the bombardment-induced conductivity mechanism in the
storage screen, while the transit time is governed by the field strength of
the objective lens. A frequency response of over 1000 Mc seems possible
with the electron optical design that is under construction; the quantum
limit of detectability for the system would be about 10" cps for an imaging
efficiency of 1% in the electron optical system. This limit could be over-
come by using over lo3 amp/cm2 for the illuminating beam, but such a
high current density beam could interfere with either the component being
observed or adjacent components. A field intensity of lo6 volt/cm could
be used in the objective lens region, giving a transit time of about 10-8 sec
for electrons over the full 6 mm path without seriously disturbing the
components. The transit time lag and spread during the final few microns
of deceleration where the contrast is developed would be several orders
of magnitude less.
The ideal way of using the mirror microscope to study component oper-
ation would be to encapsulate the components; shield them with a metallic
layer, and bring out lead wires to the surface for the mirror microscope to
view without interference from either the strong field or the stray electrons.
The input signals to the various components would normally be fed in by
connecting lead wires but it would be possible to use the electron probe to
operate the components under some conditions. The most satisfactory
method of testing would be t,o have an array of components interconnected
MICROELECTRONICS 253
ill sonic fashion similar to a divider, and rapidly pulse the input with an
rlectron beam whilc Observing the output of the divider a t frequent,
intervals with the mirror microscope.
E. Multiple-Cathode Field-Emission Microscope
By using the mirror microscope connection but leaving the illuminating
beam off, the electron optical system can become an emission microscope
capable of observing the behavior of a large array of field emission cathodes.
For this type of operation the objective lens electrode nearest the substrate
would be operated a few hundred volts positive relative to the substrate,
or just a few volts below the emission point, and the center electrode would
be operated a t a higher positive voltage in order to draw emission current
from the substrate in an area that is centered over the lens opening, and
to converge the emitted electrons into a focused beam. Thermally emitted
clectrons can also be imaged with this system provided that the substrate
does not have to be heated above 900°C. The heating mechanism would be
by electron bombardment of the substrate from the rear, and the resolution
of the system would suffer from mechanical instabilities.
The principal use of the emission microscope mode of operation would
be to help optimize the multiple cathode formation processes and to allow
direct inspection of the cathode surfaces after and during accelerated life
testing cycles and therefore help optimize their performance. It is not,
expected that the detailed emission characteristics of each emitting area
could be resolved, but rather that the location and intensity of each of the
areas could be seen with a resolution of approximately 300 A. The behavior
of each of the emitting areas could be studied under ultrahigh vacuum
conditions of approximately mni Hg. Slow temperature cycles and
prolonged heating up to a maximum of 900°C could be done while observing
the emitting surface, with some sacrifice in resolution due to the thermal
instability of the microscope. Using smaller substrates than the normal
0.4 X 0.4 inches, the temperature could be raised to the 1500°C maximum
allowed 1)y the insulating substrate material provided electrical connec-
tions were simple and did not result in a field across the dielectric. Emission
from complex surfaces involving both emitter surfaces and grid structures
could be imaged in the electron optical system without supplying the
necessary fields from the external lens electrodes. Complete structures
using cathodes, grids, and anodes could be viewed provided that the anode
is a thin film of metal partly transparent to clectrons in the multiple layer
type of tunnel effect device, or that the encapsulating layer is left off on
the single layer device and some small fraction of the total emission escapes
from the various surfaces in the form of field emitted primary electrons,
elastic primaries, or secondary electrons.
254 KENNETH R. SHOULDERS

F. Pattern Generator
'l'o carry out iiiicroinuchiiiiIig of complex pattcriis on a surface by elec-
tron beam techniques, a pattern generator is required. This generator can
vary in complexit,y from a simple flying spot scanner reading a drawing, to
a complete computer of large complexity connected to the formation
chamber in such a way that it monitors the operation and adjusts the
processes to converge the operations to some useful end. The simplest
methods will suffice for some time, but more complicated methods will be
mentioned to indicate ultimate limitations.
1. SCANNING SPOT

Using a single spot of electrons and deflecting it to various locations to


expose the resist can be done by using commercial flying spot scanners
having approximately lo6bits per field. For this requirement the field rate
or the frame rate is not important provided the exposure time can be
adjusted by some means. It would be desirable to have the frame rate just
equal to the exposure time so that the pattern would be traced over once
only. The exposure time for a scanning probe operating a t 100 amp/cm2
would be about 10 sec for the simplest type of resist having low sensitivity.
This low scanning rate requires that the frequency response of the deflec-
tion and video amplifiers extend to dc, a requirement which is not usually
met with commercial television equipment. Lower exposures would be
accommodated by lowering the intensity of the electron beam when it was
gated on. Only two levels of video voltage seem necessary for any pattern
considered. Using the lo6 bits of information provided in a single field of
scan, approximately 1000 tunnel effect components could be constructed
without including their interconnecting wires. Only about 250 components
per field could be constructed if the wires were included. The simple scan-
ning spot is a very poor method of conveying information to tjhe surface
of the substrate.
2. PATTERN SCANNING

The previous scanning spot method can be improved greatly if instead


of scanning a simple spot, the spot contains fine detail. If an image of the
tunnel effect device is formed by passing the electron beam through a mask
and then this image is deeected to some desired location, an improvement
of lo3results over the simple scanning spot method, if there are effectively
lo3 spots in the component structure. By applying analog deflection
methods to the image of the field emission component and stepping this
image from position to position, an array of components could be situated
on the surface without interconnecting wires. By demagnifying the image
MICROELECTRONICS 255
of the coniponeiils, and consequently defocusiiig it, a scanning spot would
be obtained for describing the locat ion of the interconnecting wires. Because
of the drift in analog deflection amplifiers, one cannot make use of the full
resolving power of the electron optical system, a limit is reached-some-
where not too far past 10’ bits per field-in which amplifier drift and
instability cannot be easily reduced, although t here are methods employing
a multiplicity of deflection plates and accurately clamped binary inputs
that avoid this problem.
A complete rctirinl field can bc stepped froni position to position by
staircase sweep signals obtaiiicd from htable dc sources and inechanical
(*oiitacts, provided the relatively slow s w c p rates can be tolerated. To
compensate for relatively slow accurate staircase siveeps, it is necessary to
increase the number of bits per field in the electron beam pattern that is
to be deflected. Mechanical commutation nicthods can generate up to lo4
well defined steps of voltage per second and mechanical masks to define
the beam pattern can have over lo5 resolvable elements in a square inch.
13y using this iterative method of producing parallel images, a pattern rate
of lo9 bits per second could be generated. This system would be strongly
constrained by the inflexibility of the mechanical apparatus and arbitrary
pattcrns could not be generated; however, as many as lo5completely wired
Components could be secured by this method in each field of data presented
to the lens.
3. FlELD EMlSSlON SOURCE

An ultimate pattern generator for the production of around lo5 com-


pletely wired components per field by entirely electronic means could be
made by employing simple scanning techniques and other interim methods
to generate a mosaic of field emission cathodes, grids, and interconnecting
wires that could be used as an elect,ron source. Each emitting area would
have to have a memory associated with it so that data could be serially
stepped into the mosaic from the controlling computer and then used for
processing in parallel fashion. The grid structures associated with the field
emission sources could serve to regulate the emitted current, to converge
the electrons to match the aperture angle of the electron optical system,
and t o gate the proper areas to obtain emission. If complete pattern
flexibility were desired, there would have to be lo8 individual areas for
emission, and if the components were around one micron diameter the
entire array would occupy one square inch of area. The position of the
patiern generator in the electron optical system would be in the place now
hhown for the storage screen in Fig. 25, arid the intermediate and objective
kns would serve t o demagnify the image formed. Various simplifying
configurations for the emitting source could be worked out employing
256 KENNETH R. SHOULDERS

combinations of simple accurate deflections and complex patterns or by


building in constraints; however, no serious effort need be put on these
problems for some timr.
G. Construction Details
The construction problems on this electron optical system can be broken
down into two major categories, namely, the fabrication of metallized discs
and cylinders for the lens elements, and the fabrication of a mechanical
support for the lens elements that also provides for electrical connection
to the various electrodes. Ceramic materials have been selected for the
principal construction materials because of their high dimensional stability
a t elevated temperatures and because of the ease of obtaining the forty
insulated lead wire coiinections to the various electrodes. High alumina
ceramic and fused quartz are the materials that will be used on the first
lens design, with provisions being made to substitute sapphire for the fused
quartz in the event that, suitable dimrnsioiial stability is not obtained.
1. LENS ELEMEKT CONSTRUCTlON

