XPS Sop

Simon Fraser University 8888 University Drive, Burnaby, B.C.
V5A 1S6
E info@4dlabs.ca T 778.782.8158 F 778.782.3765 www.4dlabs.ca
X-Ray Photoelectron
Spectrometer Operation
Procedure
Standard Operating Procedure
4D Labs Confidential
Revision: 2.1 — Last Updated: September 25, 2013
Revision History
# Revised by: Date Modification
1 Michael Wang 2011/09/08 Initial Release
1.1 Michael Wang 2012/08/13
2.0 Philip Kubik 2013/09/03 Extensive revisions throughout. Removed sample loading, shut-down, &
start-up. Added safety, focussing, Auto-z, x-ray source degas & warm-up,
ion source degas & warm-up.
2.1 Philip Kubik 2013/09/25 Minor corrections to ion etching section.
1
Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
Table of Contents
1 Purpose ........................................................................................................................................... 5
2 Definitions ....................................................................................................................................... 5
3 Conventions .................................................................................................................................... 6
4 References ....................................................................................................................................... 7
5 Contact Information ......................................................................................................................... 7
6 X-Ray Safety .................................................................................................................................... 7
7 Software Overview ........................................................................................................................... 8
7.1 Computer Zones ......................................................................................................................... 8
7.2 Vision Instrument Manager......................................................................................................... 9
7.3 Instrument Manual Control Window ........................................................................................... 9
7.4 Vision Processing ..................................................................................................................... 11
7.5 Mouse Operation ..................................................................................................................... 12
8 Manual Acquisition Overview ......................................................................................................... 12
8.1 Types of Spectra ....................................................................................................................... 12
8.1.1 Introduction ...................................................................................................................... 12
8.1.2 Survey Spectrum ................................................................................................................ 12
8.1.3 High Resolution Spectrum .................................................................................................. 15
2
8.1.4 Snapshot Spectrum............................................................................................................ 18
8.2 Special Sample Considerations.................................................................................................. 21
8.2.1 Insulating Samples ............................................................................................................ 21
8.2.2 Ferromagnetic Samples...................................................................................................... 21
9 Procedure ...................................................................................................................................... 22
9.1 Samples & Loading ................................................................................................................... 22
9.1.1 Sample Handling and Storage ............................................................................................ 22
9.1.2 Outgassing ........................................................................................................................ 23
9.1.3 Mounting Samples ............................................................................................................ 24
9.1.4 Loading Sample Holders .................................................................................................... 27
9.2 Check of Equipment Status & Log-in ......................................................................................... 27
9.2.1 Visual Inspection ............................................................................................................... 27
9.2.2 X-ray Source & Ion Gun Filament Check ............................................................................. 29
9.2.3 Log-in ............................................................................................................................... 30
9.3 Chiller Alarm ............................................................................................................................ 30
9.4 Focussing ................................................................................................................................. 31
9.4.1 Methods ........................................................................................................................... 31
9.4.2 Manual Sample Height Adjustment .................................................................................... 31
3
9.4.3 Auto-z............................................................................................................................... 33
9.5 Acquisition of XPS Spectra ........................................................................................................ 36
9.5.1 Manual Acquisition Panels ................................................................................................. 36
9.5.2 Acquiring Spectra .............................................................................................................. 37
9.5.2.1 Setup ............................................................................................................................................... 37
9.5.2.2 X-Ray Source Warm-up .................................................................................................................. 37
9.5.2.3 Acquisition ....................................................................................................................................... 38
9.5.2.4 Saving Data ..................................................................................................................................... 42
9.6 Wrapping up ............................................................................................................................ 44
9.7 Sample Removal ....................................................................................................................... 45
9.8 Argon Ion Etching in the SAC ................................................................................................... 45
9.8.1 Degassing ......................................................................................................................... 45
9.8.2 Turning On the Ion Gun Gas .............................................................................................. 45
9.8.3 Ion Gun Warm-up ............................................................................................................. 48
9.8.4 Ion Etching ........................................................................................................................ 51
9.8.5 Turning off the Ion Gun & Gas ........................................................................................... 53
9.9 Degassing ................................................................................................................................ 54
9.9.1 X-ray Source...................................................................................................................... 54
9.9.2 SAC Ion Gun ..................................................................................................................... 55
9.10 Ion Pump Cold Trap .............................................................................................................. 57

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1 Purpose
This document describes how to acquire X-Ray photoelectron spectra and perform ion beam etching in the
sample analysis chamber (SAC) of the Kratos Analytical Axis Ultra DLD system. This document is intended
to be a reference for trained users of the system; it is not a substitute for training by staff of the 4D Labs
Nanofabrication Facility. Readers of this document are expected to have a basic familiarity with high vacu-
um systems.
Analysis of XPS spectra is not covered in this document. Both quantification and component analysis are
well described in the Axis Ultra DLD Operator's Manual 1 so users should refer to that document for proce-
dures. In addition, the following modes of the Axis Ultra DLD are not described in this document.
 Automated operation
 XPS imaging
 Secondary Ion Mass Spectroscopy (SIMS)
 Scanning Electron Microscopy (SEM)
 Auger Electron Spectroscopy (AES)
 Scanning Auger Electron Microscopy (SAM)
 Ion Scattering Spectroscopy (ISS)
 Sample heating
 Sample cooling
Anyone interested in these modes should consult with the tool owner.
2 Definitions
AES: Auger Electron Spectroscopy

DLD: Delay Line Detector. The photoelectron detector of the Axis Ultra DLD.
FOV: Field of View. Used in reference to various photoelectron lenses, e.g., FOV1 & FOV2.
FWHM: Full Width at Half Maximum
IMC: Instrument Manual Control. A window in Vision Instrument Manager software.
1
Axis Ultra DLD Operator's Manual, Ch. 7, Kratos Analytical document 39-306, March 2005.
5
LL: Load Lock chamber. Vacuum chamber into which samples are loaded.
SAC: Sample Analysis Chamber. Vacuum chamber used for XPS acquisition.
STC: Sample Treatment Chamber. Vacuum chamber used for SIMS acquisition.
SIMS: Secondary Ion Mass Spectrometry.
S:N ratio: Signal to Noise ratio.
TMP: Turbomolecular pump. A high or ultra-high vacuum pump.
VIM: Vision Instrument Manager. Axis Ultra DLD acquisition software used for XPS.
XPS: X-ray Photoelectron Spectroscopy or X-ray Photoelectron Spectrometer.
3 Conventions
In this document, the following items are italicized.
 Hardware units
 Software menu items
 Software windows and panels
 Software box names
The following items are underlined.
 Hardware buttons and switches

 Software buttons
 Special keyboard keys, e.g., Enter.
Text to be typed is shown inside double quotation marks.
Hazard conventions:
 CAUTION indicates a hazard which may cause damage to equipment.

