Physics 366 Lab Report 1

Michael Dobbs, Sonoma State University

October 15, 2014
Abstract
A film was deposited via sputtering in a vacuum with an unknown
metal. A scanning electron microscope was used to observe the thin
film, and energy dispersive X-ray spectroscopy was utilized to obtain
the identification of the metal while micromapping calculated the location on the sample.

Introduction

A vacuum environment in a chamber is created by pumping air molecules out

of the system irreversibly using various machines. A thin film is then plated
using molecular beam epitaxy, where a metal is heated and emits a ray of
atoms that impinge onto the substrate. This sample is observed and imaged
using a scanning electron microscope, where a beam of electrons is shot at
the sample and the energy of the backscattered electrons is used to create
a 3-dimensional image. The energy dispersive x-ray spectrometer is used
to identify the sample by collecting the characteristic x-rays emitted from
the sample. The micromapping function of the EDX uses the differences in
energy of the detected electrons to calculate the position of each element on
the sample.

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2.1

Experimental Procedure
Vacuums

Vacuums were used to lower the pressure inside the plating chamber by removing air molecules. By having a very low amount of gas atoms in the
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chamber to interact with the emitted metals, the plating of a substrate occurred in a more ideal and pure fashion.
Mechanical Pumps use motors to force air molecules through two check
valves and into the atmosphere. This can lower the pressure inside the chamber to about 103 Torr. The rotary vane modules must be immersed in an
oil bath to cool the pump and lubricate the vanes. [1]

Figure 1: A Mechanical Pump

Diffusion Pumps use hot evaporated oil to trap and compress gases into
the bottom of the pump where they are ejected. A multistage jet assembly
and internal boiler are used to propel the oil vapor downward to attain pressures of 105 Torr. [1] These pumps only operate at pressures less than 100
mT so are activated after the mechanical pumps.

Figure 2: A Diffusion Pump Schematic

Sorption pumps trap gases by freezing them onto aluminum fins and
trapping them in a porous molecular sieve. The pumps are immersed in a
2-3 gallon liquid nitrogen bath to cool. [1] The apparatus must be operated
at low pressures or the fins will quickly be saturated with molecules.

Figure 3: A Sorption Pump Schematic

Turbomolecular Pumps are similar to mechanical pumps but use high

speed rotating blades (about 90,000 rpm) to irreversibly direct gas molecules
out of the chamber and can attain pressures of 106 Torr.

Figure 4: A Turbomolecular Pump Schematic

Cryopumps are similar to diffusion pumps, but use a closed-loop helium

cryogenic refrigerator to condense and absorb the gases. Cryopumps are oil
free and can operator from any orientation with high pumping speeds. [1]

Figure 5: A Cryopump Schematic

There are multiple methods to measure the pressure inside a gas cham4

ber. A thermocouple gauge reads pressures from 1-1000mTorr using an electric current, induced by the movement of the surrounding gas, that passes
through a filament. The filament heats up to a temperature that is dependent on the thermal conductivity of the gas, which is then converted into a
pressure reading.

Figure 6: A Thermocouple Gauge Schematic

A pirani gauge is similar to a TC gauge, but the temperature is calculated

by measuring the change in resistance of the filament as it is heated. [1]

Figure 7: A Pirani Gauge Schematic

A hot filament ionization gauge must be used below 103 Torr. In this
gauge, electrons are emitted from a hot filament and ionize gas molecules in
the chamber. These positively charged gas molecules will produce a current
through the electrode that follows the equation:
IP = IE S P

(1)

where IP is the positive ion current which depends on the gas species, IE
is the electron emission current, S is the gauge sensitive, and P is the gas
pressure. [1]

Figure 8: A Filament Ionization Gauge Schematic

2.2

Deposition

Once the vacuum environment is attained, the sample may now be plated
in a pure fashion. Since there arent a high number of air molecules in the
chamber, the effect on the ejected atoms will be negligible. There are multiple
methods for plating a film.
The plating process used in our experiment was thermal evaporation,
where the coating material is heated and evaporated, causing the metal atoms
to coat the substrate. [2]
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Sputtering deposition is a plating process where the coating material is

bombarded with electrons, and the dislodged atoms are accelerated by a high
voltage toward the surface of the substrate, thereby being deposited on the
surface to form a thin film.