The lens elements for a typical lens such as the objective lens are shown
in Fig. 30. The discs and cylinders are made by grinding and polishing
fused quartz blanks to the desired shapes by standard optical lens grinding
techniques. After rough grinding, the blanks are fired in high vacuum to a
temperature of around 1000°C to relieve strains and show flaws that are
not easily seen in the raw material. The parts are rotated a t low speed in
a machine with an accurate spindle while a polishing tool generates the
round and concentric surfaces. The final operation puts a chamfer of small
radius on the edge of the holes, The dimensions of the parts are checked
periodically by using optical interference techniques that are accurate to
within 5 pin. or better. This measuring technique consists of viewing the
surface with an optical microscope through an optically polished surface
that is held very close to the surface being measured. Interference fringes
result and they can be interpreted to show the roundness of the outside or
the inside surface. If both surfaces are sufficiently round and concentric
with the mounting shaft they can be considered round and concentric
with each other.
When the three principal lens electrodes itre assembled in the lens sleeve
the alignment and concentricities of their center holes must be accurate to
within about 50 pin. This is obtained by controlling the inside diameter
and roundness of the leiis sleeve and the outside diameter of the lens elec-
trodes to within 20 microinchcs. Matched parts can be selected for the
objective lens while the intermediate lens and condenser lens can make
use of the parts made to lower tolerances.
MICROELECTRONICS 257

FIG.30. Photograph of lens electrodes, sp:iwrs, sleeves, and support+

All lens electrodes aiid spacers are in:& optically flat, top and bottom,
to within 20 pin. and the two surfacth :we parallel to within 40 pin., so
that the parallelisrn of the electrodes is quit(. wit,hiii the tolerance required.
The discs are easy to inalcc fiat niid p:~r:dlcl. but long cylinders used as
spacers are a good deal more difficult.
Finished discs have been fired in a v ~ ~ c u u furiiaw
ni t o 900°C to siinulatc.
258 KENNETH R. SHOULDERS

vacuum bakeout conditions, without, evidence of sag, creep, or decomposi-


tion. The tests were made by supporting an optical flat, having the same
dimensions as a lens electrode, at three points while firing and then check-
ing the optical interference pattern after firing. It was noted that the
dimensions were within 20 microinches of the original shape after firing.
The surface was examined for alterations to the surface polish, but a
magnification of 400 failed to show any recrystallization or devitrification.
A metallized sample also appeared to be unaffected by the firing. The
metallizing used was molybdenum applied by vacuum evaporation.
The electron multiplier will be machined out of standard thickness lens
electrodes by using a high speed grinding and polishing tool a t an off-axis
angle to produce the slight overhang that is shown in Fig. 29-an overhang
that is needed for the self-shadowing of the evaporated secondary emission
coating. These concentric grooves do not need to be very accurate, provided
the first and second dynodes are concentric with the inside diameter of the
electron multiplier electrodes.
The large apertures in the system will be made from fused quartz discs
with various sized holes in the center. The objective lens aperture will be
made by bonding a molybdenum disc having a very small hole in it to a
sapphire or an alumina aperture disc; it is difficult to bond molybdenum
discs to fused quartz because of the large difference in thermal expansion
coefficients.
The electron-bombardment-heated evaporator discussed in Sectioii
VIII, A on Material Deposition has been used to metallize quartz plateh
with molybdenum. It is desirable to deposit the molybdenum a t a tempera-
ture of around 600°C after a heating to 900°C for cleaning purposes. The
heating of thc substrate was done by bombarding with electrons on the
reverse side from the evaporator. A mask of alumina is used to delineate
the deposition pattern. In order to deposit an adequate quantity of material
in the holes of the lens electrodes the disc is rotated a t an angle of about 45"
to the evaporator so as to deposit material on the straight sides. The
deposition pattern is arranged to provide a contact electrode on the outside
diameter of the electrode discs. These coatings of molyhdenuin are very
hard and cannot be scratched by the tungsten wires that are used for
contacts unless excessively high pressure is used.
Prelimiiiary tests on the welding and sticking characteristics of the close
fitting parts after heating in high vacuum indicate that there will not be
a great deal of difficulty in removing the parts from the assembly. I n the
event sticking does occur the silica surfaces will be coated with alumina by
evaporation in order to reduce the affinity for the adjacent molybdenum
film. Alumina has been successfully evaporated from the same type of
evaporator that is used for the molybdenum evaporation.
MICROELECTRONICS 259

2. MECHANICAL SUI’PO IWS

A series of support tubes, shown in Figs. 26 and 27, are used to constrain
the various lens elements and provide alignment without the need for
adjustments. The inner support tube shown in Fig. 26 is made from high
alumina and is honed to a dimensional tolerance of 0.0005 inch on the
inside diameter and 0.0005 inch cantilever distortion over the entire length.
This provides the principal guide for the various lens supports and spacers.
Clearance holes are ultrasonically drilled in the inner support tube to allow
contact springs to engage the contact pins or other electrodes of the lens
parts. These holes, along with other intentionally introduced holes, provide
the paths needed to pump out the interior of the lens without pulling the
gas through the lens apertures.
The outer support structure is made from a group of alumina cylinders
that are metallized and brazed together to form a vacuum-tight envelope.
Both ends of the enclosure are sealed with molten metal type valves, the
top one being opened and closed during a bakeout cycle of the ultrahigh-
vacuum apparat,us. The lens must be closed whenever there is a possibility
of corrosive residue from an etching or deposition cycle contaminating the
lens. An external manipulator removes the cover and the substrate after
the seal-breaking heater is operated.
The various sockets for the lens assemblies and the deflectors are simple
alumina cylinders with metallized lead wires carried through the walls; the
inside surface of the cylinders is ground smooth. The contact springs
shown in Fig. 26 float in the spring-retaining collars and serve to connect
the lead wires with the electrodes when the lens assembly is pushed into
the proper position by the socket-actuating mechanism shown in Fig. 27.
Tungsten springs fired a t 1350°C in high vacuum have been tested and
found satisfactory for the limited travel required on the contact spring.
These springs must not be under compression during high temperature
bakeout; this is accomplished by disengaging the socket mechanism. The
entire inner support tube, contact spring retaining collars, and lens ele-
ments can be removed from the main outer support having the many lead
wires by simply disengaging the socket mechanism and lifting the assembly
out. The lens elements can be removed in a similar fashion from the inner
support tube by pulling three retainer pins. This easy accessibility will be
very convenient during the testing phase of the electron optical system.
Low temperature metallizing processes will be used for the lead wires
and the joining of the various ceramic parts in the support structure.
Alloys of zirconium, nickel, and titanium will be used. A special vacuum
furnace has been constructed capable of reaching 1300°C and this will be
used for all brazing and metallizing operations.
260 KENNETH R. SHOULDERS

XII. High-Vacuum Apparatus

A. Requirements
High-vacuum apparatus is required that is large enough to contain the
deposition apparatus, etching apparatus, electron optical system, and
substrate storage and manipulation apparatus. Since most of the proofs
in this work are generated experimentally, the access time to the high-
vacuum system must be short in order to allow rapid progress to be made,
and several cycles a day must be provided for.
The degree of vacuum that must be obtained for scientific results is in
the region of 10-'0 mm Hg, although many operations can be carried out
in much poorer vacuum if variations in results can be tolerated in order to
quickly survey a range of problems. Even though the pressure in the
deposition and etching cycles rises to around 10-4 mm Hg the background
pressure or partial pressure of contaminants must be kept in the
mm Hg region to insure pure deposits. This low background pressure
requirement, coupled with a high speed vacuum requirement,, dictate high
bakeout temperatures and a short time constant for the bakeout furnace.
By introducing many high vapor pressure chemicals into the vacuum
chamber we have further increased the need for periodic thermal purging
of the residue to prevent contamination of subsequent operations, and in
one configuration of apparatus the system would have to be baked out
every five minutes. If any cold areas are left in the apparatus the chemical
residue will deposit on this site and raise the background pressure during
following operations. It has been determined that all troublesome mate-
rials can be driven from the system if a bakeout temperature of 900°C is
used, and that vacuum locks can be placed between chambers when it is
desirable to heat one without the danger of condensing material in the
other. Fast thermal time constants have been provided by using very light
construction materials and heaters contained in the vacuum system so that
they do not have to use thermally maesive insulation.
By using differential pumping methods the construction materials for
the inner vacuum system can be kept as light as required for simple
mechanical support instead of having to support an atmosphere of pressure.
I n addition, the many manipulator lead-ins to the system can be introduced
more easily in regard to leaks in the ultrahigh-vacuum system. An addi-
tional advantage of differential pumping is that all of the parts that are
heated are heated in a vacuum of mm Hg where corrosion and gas
permeability of the container are very minor factors.
The vacuum system and ultrahigh-vacuum attachment that is described
here is a complex and expensive piece of appara tus, but this can be tolerated
MICROELECTRONICS 261