 WARNING indicates a hazard which may cause injury to personnel. It may cause damage to equip-
ment as well.
6
4 References
 Axis Ultra DLD Operator's Manual, Kratos Analytical, document 39-306, March 2005.
 NIST X-ray Photoelectron Spectroscopy Database (http://srdata.nist.gov/xps/)
 Training folder on the XPS computer.
5 Contact Information
Questions or comments concerning this document or operation of the X-ray Photoelectron Spectrometer
should be directed to the tool owner at 4D Labs Nanofabrication Facility, Simon Fraser University, Burnaby,
BC, Canada. The current tool owner is listed on the web page for the tool on the 4D Labs Nanofabrication
Facility web site.
6 X-Ray Safety
Exposure to X-rays is a health hazard; however, operators of the 4D Labs X-ray photoelectron spectrometer
are well shielded from X-rays and there should be no possibility of significant exposure. X-rays can only be
generated in the sample analysis chamber (SAC) when it is under ultra-high vacuum. Consequently, it not
possible for anyone to place any part of their body directly in the X-ray beam. X-ray intensities outside the
SAC are attenuated to insignificant levels by the stainless steel walls of the vacuum chamber and the lead-
ed glass view ports. All ports on the SAC are sealed with bolts. X-ray intensities outside the SAC are meas-
ured annually or after changes to the SAC to ensure that leakage is at an acceptable level.
Nevertheless, XPS users are encouraged, but not required, to take an X-ray safety training course. Periodi-
cally, Simon Fraser University provides such a course for its faculty, staff, & students. Users are not required
to wear a personal dosimeter but SFU faculty, staff, & students may request one after taking the SFU X-ray
safety training course.
7
7 Software Overview
7.1 Computer Zones
The XPS hardware is controlled by Vision Instrument Manager (VIM) software. In order to mitigate interfer-
ence of the Windows OS or other software applications with control of the XPS hardware, two computer
processing zones are provided.
 XPS Manager: This zone is reserved for Vision Instrument Manager.

 Data Processing: This zone should be used for all other activities, including data processing with Vision
Processing and connection to the Internet.
CAUTION
Running any application, in addition to Vision Instrument Manager, in the XPS Manager zone may cause
Vision Instrument Manager to crash. If this happens, do not attempt to restart VIM yourself; instead, con-
tact the tool owner.
The desired zone may be selected by clicking on the corresponding button at the top of Windows Desktop,
as shown in Figure 7-1.
Figure 7-1: Vision Instrument Manager running in the XPS Manager zone.
Avoid opening Vision Processing in both zones; if this is done, the software will not work correctly.
8
7.2 Vision Instrument Manager
Vision Instrument Manager (VIM) is the software that manages communication between the Kratos Axis
Ultra DLD and the computer. Do not exit from Vision Instrument Manager. If Vision Instrument Manager
window is not running in the XPS Manager zone, contact the tool owner.
7.3 Instrument Manual Control Window
The Instrument Manual Control window is the interface which allows the operator to manually control var-
ious hardware modules. Normally, this window should be left open but, if it is not, users may open it from
the VIM menu bar. Select Window: Manual Window (see Figure 7-2a).
Figure 7-2: a) Opening the Instrument Manual Control window from Vision Instrument Man-
ager. b) The Instrument Manual Control window, showing the modules which can be con-
trolled.
At the top of the Instrument Manual Control window is a list of the modules which can be controlled (see
Figure 7-2b). Modules may be activated or made inactive by left clicking the box next to the module name
at the top of the IMC window. When active, corresponding panels should be open in the IMC window.
At a minimum, the following modules must be active for XPS: Analyser, Acquisition, Xray Gun, Stage, and
Vacuum. In addition, for insulating samples, the Neutraliser module is required. A brief description of each
module follows.
9
The Analyser panel (Figure 7-3) controls the modes of measurement (e.g., imaging or spectroscopy), the
type of lens used to collect and focus emitted photoelectrons, the energy resolution, and the size and
shape of the aperture.
The Acquisition panel (Figure 7-3) permits the user to define the measurement technique, the type of scan,
and the scan parameters. The expandable Energy Regions Table allows the user to create multiple scans
with individual settings, specifically, energy range, energy step size, dwell time per step, and number of
scans to average.
Figure 7-3: Analyser and Acquisition panels of the Instrument Manual Control window.
X-rays are generated by bombarding a target with high energy electrons. The X-ray Gun panel (Figure 7-4)
allows the operator to select the type of X-ray source and both the emission current (Emission) and the
accelerating voltage (Anode HT) of the X-ray generating electrons. The maximum X-ray source power that
should be used is 150 W (Emission ≤ 10 mA and Anode HT ≤ 15 kV). While it is desirable to operate the
X-ray source at maximum power to obtain the best signal-to-noise ratio, bear in mind that, for certain ma-
10
terials, e.g., polymers, sample damage is possible at elevated powers. In such cases, lowering of the emis-
sion current and, perhaps, the accelerating voltage will reduce radiation damage.
Insulating samples will develop positive surface charges due to the escape of photoelectrons, unless the
lost charge is compensated. Sample charging may produce undesirable positive binding energy shifts ~ 10-
100 eV, loss of signal, and signal distortion. Positive charge build-up on insulating samples may be com-
pensated by flooding the sample surface with low energy electrons using the Neutraliser panel (Figure 7-4).
Figure 7-4: X-ray source and Neutraliser panels of the Instrument Manual Control window.
The Stage panel allows the user to move the SAC sample stage. The Vacuum panel allows the user to ob-
serve the vacuum chamber pressures and to turn the SAC ion gun gas on or off.
7.4 Vision Processing
Vision Processing is the software used to process acquisition data. It should only be run in the Data Pro-
cessing zone. Start Vision Processing by double-clicking the corresponding icon on the Desktop. When you
are finished, please close Vision Processing.
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7.5 Mouse Operation
Left mouse button
 Selects data objects and menu items

 Activates software buttons
Mouse wheel
 When rotated: Scrolls through menu lists

 When depressed: Pastes selected objects into the window in which the cursor is located
Right mouse button
 Opens location-specific menus
8 Manual Acquisition Overview
8.1 Types of Spectra
8.1.1 Introduction
The two most common types of spectra are survey and high resolution spectra. In both cases, data are ac-
quired by counting photoelectrons in a relatively narrow energy window for a period of time and stepping
that window through a much wider range. A third type of spectrum discussed in this document is the snap-
shot. As the name implies, data are acquired in one step using a single, relatively wide energy window.
Typical parameters for each of these three types of spectra are listed in the following sections.
8.1.2 Survey Spectrum
Survey spectra cover a wide energy range at low resolution, e.g., a range of 1200 eV with pass energy 160
(FWHM of XPS peaks ≅ 4 eV). The primary purpose of a survey is either qualitative or quantitative deter-
12
mination of the elemental components on the sample surface. It is good practice to start with a survey
spectrum.
Typical settings for a survey spectrum follow (cf. Figure 8-1).
Analyser
 Mode: Spectrum
 Lens: Hybrid.2
 Resolution: Pass energy 160
 Aperture: slot3
Acquisition
 Technique: XPS
 Type: Spectrum
 Energy scale: B.E.
 Ref.: Al (Mono)
Typical spectrum parameters are shown in the Energy Regions Table in Figure 8-1.
X-ray Gun
 Source: Mono (Al)