Figure 9: Diagram of the Sputtering Mechanism

This process creates a uniform thickness of coating at a constant rate of

1nm/s and operates under pressures of 1mTorr. [1]
Molecular beam epitaxy uses a beam of molecules to slowly plate the
substrate (less than .1nm/s). This process is useful for creating controlled
samples with a desired crystal structure. [2]

Figure 10: Molecular Beam Epitaxy Schematic

Chemical vapor deposition uses chemical reactions to transform the gaseous

molecules surrounding the substrate into solid material that is then plated on
the surface of the sample. [2] This process can occur at atmospheric pressure
or low pressures.

Figure 11: CVD Mechanism

2.3

Scanning Electron Microscopy (SEM)

Once the metal is plated, an SEM is used to observe the surface of the thin
film. A scanning electron microscope heats a metallic tungsten filament that
emits electrons to form an image.

Figure 12: Tungsten Electron Gun Schematic

Tungsten is used because it has a relatively low work function (4.5eV),

so many electrons are emitted, following the function:
JC = A T 2 eEW /kT

(2)

where JC is the current density, k and A are constants, T is the temperature,

and EW is the work function. The bias voltage needed is around -400V for
maximum emission current.

The SEM lenses are used to demagnify the beam about 5000 times. Condenser lenses control the spot size of the electron beam while the objective
lens focuses the beam using the stigmator, aperture, and scanning coils. By
adjusting these various parameters of the snorkel objective lens, the working distance of the electron beam was controlled. For the best resolution,
the electron beam must diffract most effectively at an angle of about .004
radians. [3] Many effects of the lens may keep us from optimizing this angle. Aberrations in the lens cause rays passing closer to the optical axis to
focus further away than other electrons. Chromatic aberrations cause higher
energy electrons to bend more when they pass through the magnetic lens.
Astigmatism causes various angles of the sample to be viewed in a single
scan and is due to imperfections in the construction of the spherical lens.
These various problems with the lens can be accounted for by adjusting the
contrast, focus, angle of view, and magnification of the beam.
After the electron hits the surface of the substrate, it can backscatter
and head directly toward the detector, or it can enter the solid and scatter
through the lattices. This causes secondary electrons to become excited and
possibly leave the solid and hit the detector. Electrons will penetrate farther
into the specimen if they have a high accelerating voltage, high beam energy,
low atomic number, and hit directly perpendicular to the surface.

Figure 13: Electron/Specimen Interaction: Path Dependence

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Once the electron hits the detector, the imaging process may begin. A
semiconductor is hit by the electrons and positive holes are created. This
information is collected by the system and used to amplify and display the
signal on the CRT or TV screen. The image is magnified according to:
M = LCRT /LSCAN

(3)

where LCRT is the length on the CRT screen and LSCAN is the length of the
scanned specimen.
The depth of field of the beam refers to how large a distance is in focus
on the screen. The quality of focus is inversely proportional to the size of
the beam following the equation:
D=

2r
alpha

(4)

where D is the depth of field, r is the radius of the beam that causes noticeable
defocusing, and alpha is the beam divergence. [3] You can adjust the depth
of field by changing radius of aperture that in turn changes the divergence
of the beam.

Figure 14: Electron Depth of Field Schematic

The contrast of the image is affected by how the beam interacts with
the specimen. This interaction depends on the shape and composition of
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the specimen which determines the electron flux, the size and position of
the detector, which captures electrons with different trajectories, and if the
electrons are backscattered or secondary, which determines the energy of the
electrons. Contrast is defined as:
C=

S2 S1
S2

(5)

where S2 and S1 are the signals detected at 2 points of interest on the image,
usually the specimen and the environment, respectively.
The SEM may be set to backscattering electron imaging mode or secondary electron imaging mode, each capturing different types of electrons.
Each mode is used to quantify the number of electrons coming from each
type of interaction. Resolution mode can be used to image the fine details
at high magnification. High current mode is used for the best visibility and
quality in the image. Depth of focus mode is used to see a wide range of
the specimen in the z-direction by making alpha as small as possible. Low
voltage mode is used to see surface details while sacrificing image resolution.
The SEM utilizes a variety of scans to construct a 3-dimensional image on
the screen. Line scan mode develops a 1-dimensionsal image of the surface
of the sample. Area scan mode scans in x-y patterns on the sample and
contrast is created by differences in the signal intensity on various spots of
the sample to create a 2-dimensional image. [4] Digital imaging mode stores
the image in the x-y-S array and creates an image by converting the digital
information to analog.