if it proves to hc the foundation apparatus for 5 coi-nplcte factory that can


be used to economically construct high complexity electronic data proc-
essing equipment. There are two stages in the development of the vacuum
equipment. The first phase, to be described here, is essentially a large
single container or bell jar that houses all apparatus and has a single
heater for the various bakeouts. I<veiitually, in a later phase, the apparatus
will be reassembled using the same components-such as pumps, heater
designs, vacuum locks, manipulators, and valvcs-into a linear apparatus
dcsign in which the lens, deposition, and etching apparatus are suspended
on the lower side of a manifold which scrvcs to provide a n ultrahigh-
vacuum transportation path for the substratc between the various deposi-
tion and exposing operations. This design would have the advantage of
being able to bakeout the individual sections quickly without interfering
with adjacent, operations. However, the system is less flexible than the
present design and is not desirable at this state of development.

B. High-Vacuum Apparatus
The vacuum system that is prcscntly in use is shown with some of its
accessory equipment in Fig. 31. The pumping equipment consists of a
30 cfm roughing pump, backing a G-inch diameter fractioning oil diffusion
pump and water cooled baffle, with a 5 cfm holding pump. The bell jar to
be evacuated is 24 inches in diamctcr and 36 inches high with two &inch
optical ports. The bell jar and base plate are fabricated from stainless steel.
An adapter ring having 18 portholes is used to bring in various services.
All valving is controlled electrically from a rcmote panel, and some of the
large valves have air operated booht circuits on them. Thc programming of
a vacuum cycle and various fail-safe opcrntioiis c:in thus be easily accom-
plished using clcctrical signals.
A hydraulic hoist is provided for raising and lowering the bell jar. This
is done so that smooth, vibration-free opcrat ion can be secured and that
the bell jar and accessorics-such as t tie ultxahigh-vacuum bakeout
furnace-will not have to be countcr-bslaiiccd for cach weight used. The
hydraulic hoist is operated from water line pressure without any filtering
or lubrication. A minimum meter pressure of 28 psi is required to raise the
bell jar.
A blank-off pressure of around 5 x 10P mm Hg is obtained for the
vacuuni system when the adapter ring is used and a typical experiment is
installed. The poor hlank-off pressure is a function of the many O-ring
seals used in the system. This prcssurc’ is pcrfectly adequate as the sur-
round vacuum for the ultrahigh-vacuum at,tachnient, and is adequate for
some simple expcriments where contamination is not a problem. A pressure
of 1 x mm Hg can be reached in less than seven minutes after closing
262 K E N N E T H R. SHOULDERS

FIG.31. IIigh-vacuuin system, n,claptcr spool, : ~ i i delectroiiic regulator apparatus.

the bell jar, and this prcssurc is adcquak to begin thc ultrahigh-vacuum
cycle.
1. Adapter Spool
Figure 32 shows the adapter spool installed on thc baseplate of the high-
vacuum system. Starting in the front left of the picture and proceeding
MICROELECTRONICS 263

counterclockwise around the ring, the various accessories arc : w:itcr-


cooling manifold, 200 anip low voltage lend-in, 30 kv 20 anip Ie:td-in,
10 kv 200 amp water cooled lead-in, 2 kv 10 arnp octal lead-in, optical
port, two blank ports, 6 chaiiriel mcchaiiical iiianipulator lead-in, gas inlet,
gas inlet, optical port, 10 kv 10 amp octal lead-in, 2 kv 10 amp octal lcud-in,
ion gauge port, and 20 kv 10 amp lead-in. Almost any service can be
entered into the vacuum system through the I :-inch holes provided in

FIG.32. Atlnptcr spool shotviiig v:irious :ic.wssoric~s.

the adapter spool. ,411 vacuuiii seals arc made with O-ring seals for their
convenience of opmation. A large diaiiictcr O-ring seal is provided in the
lower surface of the adapter spool to scwl to the baseplate. The spool can
be remoi7ed from the vacuum system without disturbing the experiment,
and another experimeiit can be iiiscrtetl in its place. As shown in Fig. 13
the experiments arc iriounted on an nlumiuutn bnseplafe which can he
removed from the adapter spool provided the various electrical and water
cooling leads are removed. The niechanical manipulator is detached
to to ma tic ally upon raising the aliimiiium mounting plate.
264 KENNETH R. SHOULDERS

2. MYClLlNlCAL MANII’UCATION

The six-channel mechanical muriipulator shown in Fig. 33 is considered


to he well suited to the present requirements where great flexibility in
operation is required without int,roducing excessive thermal delays, lcaks
into the ultrahigh-vacuum region, or mechanical diffieu1t)ydue to operation

/INNER VACUUM CHAMBER


GE INSULATOR
WATER COOLED CONTAINER
AND ION COLLECTOR

_/-MANIPULATOR WIRES

P’
/

- MANIPULATOR
ENTRY CHAMBER

__ MANIPULATOR SEAL

\-ELECTRON SHIELD
MANIPULATOR
FILAMENT

1- -FILAMENT INSULATOR
INNER VACUUM CHAMBER SEAL

DRIVE WHEELi

FIG.33. Drawing of ion pump, inner vacuum chamber seal, and mechanical manipula-
tion method.

at high temperatures in vacuum without lubrication. This manipulator


consists of a system of capstans driven by a wheel that can be positioned
under each capstan and rotated without causing adjacent channel inter-
ference. The capstans are grooved tlo receive 0.006 inch diameter molyb-
denum-tungsten ulloy wires. These wires can be conducted to various
points in the system by using aluminum oxide pulleys and wire guides. A
MICROELECTRONICS 265

siniplified illustration of this is shown in Fig. 39 (p. 274). The position of


the various channels is shown on a scale t8hatis positioned in view of one
of the optical ports. A motion dependability of 0.01 inch can be secured by
this method. All wires are spring loaded with the springs being retained in
the cool region of the high vacuum system below the water cooled aluniiiium
plate. When manipulator leads enter the ultrahigh-vacuum system, they
are taken through a ceramic manipulator seal, as shown in Fig. 33, having
very close fitting holes to seal the wires. In addition, the gases accidentally
introduced are dueted to the ion pump through the manipulator entry
chamber.
Over eighteen channels of niechanical manipulation are needed in a
complete processing chamber to introduce new material, to operate vacuum
locks, to move substrates to various locations, and to operate shutters.
The compactness, low thermal mass, and fexihility of the wire type
manipulators are very desirable. KO maintenance problems have Iwen
encountered in the operation of properly inbtalled wire-drive manipulators.

C. Ultrahigh-Vacuum System

1. GENERAL

An ultrahigh-vacuum attachment to the high-vacuum system is being


constructed along the lines of a smaller system previously designed aiid
tested by the author. This attachment consists of three principal parts:
namely, an inner vacuum chamber aiid seal, an ion pump, and a bakeout
furiiace. These parts are shown in Fig. 34. Figure 35 shows the hase of thc
inner vacuum chamber aid the ion pump assembled on the adapter spool.
The bakeout furnace is shown in the bell jar in Fig. 36, with its electrical
power inlet and water cooling lilies being brought out one of the 6-inch
diameter ports of the jar.
Thc complete assembly of the ultrahigh-vacuum att,achment is shown
in the drawing of Fig. 37. The inncr vacuum chamber is surrounded by a
system of 0.005-iiich-thick nickel radiation shields and a water cooled
jacket. Thc inner chamber is heated by radiation from a 0.046-inch-
diameter molybdenum wire that is wourid on a nickel framework and
supported on alumina insulators. This heater operates a t 208 volts arid
23 amps to heat thc iiiiier chanibcr and base plate to 900°C in about six
miriut es.
Thc inner chamber is supported by four rods connected to the inner
vacuum chamber lift. This lift is operated froin outside the vacuum
chamber through an O-ring seal and causes the inner chamber to move up
and down about one-half inch aiid to make forceful contact with the inner
vacuum chamber seal.
266 KENNETH R. SHOULDERS

FIG.34. Ultrahigli-vacuum attachmrnts fihowing the bakeout furnace, iiiner vacuum


chamber, and ultrahigh vaciiiiin base plate with ion pump attached.