 Emission (mA): 10 4
 Anode HT (kV): 15
For delicate samples, it may be desirable to reduce the emission current and anode voltage.
Neutraliser
For electrically insulating samples, turn it on.
2
For ferromagnetic samples, use the Electrostatic lens. See Section 8.2.2.
3
When used with the Hybrid lens, the analysis area is a 700 μm x 300 μm rectangle
4
To maintain filament life, do not exceed 10 mA.
13
Figure 8-1: Typical parameters for a survey spectrum of a non-ferromagnetic sample.
14
8.1.3 High Resolution Spectrum
High resolution spectra cover a narrow range, e.g., 10-20 eV, with high resolution. The FWHM of XPS
peaks can be as low as about 0.5 eV with Pass energy 5. The primary purpose of a high resolution spec-
trum is to obtain information about the oxidation state and/or chemical bonding of an element. Depending
on the resolution required and the signal intensity, it may be desirable to sacrifice some resolution in order
to gain intensity by increasing the pass energy.
As the pass energy is reduced, the Step width may also need to be reduced in order to prevent frequency
aliasing.5 As a rule of thumb, FWHM/Step should be ≥ 4.
Typical settings for a high resolution spectrum follow (cf. Figure 8-2).
Analyser
 Mode: Spectrum
 Lens: Hybrid.6
 Resolution: Pass energy 40, Pass energy 20, Pass energy 10, or Pass energy 5.7
 Aperture: slot8
Acquisition
 Technique: XPS
 Type: Spectrum
 Ref.: Al (Mono)
Typical spectrum parameters are shown in the Energy Regions Table in Figure 8-2. For efficient acquisition,
regions should be in descending order of Centre eV in the Energy Regions Table.
5
Frequency aliasing will result in distortion of the peaks in your spectrum.
6
For ferromagnetic samples, use the Electrostatic lens. See Section 8.2.2.
7
The choice depends on the S:N ratio of the signal and desired resolution. The lower the pass energy, the higher the resolution
and the lower the signal intensity.
8
When used with the Hybrid lens, the analysis area is a 700 μm x 300 μm rectangle
15
X-ray Gun

For delicate samples, it may be desireable to reduce the emission current and anode voltage.
Neutraliser
9
16
Figure 8-2: Typical parameters for high resolution spectra of a non-ferromagnetic sample.
17
8.1.4 Snapshot Spectrum
Snapshot spectra are used for rapid, low resolution acquisition over a narrow energy range, typically ~ 20
eV. Typically, a snapshot spectrum is acquired when the area under the peak, rather than the shape of the
peak is of most interest. Common applications are the Auto-z procedure (Section 9.4.3) and depth
profiling.
Typical settings for a snapshot spectrum follow (cf. Figure 8-3).
Analyser
 Mode: Spectrum
 Lens: FOV110
 Resolution: Pass energy 160.
 Aperture: slot
Acquisition
 Technique: XPS
 Type: Snapshot
 Ref.: Al (Mono)
Typical spectrum parameters are shown in the Energy Regions Table in Figure 8-3.
 Width and Step are set by the software and cannot be changed by the operator.
 Dwell time should be substantially longer than is typical for survey and high resolution spectra. For a
strong signal, 3000 ms is usually an appropriate choice.
 Usually #Sweeps should be 1.
X-ray Gun
10
Some lenses, including the FOV1 lens, may not be appropriate for ferromagnetic samples. See Section 8.2.2.
18
For delicate samples, it may be desireable to reduce the emission current and anode voltage.
Neutraliser
11
19
Figure 8-3: Typical parameters for a snapshot spectrum of a non-ferromagnetic sample.
20
8.2 Special Sample Considerations
8.2.1 Insulating Samples
Insulating samples may require charge neutralization to prevent large energy shifts (~ 10 eV), suppression
of the signal, or distortion of the signal. To determine whether charge neutralization is beneficial, compare
spectra with charge neutralization off and on. If the sample is not charging with neutralization off, leave it
off. Turning on charge neutralization when it is not required may degrade the spectrum.
The charge neutralizer may be turned on or off with the corresponding buttons in the Neutraliser panel.
Note that, after turning the neutralizer on or off or after turning the X-ray source on or off, it may take a
few minutes for the surface charge on the sample to stabilize.
8.2.2 Ferromagnetic Samples
Spectra of ferromagnetic samples should be acquired with the Electrostatic lens. The Hybrid, FOV1, and
FOV2 lenses employ a combination of magnetic and electrostatic lenses. Ferromagnetic samples will distort
the field of the magnetic lens, which may produce signal distortion or loss of intensity.
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9 Procedure
9.1 Samples & Loading
9.1.1 Sample Handling and Storage
WARNING
Each user must inform the tool owner of any hazards associated with the user's samples. Note that nano-
particles are considered to be hazardous. If requested by the tool owner, it is the user's responsibility to
supply MSDS or other safety information prior to sample loading. In addition, the tool owner may require
special sample handling or storage procedures. Each user is also responsible for the disposal of their sam-
ples after removal from the XPS system.
1) Samples, tweezers, and sample holders should not be touched by bare hands and they should only be
placed on clean surfaces. Wear powder-free gloves when handling these items.
2) Even though great care is taken to avoid contaminating the sample, airborne contaminants (e.g., car-
bon and sodium) can still easily foul the surfaces of samples during handling. Minimize the amount of
surface contamination by adhering to the following procedures:
a) Only use tweezers to handle samples. Tweezers made from PTFE or non-magnetic stainless steel
are preferred because they are less likely to transfer contaminants to samples and will not magnet-
ize samples.
b) Stainless steel & PTFE tweezers may be cleaned and degreased by successively soaking in acetone,
methanol, and isopropanol baths for 10 minutes each. Acetone leaves residue which outgasses so
it should never be employed in the final cleaning step.
c) In general, cleaning of samples prior to surface analysis should be avoided. If it is desirable to re-
move surface contamination, a bath of high purity, volatile solvent such as isopropanol or hexane
in an ultrasonic bath may be appropriate.
22
d) A filtered N2 spray gun located near the XPS may be used to blow off dust. Do not use compressed
air; it will contaminate the sample surface with oil and water..
3) To minimize surface contamination, store and transport samples in glass jars or wrapped in clean Al
foil. Storage in plastic containers is less desirable due to the risk of contamination by volatile plasticis-
ers released from the container.
9.1.2 Outgassing
Some samples may outgas significantly, especially powders, porous materials, polymers, and liquids. In
such cases, one or more of the following treatments may be necessary to prevent contamination of the
SAC. Treatments are listed in the order of preference.12
 Pump down your sample in a vacuum oven for several hours prior to introduction into the XPS load
lock. A high vacuum or dry roughing pump should be used to prevent backstreaming of pump oil. Set
the oven temperature to the highest temperature that your sample can tolerate, up to about 250°C. If
a vacuum oven is not available or appropriate, baking at atmospheric pressure or pumping at room
temperature are less effective alternatives. Longer baking or pumping times will be required. After re-
moval from the vacuum oven, your samples should be transferred to the XPS load lock chamber as
quickly as possible.
 Keep your sample under vacuum in the XPS load lock for an extended period, e.g., overnight, prior to
transferring it to the SAC.
 Use the SAC ion pump cold trap when the sample is in the SAC (see Section 9.9). Consult the tool
owner in advance if this may be required.
 Cool the LL stage and SAC sample stage. Consult the tool owner in advance if this may be required.
If you are unsure, whether your samples will outgas significantly, consult the tool owner in advance. If, af-
ter introducing your sample, more than 10 min is required for the LL to reach 5 x 10-6 Torr, your sample is
probably outgassing significantly.
12
That is, wherever possible, use treatments higher on the list.
23
9.1.3 Mounting Samples
All samples must be mounted on a sample holder, of which there are 3 basic types.
 15 mm diameter copper stubs (see Figure 9-1)