2.4

Energy Dispersive X-Ray Spectroscopy (EDX)

After the sample is imaged, the EDX may be used to determine the chemical
composition. When the electrons bombard the sample, they can transfer
their kinetic energy to the metals electrons to bump them out of orbit of the
nucleus, and holes in a shell ar left behind.
An electron from an outer (higher energy) shell will fall down to the lower
shell (lower energy) and the difference in energy will create an X-ray with
wavelength:
hc
(6)
lambda =
Ef Ei
The wavelength dispersion is continuous because an electron can lose all
or part of its initial energy.
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Figure 15: The Energy of the Electron Can be Converted to an X-Ray

The emitted x-rays are then collected by the silicon band detector crystal. The rays are photoelectrically absorbed by the silicon and the resulting
electron is promoted to the conduction band, leaving a hole in the valence
band. The electron-hole pairs are collected by a voltage bias to form a charge
pulse. This charge pulse is then converted to a voltage pulse and read by the
computer which computes the counts of each energy (measured in keV) and
compile them. The number of charges in the detector per incident photon
follows: [5]
E
(7)
N=
e
where E is the energy of the initial x-ray, and e is the transition energy for
Silicon (3.86eV).

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Figure 16: The Energy Lost by Shell Transitions

To convert the charge pulse to a voltage pulse, the charge is swept into
a virtual ground at the input of an operational amplifier and stored in a
capacitor. [5] The capacitor is discharged with a light-emitting diode and
the signal is amplified by the pulse shaping circuitry. So as not to saturate
the capacitor and create a pulse pileup, a fast amplifier is needed to count the
pulses quickly. When the amplifier gets too many pulses and cannot process
them all, it turns off and the detector endures dead time, which lowers the
precision of your measurements. If the infrared lamp is left on, the dead time
becomes very high and there will be a lot of noise in the spectra.
To determine the identity of the peak, the computer requires a high resolution and a small standard deviation to the energy of the collected x-rays.
The INCA program will output the spectra with the interpreted identification
of the elements in the sample, taking into account ZAF (atomic weight correction, absorption correction, and fluorescence correction). [5] The program
will take the energy counts and compare them to the characteristic x-ray
spikes of each element on the periodic table to match them correspondingly.
The exact location of the elements on the film may be found using the
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Figure 17: An X-Ray Detector Schematic

micro-mapping setting on the EDX. This program back-calculates the position of each element from the energy counts of the x-rays along the sample,
and forms an image with colored dots that represent the various elements.

Data and Analysis

Spectra from the EDX and images from the SEM were obtained for various
samples given to us throughout the semester. A choice few are shown:

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Figure 18: The Spectra for the Unknown Plated Metal

After plating an unknown metal using thermal evaporation, inserting the

sample in the SEM and running the it through the EDX, we found the thin
film deposited on the silicon substrate consisted of gold and palladium.

Figure 19: A Powdered Silicon Sample

A powdered silicon sample was evaluated and found to have traces of gold
inside.

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Figure 20: An SEM Image of the Powdered Silicon Sample

The following micromapping sample spectrum allow us to determine the

location of each element found on the different samples. Two samples were
given to us to examine, both with solder inside of a metal ring. The carbon
comes from the carbon fiber sticker used to hold the samples in place and the
solder inside the ring. The oxygen comes from the oxidized metal contained
inside the ring that is bonded to the tin and lead.

Figure 21: Micromapping Image of Solder Inside a Metal Tube

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Figure 22: The Other Metal Tube

Figure 23: An EDX Spectra of the Donuts

Conclusion

A vacuum system created by a series of pumps enables the fabrication of

a pure metal coated silicon film. Deposition allows for the creation of a
controlled alloy with a desired thickness and composition. The generated
film may be precisely imaged by a scanning electron microscope at the nanolevel. The exact elemental composition of the sample can be determined
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by utilizing the energy-dispersive x-ray spectrometer and the position of the

elements on the sample is computed by the micromapping program supplied
by INCA.

References
[1] Hongtao Shi. Vacuum system and technology 1. http:http://www.physastro.sonoma.edu/people/faculty/shi/p366/lectures/Vacuum
[2] Hongtao Shi. Vacuum system and technology 2. http:http://www.physastro.sonoma.edu/people/faculty/shi/p366/lectures/Vacuum
[3] Hongtao Shi. Scanning electron microscopy 1. http:http://www.physastro.sonoma.edu/people/faculty/shi/p366/lectures/sem0 1.pdf, October2014.
[4] Hongtao Shi. Scanning electron microscopy 2. http:http://www.physastro.sonoma.edu/people/faculty/shi/p366/lectures/sem0 2.pdf, October2014.
[5] Hongtao
Shi.
Energy
dispersive
x
ray
spectroscopy.
http:http://www.physastro.sonoma.edu/people/faculty/shi/p366/lectures/edx.pdf,
October
2014.

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