The ion pump and inariipulator entry chamber arc shown assembled on
the inner vacuum chamber base plate in Fig. 33 with the manipulator
wires passing through the water cooled base plate, the radiation shields,
and the two seals on the manipulator entry chamber.

2. SEALING

Figure 33 also shorn the detail of the molten inetnl seal for the inner
chamber and of t,hc seal heater. Figure 38 shows further details of this seal
hcatrr assembly. The seal that has been tested more thoroughly than
others is silver-copper eutectic using a nickcl base plate 0.01 inch thick.
Other seal materials such as gold-nickel eutectic have been tested against
a 0.01 inch thick molybdenum metal base, and a Norton flame sprayed
“Rokide” aluminum oxide trough 011 a nickel base. An electron emitting
filament is supported by ccramic insulators attached to thc electron shield
and this clrctroii source is used to raise the moat temperature above the
MICROELECTRONICS 267

surrouncling tenipernture b y electron bornhardinciit. A water cooling coil


on t'hc base prevents heating of the base and provides mechanical strength.
Thc principal design requirenieiit of thc entire seal izsseinbly is that
proper materials be chosen t o prevent alloying of the parent metal parts.
B y using thc silycr-coppcr cutectic at temperatures not over 785°C the
seals have lwrn kept in nioltcii state for several hours or the equivalent of
many hundreds of opening and closing cycles.
Tests on sniall seals of gold-nickel eutectic on molybdenum have given
sevcral hundred operations at, 980°C. The vapor pressure of the most
volatile component of the sealing alloy is less than mm Hg a t the
respective temperatures, but there is some loss of material through evapo-
ration and capillary action along seains in the inner vacuum chamber.
Material can be prcvented from ciitcring the experiment, region through
the vapor phase b y inserting a cold MAc near the seal. The tests 011 flainc
sprayed crramic coatings did not show any signs of deterioration during
the several hours of testing tiiiic. Thcsc inatcrials were not prone to wet
to the gold-iiickcl eritect ic until a sinall airiouiit of zirconium hydride was

FIG.35. Ultraliigh-vacuiuii base plate, ion pump, and radiation s h i ~ ~ l dshown


s as-
sembled 011 a t l q i t c ~Sl)OOI and high-vuciuuii system.
268 KENNETH R. SHOULDERS

added to the sealing alloy. Some peeling or cracking of the ceramic from
the base could have gone undetected due to the thick metal overlay that
resulted from the metallizing action.
I n the present design shown in Fig. 33, the seal cannot be broken by
raising to 970°C while keeping the remainder of the experiment cold

FIG.36. Ultrahigh-vacuum bakeout furnace shown assembled in outer bell jar.

because of the warping caused by the differential expansion of the nickel


moat and the cold base plate. A modification of the shape of the moat or
a change to a low expansion material like molybdenum would be required.
The mode of operation anticipated is to raise the entire inner vacuum
chamber to the bakeout temperature around 900°C and then supply the
additional heat needed to open the seal with the seal-breaking heater.
MICROELECTRONICS 269
,,
1his is not, rspecially limiting hccausc residue must> I)(& driven froni the
inside of thc chumhcr t o a cold finger h f o r c oprning the chamber; othcr-
wise the outcr viicuuin systriii will bcconic contamin:Lted with the residue.
Scals as large as 9 inches in dianiet cr can he opciied a i d closed without

OUTER VACUUM 7..


CHAMBER
v - HYDRAULIC HOIST

/ION PUMP
/MANIPULATOR WIRES

INNER VACUUM -~
-MANIPULATOR ENTRY
MOLYBOENUM HEAT CHAMBER

RADlPTlON SHIELDS SEAL

WATER COOLED _z SEAL BREAKING


HEATER

I5/MANIPULATOR
:WSN~~~~~LECTOR

ACTUATOR

BASE PLATE __L' i ,,'


.
.

INNER VACUUM
CHAMBER LIFT
A
' MANIPULATOR
CAPSTAN

OIL DIFFUSION PUMP -


BAFFLE AN0 VALVE

FIG.37. Drawing of ultrahigh-v~cuumattachment assembled in the high-vacuum


systcm.

particular regard for the warping problem apparent in the 17-inch diameter
seal.
3. ION PUMP

A detail of the ioii pump is shown in Fig. 33. This is essentially a water-
cooled caii that, has openings a t the top and bottom for eiitxy of gas. The
caii contains mi electron emitting filament, an anode grid cage, and an
270 KENNETH R. SHOULDERS

electroil buntbardmelit type of evaporator for molybclciiuiii. The molyb-


denum metal evaporator acts as a chemical “getter” for the system whilc
the ion pumping action runovcs iioble uiid other iiiert gascs. The evaporu-
tjion of molybdcnuni is carried out iiitcrmittciitly whcncver a monolayer
of gas is formed on the previous molybdcnuni layer. To evaporate the
molybdenum it is oiily iiecessary to switch oil the voltage of the water-
cooled anodc that holds the inolybdeiiurii sample. Three thousand volt)s a t

FIG.38. Underside vicw of the ultrahigh-vacuum base platc showing elcctron bom-
bardment ~ e a breaking
l heater and cooling coil.

0.3 amp is needed to evaporate the molybdenum, and a current regulator


is uscd to obtain stable operation.
When ion pumping, the voltages will be adjusted to give about 800 volts
betwcen t>hegrid cage and the filament a t an emission current of about
0.2 amp. The grid is composed of 0.006-inch-diameter molybdenum wires
spaced 0.25 inch apart in order to provide a reasonable degree of electron
transparency and allow a long mean path length for electrons. The ion
collector is held about 100 volts negative with respect to the cathode and
accelerates the positive ions formed in the grid region into it. A portion of
MICROELECTRONICS 27 1

the ioiis ncwkrated into the wntcr-coolrct ion c.ollc.ctor w e rct:Liiid :uitl
a p u m p i ~ gaction result,s. I>uriig ioii punipiiig the iv:ttcr-cooletl aiiodc is
held near cathode potential bo LLX iiot to collcct, clwtroiis. A sniall diameter
wire is insertcld into the ceritcr of thc grid cage and opcrated atJ ground
potential to serve as an ion collcctor for measuring the pressure in the ion
pump.
When large quantities of known materials are to be pumped from the
system a separate pump can bc provided. For example, a platc of molyb-
denum hcatcd to around 600°C by electron bombardment and held adja-
cent to a water-cooled plate of nickel has bccn used to pump large quantities
of chlorine by converting the chlorine to niolybdeiium chloride arid con-
densing it on the cold plate. The prcshure cannot be pumped to lower than
the vapor pressure of the metal chloridc :itl the teiiipertLture of the coii-
densing plate. By using this bame incthod but substituting a zircoiiiurn-
coated plate, carbon monoxide was rapidly pumped from a systcm without
introducing contariiinatioii from liquid pump oils.
No data is available yet on the puinpiiig speed of the pump shown in
Fig. 33, but previous experience with smaller pumps of similar design indi-
cate that for active gases the pumping ac%ionis similar to a 3-inch-diameter
infinite sink. Due to the differential pumping of the entire vacuum system,
the inert gases are not present in any significaiit quantity, and it has been
found that the high bakeout teinperaturcs clcconiposc organic materials
and oils to their simpler coinpoiicnts
4. TPPIC.1L OPERATIOS

Based on previous experience with L: sniallcr vacuum syhtein of similar


design, the author has found a strong dcpcridciice of the degree of vacuum
obtained, and the speed of ohtaiuiiig thc vacuum, o i l the bakeout tempera-
ture and speed of heating and cooling. For twmiplc, it has been possible to
evacuate a 9-inch-diameter by 12-inch-long vessel from atmospheric
pressure to the lo-'" region in as short a time as 15 niinutcs. The time
constant of the heater and of the cooling mechanism for the present design
indicate that the same region of evacuatioii speed will be obtained. The
vacuum cycle that might be considcrccl typical is as follows: (1) roughing
of bell jar with inner chamber open-6 minutes; (2) diffusion pump cycle
to lop4mm Hg-1 minute; (3) heating of ultrahigh-vacuum chamber to
900°C with inner chamber open-6 minutcs; (4)closing of inner chamber,
firing of ion pump evaporator, and cooling of inner chamber by forced
nitrogen gas and then water-6 minutcs; (5) ion pumping at, low temper-
ature--3 minutes. A total of 22 miiiu to reach t)he 10-'O region would
seem reasonably near the niinii~iumtime that could be expected for the
vacuum equipment described here, which has $11inner chamber size of
272 KENNETH R. SHOULDERS