 130 mm x 15 mm standard bars (see Figure 9-2)
 130 mm x 15 mm constant height bars (see Figure 9-3)
Figure 9-1: Sample stub. a) Top view. b) Side view. The red arrow points to the groove for
the spring clip. c) Top view of a stub with a foil sample held by a spring clip.
Figure 9-2: Standard sample bar. a) Top view. b) Side view. c) Sample held by copper strips.
d) Samples held by double-side carbon tape.
24
Figure 9-3: Constant height sample bar.
Maximum sample dimensions are listed in Table 9-1; however, preferably, the sample should not extend
beyond the edge of the bar or stub.
Table 9-1: Maximum sample dimensions.
Mounting Method Width Length Thickness

(mm) (mm) (mm)
Stub 25 40 4
Standard Bar 25 100 4
Constant Height Bar 25 30 8
CAUTION
If the sample extends beyond the sample holder, use great care when moving the sample. Damage to the
instrument, especially the dual anode X-ray source, may result from a collision.
Samples may be mounted on stubs using spring clips, which slide into the uppermost groove of the stub
(see Figure 9-1b & Figure 9-1c) or vacuum-compatible double-sided tape. Both carbon tape (electrically
conductive) and masking tape (electrically insulating) are available. Both types of tape outgas significantly
so clips are preferred, if suitable. Minimize the amount of tape used, e.g., ≤ 2 x 2 mm2. Do not use the
special stubs with grating embedded.
25
Thin samples may be clamped to standard bars (see Figure 9-2) by copper strips or bonded with vacuum-
compatible double-sided tape. Copper strips may be removed to accommodate longer samples.
A variant of the bar called the constant height bar (see Figure 9-3) can accommodate thick samples. Sam-
ples are clamped by spring-loaded disks. Ensure that the disk surface is horizontal or the bar may distort
and be difficult to transfer to or from the SAC stage. In addition, XPS measurements may be degraded.
Spacers may be added to make a disk horizontal.
Unless they are electrically conductive and grounded to the sample holder, samples exposed to X-rays or
ion beams will be subject to charging, which may result in a number of undesirable effects: binding energy
shifts, peak distortion, and reduction in signal intensity. Although these effects can be mitigated by turning
on the charge neutralizer, it is preferable to avoid them altogether. Consequently, electrically conductive
substrates are preferred for electrically conductive films. Such substrates should be grounded to the sample
holder. If the substrate is non-conductive, a conductive film may be grounded to the sample holder using a
copper clip or conductive tape (copper or carbon).
For insulating samples, masking tape may be preferred to carbon tape because conductive tape may result
in greater charging non-uniformity.
Fine powders may be suspended in an appropriate solvent, dropped onto a substrate (preferably electrically
conductive), and allowed to dry. Choose a volatile solvent which will not leave residue. Do not drop a sus-
pension directly onto a sample holder. Ensure that the sample has dried thoroughly before loading into the
XPS system. Baking in a vacuum oven may be desirable, especially if the solvent is water.
Coarse powders may be pressed into vacuum-compatible double-sided tape or indium foil.
Some stubs have a well for liquid, powder, or granular samples (see Figure 9-4). Powders should be held
within the well of the stub by bonding them to a small strip of vacuum-compatible double-sided tape (e.g.,
carbon tape or masking tape). Otherwise, they may blow off during pump down or venting in the load lock.
26
After mounting a sample, always check that the sample is secured by tilting and gently shaking the sample
holder.
Figure 9-4: Stub with a well in the top surface for powder and granular samples.
9.1.4 Loading Sample Holders
Loading sample holders into the load lock chamber and transferring them into the SAC are risky opera-
tions, which may only be performed by Nanofab staff. Users are advised to make arrangements with the
tool owner at least one day in advance.
9.2 Check of Equipment Status & Log-in
9.2.1 Visual Inspection
Before operating the Axis Ultra DLD, check that:
1) The system status sign reads "UP".

2) The STATUS indicator on the Controller Processor Unit displays "d.3", with the period flashing (see
Figure 9-5).
27
Figure 9-5: STATUS display on the Control Processor Unit.
3) Chilled water temperature = 20 ±1°C.

4) Chilled water pressure at the outlet of the water filter is ≥ 68 psi (X-ray source off).13
5) SAC pressure ≤ 1 x 10-8 Torr and STC pressure ≤ 5 x 10-7 Torr (see Figure 9-6).
13
With the monochromatic Al X-ray source on, the pressure at the outlet of the water filter should be ≥ 58 psi.
28
Figure 9-6: Vacuum panel of the Instrument Manual Control window. Idle mode.
Proceed with data acquisition only if all of the above conditions are satisfied. If any anomalies are ob-
served, contact the tool owner. Do not proceed until the issue is rectified.
9.2.2 X-ray Source & Ion Gun Filament Check
Open the XPS user log (Excel spreadsheet), e.g., by double clicking the icon on the Windows Desktop. De-
termine the last time that the X-ray source and ion gun (if required) filaments were used. There is one
monochromatic X-ray source filament and two ion gun filaments, denoted SAC1 and SAC2, but only one of
the latter is needed. In either case, if more than two weeks has elapsed since the filament was used, it
must be degassed before use.
29
CAUTION
Failure to degas a filament that has not been used for more than 2 weeks may result in damage to the fil-
ament and contamination of your spectra and those of future users. Filament replacement is an expensive
(thousands of dollars) and lengthy (≥ 2 weeks) repair.
You may degas a filament yourself (see Section 9.9 for the X-ray source and Section 9.9.2 for the SAC ion
gun) or request that the tool owner degas the filaments. In either case, there is no charge. Degassing the
X-ray source filament takes most of a day, whereas degassing an ion gun filament takes about 35 min.
9.2.3 Log-in
Log-in on the XPS user log. Include the techniques to be used (XPS, etch, etc.) and whether any of the fol-
lowing will be required: ion beam etching, LN2, or sample loading & unloading.
Any problems that you encounter should be recorded briefly in the Comments column of the user log and
the tool owner should be informed. Detailed problem descriptions should be recorded in the log book, lo-
cated in the drawer of the computer monitor desk.
Create a ticket on the Nanofab web site.
9.3 Chiller Alarm
CAUTION
If, at any time, the chiller alarm sounds (a continuous, piercing tone), immediately turn off the X-ray
source. If the ion gun is on, turn off the ion gun and press the Ion Gun Gas Off button (Section 9.8.5). Si-
lence the obnoxious alarm by turning off the chiller power switch. Inform the tool owner as soon as possi-
ble.
30
9.4 Focussing
9.4.1 Methods
After your sample is loaded into the SAC, adjust the sample height so that the photoelectrons emitted from
the sample surface are focussed on the detector. There are two focussing methods:
 Manual sample height adjustment

