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Microelectronics Using Electron-Beam-Activated Machining Techniques
Microelectronics Using Electron-Beam-Activated Machining Techniques
Microelectronics Using Electron-Beam-Activated Machining Techniques
Machining Techniques*
KENNETH R . SHOULDERS
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
1. Introduction
A. General Concepts
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
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
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
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.
A. General Considerations
1. CONSTHUCTION PROCESS CONSIDERATIONS
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
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
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
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
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
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
- TOP VIEW
SIDE VIEW
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
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
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
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
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
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
V. Accessory Components
PHOTO SURFACE
ENCAPSULATION
ANODE
SECONDARY
EMISSION
CWTING DYNDDE- OUTPUT
GRID
CATHODE
GROUND
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
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
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.
K==?l- ANODE
CATHODE
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
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.
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
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
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.
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.
SUBSTRATE HEATER
I tNIPULATOR
RES
-
-
-L
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.
EVAPORATING MATERIAL 7
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.
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.
FILAMENT SUPPORT
SUBSTRATE HOLDER
b-lcm4
-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
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
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
3. DEEI' ETCHING
X. Resist Production
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
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.
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
h) STIGMATOR SURFAC
ELECTROOE SPKERS
SPRING RETAINER
I
I
h)
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
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
h)
.s
OD
PRIYARV
ELECTRONS
FLY
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
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
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
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
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
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
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
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
_/-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.
C. Ultrahigh-Vacuum System
1. GENERAL
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
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
/ION PUMP
/MANIPULATOR WIRES
INNER VACUUM -~
-MANIPULATOR ENTRY
MOLYBOENUM HEAT CHAMBER
I5/MANIPULATOR
:WSN~~~~~LECTOR
ACTUATOR
INNER VACUUM
CHAMBER LIFT
A
' MANIPULATOR
CAPSTAN
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
FIG.38. Underside vicw of the ultrahigh-vacuum base platc showing elcctron bom-
bardment ~ e a breaking
l heater and cooling coil.
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
O U T E R VACUUM
CHAMBER HYORAULIC H O I S T
INNER VACUUM
CHAMBER
MULTl CHANNEL
YANIPULAT ORS
SUPPORT TUBINQ
DEPOSITION CHAMBER
. . I
HYORAULIC HOIST
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
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.
Fig. 40, that also houses the vacuum deposit>ionapparatus used in the
micromachining program.
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
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
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
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
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
XV. Summary
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
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
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290 KENNETH R. SHOULDERS
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