17 iiichcs by 30 inchcs. As the complexity of the apparatus in thc vaciium


cnclosurc iiicreascd, the thermal time constant and the processing time
would also increase. It would be reasonable to expect a time constant of
45 minutes per vacuum cycle for a moderately complex experiment.
Thc cycle for opening the vacuum apparatus would be primarily a func-
tion of the t,hermal time constants of the molten met$alseals. If independent
seal brcaking heaters were used, the opening time could be as short as
four minutes; however, it would be in the region of 12 minutes if the entire
system had to be heated and cooled to break the seal and drive out the
residue from some previous experiment.
5. ULTRAHIGH-VAC UUM ACCESSORIES

Because of the high temperature hakcout, a range of accessories is


rireded for the ultrahigh-vacuum attachment, that is not compatible with
the high vacuum accessorieh now commercially available. These accessories
arc vacuum valves, vacuum locks, electrical lead-ins, optical ports, and
cooling-water inlets.
The valvc and vacuum lock requirements are met by combinations of
the wire manipulators arid the molten metal seals. A bmall seal of the type
employed in valves aiid locks is shown in the drawing of Fig. 27, as used
with the electron optical system. These valves are patterned after the
molten metal seals used in th r base of thc inner vaeuum (*hamheraiid a r r
heated by electron bombardment.
Electrical leads are fed into the system through high alumina ceramic
terminals that have electrodes brazed into them. The entire electrode as-
sembly containing 12 leads of 0.040 molybdenum wire in t n o h e a r rows
of six each is brazcd into the base by electroii bombardment while in a
lop4mm Hg vacuum. Large insulated lead-ins, such as the oiie shown oil
the ion pump in Fig. 33, are brazed in a similar fashion.
Optical ports can be obtained by brazing ground and polished discs of
sapphire in the baseplate for the inner chamber, but if adequate electrical
instrumentation is used there is no need for optical ports.
Cooling-water lines can be brazed in position by flanging one end of a
pipe while leaving the other straight, as shown in Fig. 33. A small quantity
of gold-nickel eutectic can be used many times over for this operation, and
it will be found that removal of any part properly brazed in place is a
simple matter of reheating in vacuum with ail elcc%-on bombardment jig
and letting thr part fall out hy gravity or by removing it with a manip-
ulator.
One feature that is a by-product of the high temperzlture bakeout furnace
is t,he ability to coat the inside of the vacuum apparatus with thin, chem-
ically-resistant films of alumina or silica. This is done by sealing up the
MICROELECTRONICS 273

system and adniitting a small quantity of aluniinum chloridc and water


vapor, or tetraethylorthosilicate, while the temperature is being raised. All
apparatus exposed to the chemicals, suvh as lead wires and coiinectors, are
coated with insulation, and those drvires that must, he free of coat4ingshould
he removed from the system. For somr purposes, this coatiiig gives the
Fame rcsults as working in a glass vacuiini systrm.
In addition to conventional ion gaugc instrument at ion of prcshure in the
system, it, has bccn found uscful to include a field cmissioii cathode near
the surface that is to be dcposited upon. When this field emitter is used
as a ficld emission microscopc electron source, the effect is to produce an
integrating vacuum gauge where spurious deposits on the tip can be identi-
fied by their emission pattern and by their activation energy. This inte-
grating effect has hecii used to identify aiid locate bursts of solid materials
that escape detection by ion gauge techiiiqut.s, but nevertheless form coii-
tamiiiating deposits on thc surfscc k i n g co:it,ed. These bursts of solids
frequently arise from monicntary eloct rical discharges in the vacuum sys-
tcm 1vhic.h dislodge materid froin the w:ills by inadvertent rlectron and
ion bombardmcnt. Materials have also becn removed from thc walls by
displaccrnent reactions in which a short lived species of volatile material
is produced that is difficult to see 011 an ion gauge. ,4niass spectrometer
will be incorporated into thc vi~cuu~ii system j i i the future to help identify
these materials and their sources, but thrir detection usually requires an
integrating devicc because of their sporadic appearance.
D. Integration of Apparatus
, I dr:~n.iiigof oiie layout for the various pieces of apparatus is shown in
Fig. 30. This drawing shows a single dcpositiori and etching chamber that
is capahle of k i n g sealcd off from thc main ultrahigh-vacuum system to
prevent cont,aniination duriiig the purging cycles hetwcen dcpositions. A
valve or vacuum lock i b providcd in thc top t o allow the transport of a
substratr bctwecri the depohitioii chamber and the clectrou lens. Storage
spacc for scveral substrates is provided in the iiiner vacuum chamber so
t hat, various experiments can hc carried out without opening the vacuum
charnbcr. Vwuum locks are also provided on the lower side of the deposition
chambcr so that inatcrial not able t o withbtaiid the bakeout temperatures
may be eiitcred from the cool portionr of the high-vacuum chamber.
The clcctroii lens usscmhly is capahle of being sealed from the remainder
of the vacuum chamber. Thr sealiiig ( ~ v e aiid r the magnetic shield cap
shown in Fig. 27 must he manipulatrd out of thc path of the suhstratc
: L I ~suhstratc holdw. ‘I’hcb ~~wrss:try slor:igr spncc for tlic~sc~(wwrs is
providcvl i l l the iiiiior V:WULIII~ (~h:mlwr.‘l’lie sockct-cwg:igiug mcdiaiiim
for the elec’troii lciis is operated through the inanipulator located in the
MOLYBDENUM HEATER ELECTRONLENS ENCLOSURE

RADIATION SHIELDS SUPPORT TUlllNG

O U T E R VACUUM
CHAMBER HYORAULIC H O I S T

INNER VACUUM
CHAMBER

DEPOSITION AND ETCHING


CHAMBER
MANIPULATOR WIRE

DEPOSITION CHAMBER MANIPULATOR S E A L S


VALVE

MULTl CHANNEL
YANIPULAT ORS

SUPPORT TUBINQ

DEPOSITION CHAMBER
. . I
HYORAULIC HOIST

VALVE MANIPULATOR WIRE


PULLEYS

MANIPULATOR W I R E
GUIDES
DEPOSITION AND ETCHING
CHAMBER
MANIPULATOR WIRES

MANIPULATOR W I R E
QUIDES

ION PUMP

MANIPULATOR ENTRY
CHAMBER
ELECTRON L E N S ENCLOSURE

MOLYBDENUM HEATER

RADIATION SHIELDS
ADAPTER SPOOL
NER VACUUM CHAMBER
SEAL

I
BASE PLATE
‘-MULTI CHANNEL
MANIPULATOR

FIG.39. Layout drawing of ultrahigh-vttcuum system containing the electron optiral


system, deposition and etching chamber, vacuum locks, and mechanical manipulation.

274
MICROELECTRONICS 275

bottom of the electron lens enclosure. This manipulator must exert a large
force or the socket and manipulator wires cannot be used.
The manipulation methods used for the various operations are dis-
cussed in Section XIT, B. It is iieccssary to consider manipulation methods
that caii be hinged at a comnioii point, or quickly removed in order to allow
rapid access to the various components of thc system. For example, Fig. 39
shows the electron leris covered by the manipulatms, hut this is not trouhle-
some when disassembling the electron lens enclosure because the manip-
ulator assembly pivots immediately abovc the upper manipulator wire
guides, and the entire assembly can be rcmovcd a i d replaccd in a few
seconds without disturbing the manipulator wires.

XIII. Electron Microscope Installation

-1 Hitachi IIU-10 clectron microscope is used in this work to serve as


an analysis tool for the various processes heing studied, and, in this initial
phase of the work, to serve as a high resolution demagnifying lens for the
micromachining prow The following accessory items are also useful:
Reficvted dectron microscopy attachment
IClcctron ..pray g u n charge ncutralizcr
Specimen hcating slid specimen cooling stage
X-ray point projection microscopy at tachmerit
High resolution diffraction attachment.
The specifications as statrd by thc manufacturer arc :
Acc~eIer:itingvoltages: I00 kv, 75 kv, 50 kv
Magnificat ion: 400 to 180,000 electronically
(:uaraiitcvxI resolving powor: 10 A
Rcsolving Irides (Diffraction) :
Sclected area diffraction 5 X
High resolution difimction 5 x
Illuniinnting System:
J)oul)le cnndciiser lens with 5 square micron niiniinum arm of
illuniinntion
Optical System:
Thrw stage magnet ic leiis systcin. P'our sets of polc pieces for the
project or, changeable during operation.
This instriiment hns passrtl rcsolution and stability tests made by oh-
t aiiiiiig pictures of 1 lattice of copper p~iiIi:blociaiiilicat a magnification of
h i

800,000 for thrw coiisccutivc days. This dcinoiistratc~sa resolution in the


range of 8 A. The instruinerit was i~istnIlc(1ill a clcan room facility, shown in
276 KENNETH R. SHOULDERS

FIG.40. Hitachi HU-10 electron microscope installation.