 Auto-z
Manual sample height adjustment should always be performed at your first sample position and may be all
that is required. This method relies on the fact that the camera focal point has been adjusted to be the
same as the photoelectron detector focal point.
Auto-z is an automated procedure in which the sample height (Z) is varied incrementally above and below
the starting height and a snapshot spectrum is measured at each position.14 The peak area is automatically
calculated at each position; the optimum Z is the value for which this area is maximized.
Auto-z is useful if you have difficulty focussing using the manual method, e.g., your sample surface is very
clean and smooth so there are no features to focus on, except the edges of the substrate. It is also useful
when measurements are performed at several (lateral) positions for which the height of the sample surface
is approximately the same. The initial height should be close to the optimum height so focus by the manual
method first.
9.4.2 Manual Sample Height Adjustment
After the sample holder has been transferred into the SAC, adjust the sample height so that the camera is
focussed on the sample surface, as described below. The CCD camera image is displayed on the video
monitor on top of the XPS electronics cabinet.
14
Axis Ultra DLD Operator's Manual, Kratos Analytical, document 39-306, Section 4.8.4, March 2005.
31
1) Minimize the camera magnification, using the thumb wheel on the right side of the camera, just above
the mounting flange.
2) On the Stage panel of the IMC, check that the Calibrated button is green. If not, contact the tool own-
er. Do not proceed until the stage has been calibrated.
CAUTION
Do not attempt to calibrate the stage yourself. Damage to the instrument, especially the dual anode X-ray
source, may result from a collision.
3) Use the SAC stage X and Y controls to position your sample laterally under the camera. If possible,
adjust the X and Y positions so that there is a defect, which you can focus on, in the field of view.
4) Use the SAC stage Z control to position the sample so that the best focus lies approximately in a diag-
onal band from the top left corner of the video monitor to the bottom right corner. If the upper right
has better focus, move down. If the lower left has better focus, move up. Don't bother focussing pre-
cisely at low magnification; fine tuning the focus is best done at the highest magnification.
5) Increase the camera magnification a little.
6) Repeat steps 3) -5) until you have good focus in the diagonal band at the maximum magnification.
7) If desired, save the sample position in the Position table, located in the Stage panel, as follows. This is
recommended if you intend to acquire spectra in more than one location.
a) In the Stage panel, press the Add button. The coordinates of the current SAC stage position will be
inserted in a row immediately below the existing entries in the stage Position table.15
b) Change the name of the new position to something meaningful & click Enter (optional).
c) Save the position table in the C:\Stage Positions directory by clicking Save Table (optional). Include
your name or initials in the file name.
15
More precisely, the current position is copied to a new row, which is inserted above the uppermost empty row.
32
9.4.3 Auto-z
Perform the Auto-z procedure as follows.
1) Position your sample laterally so that the analysis position is in the centre of the video monitor (at the
red dot).
2) Adjust the sample height approximately to the camera focal point (see Section 9.4.2: Manual Sample
Height Adjustment).
3) Save the sample position in the Position table, located in the Stage panel, as follows.
a) In the Stage panel, press the Add button. The coordinates of the current SAC stage position will be
inserted in a row immediately below the existing entries in the stage Position table.16
b) Change the name of the position to a meaningful name & click Enter (optional).
c) Save the position table in the C:\Stage Positions directory by clicking Save Table. Include your
name or initials in the file name.
4) Turn on the charge neutralizer, if required (see Section 8.2.1).
5) If you know the position of a strong XPS peak from your sample, jump to step 6). Otherwise, do the
following.
a) Collect a survey spectrum (see Section 9.5: Acquisition of XPS Spectra)
b) Select any strong peak in the spectrum, e.g., O 1s.
6) Type the spectral parameters of the desired XPS peak, e.g., O 1s, into a row of the Energy Regions Ta-
ble of the Acquisition panel, as follows. After typing each entry, press Enter.
a) Region Name: name of the desired XPS peak, e.g., "O 1s".
b) Centre: energy of the desired XPS peak.
c) Ignore the Width & Step values.17
d) Dwell: 3000 ms.
e) # Sweeps: 1.
16
More precisely, the current position is copied to a new row, which is inserted above the uppermost empty row.
17
When the acquisition Type is set to Snapshot, the Width & Step values will be set automatically.
33
7) Ensure that the desired XPS peak is the only active row in the Energy Regions Table.
8) Set up a snapshot spectrum acquisition using the following parameters.
Analyser
 Mode: Spectrum
 Lens: FOV1
 Resolution: Pass energy 160
 Aperture: slot
Acquisition
 Technique: XPS
 Type: Snapshot
 Ref.: Al (Mono)
X-ray Gun

 Emission (mA): 10
For delicate samples, it may be desirable to reduce the emission current and anode voltage.
9) Set the X-ray source to On.

10) Ensure that the current position is selected in the Position table.
11) Ensure that the Auto-z panel of the Stage panel is open (see Figure 9-7).
34
Figure 9-7: Stage panel with Auto-z panel open.
35
12) Enter the desired parameters in the Auto-z panel. Usually, the default parameters are satisfactory. Af-
ter typing each entry, press Enter.
a) No. Increments should be odd.
b) Ordinate Choice should be Area.
13) Click Grab Scan.18
14) Click Optimize. Auto-z should commence.
15) Wait for Auto-z to complete.19 On completion, a data object named Auto-z should be created in the
data region of VIM and the sample stage should have moved to the optimized Z value.
16) If desired, save the Position table by clicking Save Table.
17) The results of the optimization (peak area vs. Z) may be viewed by selecting the Auto-z data object and
pasting it into the Real-Time Display window.
18) If the optimum Z is at either end of the range, repeat the Auto-z procedure.
9.5 Acquisition of XPS Spectra
9.5.1 Manual Acquisition Panels
Manual data acquisition is controlled from various panels in the Instrument Manual Control (IMC) window.
Panels may be activated or de-activated from the toolbar at the top of the IMC window. To simplify opera-
tion and reduce the chance of errors, it is recommended that only the required panels be active.
The following panels should always be active.
 Vacuum
 Stage
18
Ignore the Centre and Width values in the Auto-z panel. These should correspond to the values in the active row of the Energy
Regions Table, but due to a software bug, usually they do not. Nevertheless, the Auto-z procedure should use the correct values.
Check by observing the snapshot spectra in the Real-Time Window during optimization.
19
Progress may be observed on the Status panel.
36
For X-ray photoelectron spectroscopy, the following panels are required.
 Analyser
 Acquisition
 X-ray Gun
 Neutraliser – only for insulating samples
The following sections describe the parameter settings for a few basic types of spectra.
9.5.2 Acquiring Spectra
9.5.2.1 Setup
Before acquiring a spectrum, check the following.
1) At the bottom of the Analyser panel, both Analyser and Channelplate are in standby mode. If not,
press the Set Standby button. Both should now be in standby mode.
2) At the top of the Stage panel, the Calibrated button is green. If not, contact the tool owner.
CAUTION
Do not attempt to calibrate the stage yourself. Damage to the instrument, especially the dual anode X-ray
source, may result from a collision.
3) SAC pressure < 5 x 10-8 Torr. Do not turn on the X-ray source, if it is higher.
9.5.2.2 X-Ray Source Warm-up
When the X-ray source is turned on for the first time each day, it should be warmed up gradually as fol-
lows. Here, it is assumed that the desired settings are emission current = 10 mA and anode HT = 15 kV. If
your desired values are lower, stop at the lower values.
37
CAUTION
Monitor the SAC pressure throughout the warm-up procedure. If, at any time, the SAC pressure exceeds 2
x 10-8 Torr, immediately reduce X-ray source Emission to 1 mA and Anode HT to 6 kV. In extreme cases,
turn the X-ray source off. When the SAC pressure has dropped below 1 x 10-8 Torr, it is permissible to re-
start the warm-up procedure from the beginning. If the SAC pressure exceeds 2 x 10-8 Torr a second time,
turn off the X-ray source and degas it (see Section 9.9).
1) Ensure that the ion gun gas is off.