Fig. 40, that also houses the vacuum deposit>ionapparatus used in the
micromachining program.

XIV. Demonstration of Micromachining


A demonstration of micromachining has been conducted using simple
vacuum deposition equipmciit and a commercial electron microscope. The
optimum properties of the process cannot be secured by using such make-
shift methods, but the goal of denionstrating the machinability of materials
by electron beam techniques is attainable to some small degree. Some ap-
plications for electron beam machining would conceivably need no more
elaboration than is used in this demonstration.
Briefly, this demonstration consisted of depositing niolybdeiium metal
on a thin film of aluminum oxide which is supported on an electron micro-
scope specimcn screen, coating the molybdenum with the triphcnylsilanol,
cxposiiig in the clcctron microscopc with a rcducctl pattern of n scrcci~
wire mesh, and etching thc molybdeiium in chlorine. Thc fiii:il rcsulf, is
shown by a photograph taken in the elcctroii microscope.
MICROELECTRONICS 277

A. Substrate Preparation
A c o p p c ~wweii of 200 mrsh is covrixl with a collodion film made by
spreading a 2% solution of ccllulosc nitrate in ainyl acetate on water,
:ih described i i r :uiy st:indard text OII dcctron microscopr specimen screen

pi*rpnration. The collodioii is typicdly 200 A thick. This s(’re(’n is thrn


put i n a \~acuunisystem, swh a< thc oiir shown in Fig. 31, and coated
\L ith :L 800 Li-tliickfilm of nlruninurii oxide I)y cuaporatiiig from a tungsten
1)uskct hratrd by rlcctroii t)oml)ardrncnt iii the apparatus shown in Fig. 13
and described in Section I’IIT, A on Matrrial Drposition. The copprr
screen and films are heat c d t o urouiid 800°C by the srniill ceramic substratc
heater shown in Fig. 24 to drivr off the collodion a d stabilize the evap-
orated :Llumiiia. Higher tempcrat u r ~ sivould he desirable but, the coppcr
srreeii is prone to evaporate : u d mrlt hcfore thc rrcrystallizatiori of the
aluiniiia a t 900°C; this is caused I)y thc fact that the copper is hottcr than
the film of alumilia, since they :irr i i o t in I~lackbodycqiiilibrium with thc
sritistr:it(>heater.

B. Film Deposition
?‘he inoly1)deiium as evaporated on1o the aluiniiia surface with the
apparatus shown in Fig. 13. The molybtlrnum sourcc is simply a self-
Fupporting rod of vacuum melted niolybdrnum that is heated by electron
tiombardment . The thick1 of the molybdenum film is optimum for our
purposes when betwcen A :~nd200 A. Heavy drposits cannot be
penetrated by the electron beam during h t r r aiialysis for surface defects,
such as spotty resists or piles of foreign material, that may have been pro-
duced. Thinner films fail to give adequate coiitrast iii the micrograph duc
t o electron scattering from thr substratr. The tempcraturc of the substrate
during the deposition is not important but is usually in the region of 300°C
t o prcvrnt oil films from \)ring dcpositcd siinultarirously with the molyh-
dciiuin. The vacuum was rarcly better than 5 x 10-5mm IIg and the oil
pumps have hrcii k i i o ~ ~to t i hckstrcani :md coiitaniiiratc~v:trious samplrs.
Thc rntc of deposit ion was fairly slow for t molybdenum source that l i : ~
h ( b

lieen used I)ecnusc of the small diameter. A typical drposition required


three minutrs for a 150 A film of molyhtlriiiim.
Aftcr deposit ion, the film iis heated to tiround 700°C to stabilize and
rccrystallizc the molybdeiiuni. A micrograph of thc film after pro
is shon-ii in Fig. 41, and a diffmctioii pntterii iii Fig. 4%.
Thc f i l i n is c h o o l ( 4 to room trniprmtui~cand a cwatiiig of tripht’irylsilaiit,I
\\:is :ipplicd l)y \ w u u i i i ( ~ v : t p ( ~ ri oaiti froni :1 m i i l l glass crricith with t h
~ : L I I I Capparat us usrd previoiihly. ‘I’hc. cruci\)l~ is hcld in :I iiiolyldriiuin wirr
holdcr \vhicdi rcceivrs the elect roil 1)oriihardmciit for heating. A filrri thick-
KENNETH R. SHOULDERS

FIG.41. Electron micrograph of 200 A-thick molybdenum film deposited on 200


A-thick aluminum oxide by thermal evaporation.

iiess of about 50 A is optimum for the resist layer. Thicker films tend to
agglomerate and grow into feathery shaped patches. Thinner films can be
used but the possibility of developing a hole in the resist is higher. Upon
completion, the compositcb of films was removed from the vacuum system
arid inserted i n the rlrct,mn microscope for exposing.
C. Resist Exposing
The 1Iitach@IU-l0 electron microscope pictured iii Fig. 40 and described
in Section XI11 has been modified slightly by installing a removable 500
MICROELECTRONICS 279
mesh screeii above the objective leiis in such a way that) the screeii can be
dernagnified by 200 times. The focal length of the objective lens is 0.5 mm
during normal operation aiid thc w r w n riiust be spaced about 100 mm
above the principal plane to obtaiii the 200 t o one demagnification. The
specimen holder for the microscope was modified by extending it approxi-
mately one-half millimeter below thr principal plane of the lens. This
specimen holder was used for csposing only, aiid iiot for microscopy. .4p-
proximately 50 specimen holders conic with the iiistrurneiit so that modi-
fying oiic is of little coiisequciice.
The illumination system was stopped down by usiiig a small aperture
iii the second condenser h i s . This leiis has three movable apertures that
can be changed during the oprration of the instrumcnt without breaking
the vacuuni. The aperture size used for cspoxiiig resists was approximately

FIG.42. Electron diffraction pattern of ruolybcleiiriin-LIlumirla sample shown in Fig. 41.


280 KENNETH R. SHOULDERS

0.002 inch in diameter. The illuminating intensity of tlhe instrument was


reduced t o the lowest possible value by increasing the grid bias on the elec-
tron gun with the switch provided for that purpose. The intensity was
further reduced by reducing the filament temperature. The only method
of rontrolling the aperture angle of the illuminating electron beam into the
objective lens is by adjustiiig the second rondenser lens current. The con-
denser lens thus determines the number of grid wires seen arid the ohjective
lens controls the size of the image, although strictly spraking there is only
one magnification that is properly focused, namely 200. The current
density under typical exposure conditions is about 10 ma/cmz and the
beam velocity is 50 kv.
During exposure, the intermediate and projector lens were used as a
microscope to observe the position of the specimen screen. These lenses do
not, have enough resolution to observe the fine detail of the image used for
exposing nor is the brightness high enough to see any detail. At best the
microscope was used to tell whether or not the exposure was being made
on a n open area of the specimen screen. The method that was most effective
for determining corrrct focus was to cause t,he beam to converge to a point
on the specimen screen, as indicated by the point projection niicroscopy
produced, and then to increase the objective current a small but known
amourit]. Another indication of focus can be observed in the diffraction
pattern of the sample whereby the minimum number of spots appear when
the beam is at, crossover.
After proper alignment the exposures were made by moving the manip-
ulator for the specimen screen in small increments, observing on the fluores-
cent screen that, the exposures were being made on the open spaces of the
specimen screen. The exposures had to be long enough to prevent blurring
of the image during the time in moviiig froni one sample to the next because
beam blanking was not used. A oiie to three sccond exposure was normal
since the manipulator could be moved rather rapidly froni one spot to the
next.
D. Etching
After exposing, the samplc was retumed to the vacuum system and
inserted in the small substrate heater. The chamber was evacuated to the
region of 5 X mm Hg and the sample was heated to 600°C. A stream
of chlorine was admi d to the system through a valve and a length of
aluminum tubing. The tubing was tcrmiiiated within 5 inches of the surface
being et,ched; duc to the pumping action of the vacuum system the pressure
was highrr :It thc surfncc than is indicated 011 a remote gauge. Thc chloriiw
prcssurc was rchgulatecl l)y hand to a value uf 5 x 10 ' rnrn Hg, as iiidicatd
by operating oiic of the evaporator positions as an ion gauge. 'l'he etching
MICROELECTRONICS 281

was complctcd in a fcw seconds; the chlorine prcssurc \vas rccluwd; aiitl
the suhstratc tcmperaturc lowered. 0t)scrvatioii of the surface during
etchiiig revealcd that the appearailre chaiiged flwn L: rcflcctiiig metallic
surface to a traiisparent dielectric surface. Thc sample was removed from
the vacuum system and inserted in the electron microscope for viewing.
Figurcs 1.3 and 44 show typical samples.
E. Discussion of Results
ils indicated on Fig. 44, the image size is such that the scrccii wire
spacing is 2500 A or 100,000 mesh per inch. 'l'he image has heen distorted

FIG.43. Low inngnificatioii electron niirrogr:ipti of ~nic~oma.ctiiiied


molyhde~lum
2OU A-ttiick on slumiriurii oxide substrate.
282 KENNETH R. SHOULDERS

FIG.44. High magnification electron micrograph of micromachined molybdenum


200 A-thick on aluminiiin oxide substrate.

into a pincushion shape by the electron optical system so that the current
density falls off approximately as the square of the distance from the center
of the axis. This effect is beneficial for determining the condition of exposure
and the effect of the etching on underexposed areas. As can be seen, the
transition region between properly exposed areas and unexposed areas
produces patchy etching caused by having the resist too thin. I n the center
region the transition is rapid enough to produce relatively sharp edges.
The resolution shown iii the micrograph is in the region of 300 A, with the
MICROELECTRONICS 283

priiicipal error resultiiig frc~mthe raggctlness causecl I iy tlic l):~(:kgrouiid


fog effect.
The background fog, or patclics ( J f niolybdeiium abut 300 A in diameter,
have been mused hy migration of unstable, recrystalliziiig aluminum
oxide during the various hcating cycles. This aluminum oxide forms a
chemically resistant film around the small granules of molybdenum and pre-
vents further etching by chlorine. This tiackground fog can be removed by
using a very short etch of phosgeiic gas to remove the thin film of alumina.
Close inspection of Fig. 44 reveals that most of the molybdenum particles lie
adjacent to a light area in thc supporting substrate, which could be inter-
preted to nican that the alumina came from these arms. By using high
temperature screens aiid stabilizing the alumina to alpha form, most of the
background van be removed, although there is still a very small reaction
bctwecii thc niolybdeiium aiid the alumina. The dark areas i n the molyb-
denum film are caused by selcctiw rlcct roil scattering within the molyb-
denum crystallite. When these films are being observed in the electron
inicroscope the arcas alternate between light and dark, and under dark-
field illuminatioil they are even more pronounced. The thickness of the
film is apparently uniform.
Figure 45 shows a specimen scrceii of silicon on silicon dioxide made h y
techniques comparable to the oiics used for the micromachining of molyb-
denum. The specimen support film had been torn from the screen and rolled
back to produce the dark ragged line adjacent to the light area. As can be
seen, several images were exposed on the same screen opening. These
samples were oxidized slightly in transferring between the electron micro-
scope and the vacuum deposition chamber, which resulted in another type
of background fog, namely, silicoii dioxide on silicon. The only completely
effective remedy for this is to keep the silicon under vacuum a t all times by
incorporating the electron optical system with the deposition apparatus.
This denionstrat ion has purposely been doiie with relatively crude equip-
ment aiid techniques, with the exception of the electron microscope, so that
they could he carried out without modification in any establishment out-
fitted with iiornial deposition apparatus, and having access to an electron
microscope. With only minor additions, almost ally electron microscope
with rcsolution greater than 100 A can be used for exposing.

XV. Summary

A. Microelectronic Component Considerations

The fabrication of one-micron-sized components, incorporated into a n


electronic system having over-all dimensions of one inch on a side and
284 KENNETH R. SHOULDERS

coiitaiiiiiig 1W coinpoiicrits per cubic inch, is prcsciitly limited by coiistriw


1 ion tcchiiiqucs. Intcrconiicctioii betwccii widely separated components
is coiistraiiicd by t hr high rlwt ricd rcsistiLii(ac of traiismissioii lilies, which
can h a w a dc rcsistaiice of l o 5 ohms per liiiear inch for 3000 A diametcr
conductors. To keep potentially high transmission line loss to acceptablc

FIG.45. Electron Inicmgraph ol niic.roiii:ic.liiiic,tl silicon 200 A-thick on silica 100


A-thick.

lcvels, active compoiiciits of high iinpcdaiice are required. Uiidcr these


conditions, :ui optimum switchiiig time coiist,aiit for the active component
lies in the 10-11 sec rcgioii; shorter switching times than lo-" scc result in
exccssive interconncctioii loss at room tcmpcrature and above. Powcr
densities of 10* watt/cm2 appear pcrmissiblc for onc-micron-sizcd com-
ponents; these high power densities permit high data processing rates.
For large arrays of cornpoileiits, a low quiescent, power for each component
MICROELECTRONICS 285

is required; peak power densit>yduring operation should he as high as 10'0


above the quicsccnt state.
LC filtcrs of onc-micron-size would 1)c cupectd to have a Q as much as
lox below the Q for convciitional sized filtcrs, thus making thrm relatively
useless. RC filters would bc prone to tcmperature drift when scaled down
in size because of the necessity for scaliiig up resistivity and the attend-
ant highcr tcmperature coefficient of resistivity. Electrostatically operated
elcctromcchaiiical filters that apprar ncll suited to the micron size rarigc
and coiistruction processes arc discusscd.
The rcsistivity of conductors is not affected in the size range under
iiivcstigation, hut in the submicron range thc dielectric breakdown strength
of insulators can bc incwascd to lox volt 'cm. Scaling dowri in size gives a
high sur.facc-to-volume ratio that cauws materials to migratr under the
action of surface t crision forces, and iii addition causes iiicrc:iscd carrier
recomhiiiation at thc surfnres of srmiconductors. The most difficult prob-
lems in inaterial handling involvc tlicl protluction of uniform crystalliiiity
in films.

8. Tunnel Effect Components


Electmiiic components 1)asrcl upon the quantum 1nechiic:d t uaneliiig
of electrons from a metal into a high \ w i i u r t i are proposed; with this tcch-
iiique, only stable metals and dielectrivs arc employcd iii various grometrics
to produce diodrs, triodcs, and tctrodcs. With suital)lc drsigii that makes
iisc of the l~allisticaproperties of thc clcctroris in vacuum, control grids
and srrerii grids of such deviccs caii he operated at a positive potrritial
without drawing apprcciable currents. Operatiiig voltagrs as low as 10
volts, with currcmts in the region of 100 p unip for lo4 :mp/rmz currciit
densities, appear possMc without aclvcrsc space chargc eff
the high field iiitciisities used. Normal grid voltage variations used in
various circuits would produce a chaiige in cathode current of about lolo,
which is highly desirable for low poner quicscciit operation. The amplifi-
cation factor for triodes can be in thr vicinity of 100, with a traiisronduc-
taiicc of 1000 p i t h o / ma and a platc rcsistancc of about lo5ohms. With a
power driisity of lofi wat,t,/cm2, a switrhing time constant of 10-lo sec
appears possit)lc for a oiie-microii-sizr.d devicc, with an indicated transit
time lag of src. High-frequeiiry grid-loading would bc iicgligiblc a t
100,000 hlc because of the short transit time lag. An array of 10" vacuum
tuiiriel cf'fcct devices containcd iii oiie cubic inch of spacc could opcratc
from arhitrarily low tempcratures up to arouiid 800°C. A t a inasimuni data
proccssiiig rate of lot5bits per second, thc machine would self-hcat, to
around 800°C. The iriseiisitivit,y of thc dcvice to local crystallographic
286 KENNETH R. SHOULDERS

properties would indicate an immunity to radiation damage about los


timrs greater than present single-crystal semiconductor devices.
Methods of potentially forming stable, mutiple-tip field emission cath-
odes having radii of 100 A are discussed ; here, self-formation methods would
be ueed to generate arrays of over lo8 active components per layer. The
methods would have to form components with uniform characteristics by
degenerative processes. Vacuum encapsulation methods are discussed that
are applicable to large arrays of film components, and corrosion methods
of testing the encapsulation are described which indicate a component
lifetime of several hundred years.
Solid-state tunnel-effect amplifiers are considered ;however, high grid cur-
rent, low impedance, temperature sensitivity, and device nonuniformity
make them less desirable than vacuum devices.