2) Ensure that SAC pressure < 1 x 10-8 Torr.
3) Go to the the X-ray Gun panel.
4) In the Emission (mA) box, type "1", then Enter.
5) In the Anode HT (kV) box, type "10", then Enter.
6) Click the X-ray source On button. Monitor the SAC pressure.
7) Allow the current and voltage to ramp up to the setpoints and, then, continue to monitor the SAC
pressure for 1 minute.
8) Gradually increase Anode HT to 15 kV in 1 kV increments, while monitoring the SAC pressure.
9) Gradually increase Emission to 10 mA in 1 mA increments, while monitoring the SAC pressure.
Later in the same day, if the X-ray source is turned on again after being off, warm-up is not required. In-
stead, Emission and Anode HT may be set to the desired values immediately. Monitor the SAC pressure.
9.5.2.3 Acquisition
Acquire spectra as follows.
1) Ensure that the ion gun is either off or in standby mode.

2) Ensure that SAC pressure < 3 x 10-8 Torr. Ion gun gas may be on, provided that this pressure condition
is satisfied.
38
3) If charge neutralization is desired, turn it on by clicking On in the Neutraliser panel.

4) Set the desired parameters in the Analyser & Acquisition panels, as described in Section 8: Manual Ac-
quisition Overview. For convenience, typical parameters for survey and high resolution spectra are re-
produced in Figure 9-8 & Figure 9-9, respectively.
Figure 9-8: Typical parameters for a survey spectrum of a non-ferromagnetic sample.

39
Figure 9-9: Typical parameters for high resolution spectra of a non-ferromagnetic sample.
5) In the X-ray Gun panel:
40
a) In the Emission (mA) box, type the desired value, then Enter. Do not exceed 10 mA.20
b) In the Anode HT (kV) box, type the desired value, then Enter. Do not exceed 15 kV.21
c) Press the On button.
d) Wait for the X-ray Gun panel On button to turn green.
6) In the Acquisition panel:
a) Ensure that only the desired spectra in the Energy Regions Table are active.
b) Press the On button. It should turn green and acquistion should commence.
c) Press the Off button.22 It should flash amber until acquisition is completed.
7) At least once every hour, check the following. If anything is amiss, turn off the X-ray source & contact
the tool owner.
a) SAC pressure ≤ 5 x 10-8 Torr.
b) Chilled water temperature = 20 ±1°C.
c) Chilled water pressure at the outlet of the water filter ≥ 58 psi (X-ray source on).23
CAUTION
If, at any time, the chiller alarm sounds (a continuous, piercing tone), immediately turn off the X-ray
source. If the ion gun gas is on press the Ion Gun Gas Off button (Section 9.8.5). Silence the obnoxious
alarm by turning off the chiller power switch. Inform the tool owner as soon as possible.
To observe your spectra as they are acquired:
20
For X-ray sensitive samples, a lower value may be desirable.
21
For X-ray sensitive samples, a lower value may be desirable.
22
Pressing the Off button will cause the acquisition to terminate when all of the sweeps in the active scans in the Energy Re-
gions Table have completed and the spectra will be saved in volatile memory. Otherwise, when all of the scans are completed,
they will be deleted and a new set of scans will commence.
23
With the monochromatic Al X-ray source off, the pressure at the outlet of the water filter should be ≥ 68 psi.
41
1) Activate the VIM window.

2) From the VIM menu, select View: Real-Time Display. The Real-Time Display window should open.
3) Ensure that no data objects in the Data Review panel are selected. If any are, de-select them by click-
ing in the background of the Data Review panel.
To abort an acquisition immediately:
1) Go to the Acquisition panel of the IMC window.

2) Click the Restart button.
Completed sweeps are stored in volatile memory and data objects are created for each scan. Any sweep in
progress is discarded.
When the acquisition is completed:
 In the Acquisition panel, the Off button will be green and the On button will be grey.
 The X-ray source will remain on.
If you remain in the room and expect to acquire more spectra, the X-ray source may be left on. Otherwise,
place the X-ray source in standby mode or turn it off.
To view acquired spectra in the Real-Time Display window:
1) Use the left mouse button, to select the corresponding data objects in the Data Review panel of the
VIM window.
2) Move the mouse cursor to the Real-Time Display window and press the mouse wheel (Paste button).
3) Scroll through the spectra using the scroll bar on the right side of the Real-Time Display window.
9.5.2.4 Saving Data
Acquired data are temporarly saved as data objects in volatile memory. Data may be saved to the hard disk
as follows.
42
1) Ensure that Acquiring is selected just above the Data Review panel of the Vision Instrument Manager
window (see Figure 9-10a). The Save… button should appear immediately to the right (Red arrow #2
in Figure 9-10a).
Figure 9-10: Saving data objects in Vision Instrument Manager. a) Vision Instrument Manag-
er window, showing 1. Selected data objects and 2. Save… button. b) Save Selection win-
dow.
2) Select the data objects to be saved in the Data Review panel of the Vision Instrument Manager
window (Red arrow #1 in Figure 9-10a).
3) Click the Save… button. The Save Selection window should open (Figure 9-10b).
4) In the Directories panel of the Save Selection window, navigate to your directory.24 The datasets in your
directory should appear in the Files panel. 25
5) Either
a) Select the dataset to which the data are to be saved in the Files panel.
or
b) Type the name of a new or existing dataset in the Selection box.
6) Click OK. The new data objects will be appended to any existing data.
24
To move up one level in the directory hierarchy, double click the item in the Directories panel that ends in "..".
25
If your dataset does not appear in the Files panel, try clicking the Update button.
43
9.6 Wrapping up
1) Ensure that all of the following are off.