C. Accessory Components
Secondary electron emission effects having high stability, high current
density, negligible time delay, and temperature insensitivity are discussed
for appliration t o transmission-type electron multipliers and for coupling
between tunnel effect components.
Multiplier phototubes having 100 Mc bandwidth, negligible transit time
spread, and a sensitivity adequate for detecting ft-c appear possible
using film techniques. Such tubes would make photodetectors available
with diameters ranging between 0.01 inch aiid 0.2 microii for application
to the intercoiinection of large arrays of componrnts, and for micro-
document reading.
A method for using electronic micromarhiniiig techniques to record data
011 glass plates, with subsequent electrooptical read-out, yields a document
storage scheme with a data density of 10'' hits per square inch and a read-
out rate of 1O'O bits per second.
Electrostatically operated mechanical relays, operating in vacuum a t
30 volts, mid with frequencies up to 10 Mc, seem applicable to switching
low level signals and for power distribution.
Electromcchaniral filters composed of simple metal and dielectric dia-
phragms could serve as communication filters between 4 Mc and 600 Mc.
Field strengths as high as lo7 volts make possible electromechanical coup-
ling coefficieiits up to O.G, which would permit temperature compensL' t'ion
by electrical interaction with internal thermal bimetal capacitors.

D. Component Interconnection
I n the absence of thermally stable fixed rcsistors, tunnel effect diodes
will be employed for some resistor functions in an effort to match thc tern-
peraturf~._cocfficic.iitsof active elements. Low dissipation circuits are dis-
MICROELECTRONICS 287

cussed in which the wide current swing of tunnel effect components is


utilized. Thew low dissipation circuits would be employed in an active
niemory in which the switching time may be 10-'O src, with quiescent
power of watt for either a negative re ance or a flip-flop type of
circuit element,.
Low noise amplifiers arc discussrd in nhich a field emission cathode
produces a virtual, space-charge-limited cathode for a iicgative grid tube.
A method of using elcctrirally stccrable rlcctron guides for the purpose
of eliminating transmission liiics from future systems and for increasing the
logical freedom of a system is also discussrd.
E. Substrate Preparation
Sapphire platrs, 1 inch square and 0.01 inch thick, are considered to
be an optimuni substrate size. The platrs are mrchanically ground and
polishrd ; clcanrd by high-vacuum methods using the explosive removal of
a filmof niatcrial from the surface; then smoothcd in vacuum by drpositing
a film 011 a temporary fill material, volatilizing the fill material, and sintcr-
irig the film into the substrate. Terminals are prepared by firing molyb-
denum metal electrodes onto the plate iti a high-vacuum furnace.
F. Material Deposition
Electron boriibardnient and rt4stively-heatcd t h r r n d evaporation
sources have been built pcrmitting automatic regulation of evaporating
material to within 2 7 , of a predetcrmined value 1)y using ion gauge moni-
tors and electronic regulators. A bubstrate heatrr is described that is
heated by a 3 kv, 0.1 amp elwtron lwani. The heater is completely enclosed
by ceramic and is capable of achieving 1700°C operating temprratures for
use with reactive deposition. Reactive deposition methods are discusscd in
which dual thermal cvaporators are used to deposit stable, dcnsr, and
pinhole-free niaterials like molybdenum and aluniiiium oxide films. These
films wcre tested in the form of an encapsulatrd capacitor having a 200-A-
thick dielectric a t temperatures of 800°C and field strengths of 10' volt/cm
to reveal impurities or imperfections. Solid state tunnel emission was ob-
srrved to orcur bct\seeii elcctrodcs. Tcsts for stability of aluminum oxide
and molybdenum were carried out on the tips of a ficld emission microscope;
the tests revealed no impurities caused by the dcposition and etching
process. Mrthodx of potentially growitrg single crystd films of mattvials
iiivolvirig reactive deposition and a sweeping t hcrmal gradient are dis-
cussed relative to deposition processes.
G. Material Etching
Using molecular beam techiiiqucs in a high-vacuum chamber, both solid
and gaseous sources are employed to etch the surface of materials siich
288 K E N N E T H R. SHOULDERS

as molybdenum and aluminum oxide, converting them to volatile com-


pounds. Tests for the clcariliiiess of this process have been carried out on
field emission microscope tips and 110 cvidence of etchant residue was ob-
served. The parameters necessary to etch holes wit,h depth-to-diameter
ratios of 10 : 1 in a molybdeiiuni film are discussed. Atomic beam etching
methods arc discussed for application to low temperature etching of ma-
terials, such as the room temperature etching of silicon by atomic hydrogen.
Alet,hods of using ion beams to sputter material from a substrate have
shown very straight sided etching with no undercutting. Depth control
methods effcrtivr to 1% are considered for various etching methods.

H. Resist Production
Evaporated niat,er.ials such as silica and alumina can make effective
etching resist,s by deposit,ing t,hem through masks; however, the resolution
is limited by t,he mask. Resists can be produced by electron bombardment
of materials such as triphenylsilnnol, which decomposes to form silica with
a quant,um yield of about. one and a resolution of over 100 A for films 20 A
t,hick. Multilayer met,hods of producing resists have shown a quantum
yield of lo4molecules per electron with a resolution of 300 A. Consideration
is given to finding resist-producing processes that are compatible with
vacuum processing and t'he electron optical system. One of the chief re-
quirement's is to maintain the surfacc uriipot)eritialduring resist formation,
thus preveiitiiig electron bcsm distortion.
I. Electron Optical System
The desigii of an clectrori opt,ical system is described that is irit,ended
to become a micromachining electron source, a scanning electron micro-
scope, a mirror microscope, arid an X-ray fluorescence probe. An elcctro-
static lens syst,em made from met,alized ceramic parts is currently being
built; t,he lcns syst,em is capable of being baked in ultrahigh vacuum to
a temperature of 900°C wit,hout t,he need for mechanical realignment t o
obt.ain 200 A reso1ut)ion. Problems in obtaining registration between ad-
jacent fields are discussed, and a regist.rat,ion of 500 A is predicted. The
scanning microscope may approach a resolution of 200 A, which is equiv-
alent to the micromachining mode. Only lo6bits per field would be expected
for these two modes of operation because of limitat,ions in the deflection
system. A n electron multiplier t.hat is integrated with the lens should pro-
vide most of the neccssary gain for the scanning microscope. The X-ray
fluorcscence mode of operation should ultimately give a 1yo quantitative
analysis on grams of material, with a resolution of one micron.
Operation as a mirror microscope would give the ability t,o measure volt'ages
down tjo 0.2 volt with a resolution of' 500 A and make dynamic voltage
MICROELECTRONICS 289

~nct~snrcinrnls to 1000 M c . By usiiig the leiis as an emission microscope,


multiple cathodc ficld cmihsion arrays could be imaged with 300 A resolu-
tion and thus greatly assist in forming uniform arrays. The requirements for
various pattern generators are discussed; the ultimate geiicrator would be
able to take full advantage of the lens hy producing a 10*-hit pattern every
tenth of a setwid.
The construction techniques for producing accurate lens elements are
reviewed and some of the tests performed on the elements are described.
J. Vacuum Apparatus
A 24-inch diameter, metal, bell jar-type vacuum system is described
which is pumped by a 30 rfm roughing pump and a 6-inch oil diffusion
pump. An adapter spool having 18 entry ports for accessories is shown arid
ories such as cooling-water manifolds, electrical lead-ins, an
optical port, and mult,iplc chaiiiicl manipulators are described. A demount-
able ultrahigh-vacuum attachmrwt is descrihcd which when completed,
should be capable of attaining a vacuum of 1 X lo-'" mm Hg in 25 minutes.
A 900°C bakeout] temperature is employed in this differentially pumped
unit with a molten metal seal separating the high-vacuum and the ultra-
high-vacuum regions, the ultrahigh vacuum being produced by ion pump-
ing. A range of accessories for the ultrahigh-vacuum unit are discussed, and
considerations for iiitegration of the electron optical system and the deposi-
tion and etching apparatus are presented.

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