a) X-ray source
b) Neutralizer
c) Ion gun
d) Ion gun gas (see Section 9.8.5)
2) Click Clear All Rows in the Energy Regions Table.
3) Return the Analyser to the settings for a survey spectrum (see Section 8.1.2: Survey Spectrum).
4) Delete any positions that you added to the Positions table in the Stage panel.
5) Ensure that all of data objects you wish to keep have been saved to a dataset.
6) Delete your data objects from Vision Instrument Manager as follows.
a) Right click in the background of the Data Review section. A menu should open.
b) Left click Close Dataset in the menu.
7) If desired, data objects may be exported to ASCII files for analysis with other software. This must be
done for each data object individually.
a) In Vision Processing, open the relevant dataset.
b) Select the desired data object.
c) Paste the data object into the Display Window.
d) Right click anywhere in the Display Window. A menu should open.
e) Select Export to ascii.
f) Navigate to your data directory.
g) Type the ASCII file name, including the file extension .ascii. Otherwise, the file name will have no
extension.
8) Close Vision Processing.
9) Copy your data to your own storage medium, e.g., USB drive.
10) Complete your record in the XPS user log.
11) Complete your ticket on the Nanofab web site.
12) Inform the tool owner that your samples are ready to be removed.
44
9.7 Sample Removal
Transferring sample holders from the SAC into the load lock chamber and unloading them from the load
lock are risky operations, which may only be performed by Nanofab staff. Users are advised to make ar-
rangements with the tool owner in advance.
After the sample holder has been removed from the load lock, remove your samples from the holder. Clean
the holder and tweezers. Wiping with a lint-free tissue, dampened with isopropanol, is usually sufficient.
Return the holder to its case and the tweezers to their drawer. Take your samples with you even if you no
longer require them; it is your responsibility to dispose of them appropriately.
9.8 Argon Ion Etching in the SAC
9.8.1 Degassing
If the ion gun filament has not been used for more than 2 weeks, it must be degassed before use. You may
either:
 Request that the tool owner degas the ion gun for you. In this case, you are advised to inform the tool
owner at least one day in advance of your reservation.
 Degas the ion gun yourself. See Section 9.9.2.
9.8.2 Turning On the Ion Gun Gas
CAUTION
Excessive gas flows will cause the SAC ion pump current to rise rapidly. This may blow a fuse, causing the
ion pump to turn off, and possibly damage the ion pump. If this occurs, close the CVT valve immediately,
activate the automatic sequence Ion Gun Gas Off, and contact the tool owner.
45
For ion etching, it is necessary to have a small flow of Ar gas into the ion gun to provide a source of ions.
This section describes how establish such a flow.
1) Ensure that the X-ray source is off or in standby mode.

2) Ensure that the ion gun is off.
3) Ensure that the manually operated CVT valve, just behind the ion source is closed.
4) Ensure that both:
a) STC pressure ≤ 5 x 10-7 Torr.
b) SAC pressure ≤ 1 x 10-8 Torr.
5) In the Vacuum panel, activate Automatic Sequences, as shown in Figure 9-11.
Figure 9-11: Vacuum panel in idle mode. Automatic Sequences is active, as indicated by the
red arrow.
46
Figure 9-12: Vacuum panel after completion of Ion Gun Gas On sequence.
6) Select the Ion Gun Gas On button in the Automatic Sequences panel to flow argon gas into the ion
gun.
7) Wait for the sequence to complete. On completion, the Vacuum panel should look like Figure 9-12.
8) Adjust the ion gun gas flow with the manually operated CVT valve until SAC pressure ≅ 1-2 x 10-8
Torr, as follows. 26 Do not allow SAC pressure to exceed 5 x 10-8 Torr during this procedure.
a) Initially, the CVT valve should be closed. (Setting = 7 at 3 o'clock).
b) Set up the Magnifier application so that you can read both the STC and SAC pressures on the
computer monitor while you adjust the CVT valve.
26
CW rotations reduce the gas flow and CCW rotations increase it.
47
c) While watching the STC and SAC pressures, rotate the CVT valve 0.8 turns CCW to a setting of 5
(at 3 o'clock). Probably there will have been no change in the SAC pressure but the STC pressure
may have risen slightly.
d) Wait for the STC and SAC pressures to stabilize.
e) While watching the STC and SAC pressures, slowly rotate the CVT valve another 0.1 turns CCW
to a setting of 6 (at 3 o'clock). There should be a significant rise in the STC pressure but the SAC
pressure should still be below 1 x 10-8 Torr.
f) Wait for the STC and SAC pressures to stabilize.
g) While watching the STC and SAC pressures, very slowly rotate the CVT valve CCW until SAC
pressure ≅ 1-2 x 10-8 Torr. STC & SAC pressures will change rapidly in this region so it
important to proceed carefully. Typically, SAC pressure ≅ 2 x 10-8 Torr when the CVT valve is
1 turn CCW from the closed position, i.e., at a setting of 7 (at 3 o'clock). If the SAC pressure ex-
ceeds 1 x 10-7 Torr, close the CVT valve immediately, activate the automatic sequence Ion Gun Gas
Off, and wait for the SAC pressure to drop below 1 x 10-8 Torr. Then, you can start again from the
beginning of this section. If the SAC pressure rises to more than 5 x 10-7 Torr, contact the tool
owner.
CAUTION
Do not operate the X-ray source if SAC pressure > 5 x 10-8 Torr. Otherwise, the X-ray source may become
contaminated and be damaged.
9.8.3 Ion Gun Warm-up
The ion gun should be warmed up slowly, the first time that it is turned on each day. Only perform this
procedure, if the ion gun has been turned on or degassed within the last 2 weeks; however, if the ion gun
was degassed earlier the same day, it need not be warmed up.
48
In this section, unless otherwise noted, all operations are performed in the Ion Gun panel. It is assumed
that the ion gun is off but the ion gun gas is on (Section 9.8.2).
1) In the Ion Gun panel (Figure 9-13) activate Table to display a list of pre-set ion gun parameters. Scroll
down the list and select a suitable setting.
2) Click Restore Row at the top of the Table panel. The parameters selected in the Table panel, should be
copied into the Settings panel.
Figure 9-13: Ion Gun panel with the Settings, Table, & Status panels displayed. The
"4kv_small spot" ion gun settings are selected.
3) Activate Tuning to open the Tuning panel. Observe which ion gun filament is selected and record it in
the Ion Gun Filament column of the XPS user log as either SAC1 or SAC2. Do not adjust any parame-
ters in the Tuning panel, except the Filament Current Limit as described below.
49
4) Make a note of the value of the Filament Current Limit; it should be in the range 2.5 – 3.0 A. If it is >
3.0 A, inform the tool owner. Filament Current Limit should never exceed 3.0 A.
5) Set the Filament Current Limit to 1.5 A.
6) Set the ion gun to standby mode. Filament current27 should slowly ramp up after a short period.
7) Monitor the SAC pressure. If it exceeds 5 x 10-8 Torr, turn the ion gun off, activate the automatic se-
quence Ion Gun Gas Off, close the CVT valve, return Filament Current Limit to its original value (≤ 3.0
A), and degas the ion gun, as described in Section 9.9.2. After degassing the ion gun, turn the ion gun
gas on (Section 9.8.2). Then, you may skip this section and proceed directly to ion etching (Section
9.8.4).
Figure 9-14: Ion Gun panel with the Status table open. Red arrows indicate the actual values
of the Emission Current and Extractor current. The black arrow indicates the Raster Size
scroll bar.
27
Filament/(A) in the Status table.
50
8) Monitor the ion gun parameters in the Status table in the Ion Gun panel (Figure 9-13).
9) When the filament current reaches 1.5 A, wait 2 min.
10) Increase the Filament Current Limit incrementally to its original value (≤ 3.0 A) in 0.1 A steps. Wait at
least 30 s after each change for the ion gun parameters, especially Emission Current and Extractor cur-
rent, to stabilize (see Figure 9-14). Be especially attentive, when the Filament Current Limit ≥ 2.0 A.28
11) Once the Filament Current Limit has reached its original value (≤ 3.0 A) and the ion gun parameters
have stabilized, deactivate Tuning to close the Tuning table.
12) If the extractor current29 is at its setpoint30 and emission current ≅ 15-25 mA, proceed to step 13).
Otherwise, proceed as follows.
a) If the extractor current equals its setpoint and the emission current < 15 mA, close the CVT valve
slightly (CW rotation) and wait for the ion gun parameters to stabilize. Repeat until emission cur-
rent ≥ 15 mA.
b) If the emission current > 25 mA, open the CVT valve slightly (CCW rotation) and wait for the ion
gun parameters to stabilize. Repeat until emission current ≤ 25 mA.
13) Leave the ion gun in standby mode until you are ready to begin etching.
After ion gun warm-up, the CVT valve may be closed partially or fully to reduce the SAC pressure, in order
to acquire a spectrum.
9.8.4 Ion Etching
This section describes the procedure for ion etching a sample. It is assumed that:
 the ion gun gas is on (Section 9.8.2),

 the ion gun was warmed up (Section 9.8.3) or degassed (9.9.2) earlier in the day, and
 the ion gun is in standby mode.
28
Emission current is limited to 30 mA.
29
Status panel.
30
Settings panel.
51
If any assumption is invalid, rectify the situation before proceeding.
1) Ensure that the X-ray source is either off or in standby mode.

2) For insulating samples, ensure that the neutralizer is on.31
3) In the Ion Gun panel (Figure 9-13) select Table to display a list of pre-set ion gun parameters. Scroll
down the list and select “4kv_small spot” for deep etching or "duster" to remove surface contamina-
tion.
4) Click Restore Row at the top of the Table panel. The selected Table parameters should be loaded into
the Settings panel.
5) Wait until the ion gun parameters stabilize.
6) If the extractor current32 is at its setpoint33 and emission current ≅ 15-25 mA, proceed to step 7). Oth-
erwise, proceed as follows.
a) If the extractor current equals its setpoint and the emission current < 15 mA, close the CVT valve
slightly (CW rotation) and wait for the ion gun parameters to stabilize. Repeat until emission cur-
rent ≥ 15 mA.
b) If the emission current > 25 mA, open the CVT valve slightly (CCW rotation) and wait for the ion
gun parameters to stabilize. Repeat until emission current ≤ 25 mA.
7) Type the size of the area to be etched in the Raster Size (mm x mm) box.34 Note that the nominal etch
rate, which appears in the row above, will change with the raster size.35
8) When you are ready to begin etching do the following.
31
For insulating samples, ions will be deflected from the region to be etched if it is not neutralized.
32
Status panel.
33
Settings panel.
34
Bear in mind, that there will be contamination near the edges of the etch pit so the dimensions of the etch pit should be sub-
stantially larger than those the XPS analysis region. Ideally, the raster dimension should be at least ten times the dimensions of
the analysis region. If your signal is weak and contamination is less of an issue for you, you may wish to reduce this to a factor
of as little as three.
35
Listed etch rates were measured for Ta2O5. Other materials will etch at substantially different rates. Oxides and nitrides gener-
ally have relatively low Ar ion etch rates. Metals and polymers typically have Ar ion etch rates 3-10 times higher.
52
a) Switch the ion gun on.

b) When the On button becomes green, start the timer. Ion etching commences.36
9) During etching, continue to monitor the emission current. If it reaches its upper limit of 30 mA, you
may wish to increase the gas pressure by opening the CVT valve slightly.37
10) Terminate etching by setting the ion gun either to standby mode or to off. If you have no more etching
to do, turn off the ion gun and ion gun gas as described in Section 9.8.5.
If you plan to acquire a spectrum, you may need to reduce the SAC pressure by closing the CVT valve
somewhat. Wait until SAC pressure < 3 x 10-8 Torr before turning on the X-ray source.
9.8.5 Turning off the Ion Gun & Gas
On completion of all of your ion etching, turn off the ion gun as follows.
1) Ensure that the ion gun is off.

2) In the Automatic Sequences panel, select Ion Gun Gas Off. Automatic Sequences must be active.
3) Wait for the sequence to complete.
4) Close the CVT valve.
Wait until SAC pressure < 3 x 10-8 Torr before turning on the X-ray source.
36
Actually, etching commences a few seconds later when Source HT, Align X1, and Align X2 have reached their final values. For
accurate etch times, start the timer at this point.
37
If the emission current reaches 30 mA, you lose control of the extractor current and the etch rate.
53
9.9 Degassing
9.9.1 X-ray Source
If the X-ray source has not been used for more than 2 weeks (check the user log), its filament must be
degassed before the gun is turned on (see Section 9.2.2). Warm-up is not an acceptable substitute for
degassing in this case.
Figure 9-15: Vacuum panel of the Instrument Manual Control window. Idle mode.
54
Degas the X-ray sources as follows. It will take most of a day.38
1) Ensure that the ion gun gas is off (Section 9.8.5); valve states and vacuum conditions should be as
shown in Figure 9-15.
2) Ensure that SAC pressure < 2 x 10-8 Torr.
3) Go the the X-ray Gun panel in the IMC window.
4) Open the Degas panel.
5) In the Degas panel, click the Degas button. It should turn green.
6) Wait until the Degas button turns grey, indicating that degassing is complete.
9.9.2 SAC Ion Gun
If the ion gun filament has not been used for more than 2 weeks, it must be degassed before use. For this
reason, if you wish to use the ion gun, you are strongly advised to inform the tool owner at least one day
in advance of your reservation. Otherwise, you may be delayed while you wait for the ion gun to be de-
gassed.
Degas the SAC ion gun as follows. Ion gun gas should be off during degassing.
1) On the Vacuum panel, check the following valve states.

a) Closed: LL-STC gate valve, STC-SAC gate valve, V19, V2, V5, V8, & V9.
b) Open: V20 & V3.
If you observe any differences, activate Automated Sequences mode, press the Ion Gun Gas Off button,
and wait for the sequence to complete. Check the valve states again. If they are still incorrect, contact
the tool owner.
2) Activate Safe Manual mode.
3) Open valve V2. The vacuum schematic should appear as in Figure 9-16.
4) In the Ion Gun panel, activate the Degas panel.
38
All 3 X-ray sources are degassed sequentially, starting with the monochromatic Al source.
55
5) Click the Degas button. It should turn green.

6) Wait for the ion gun degassing sequence to complete – a little more than 30 min.
7) Close valve V2.
8) Activate Automated Sequences mode.
Figure 9-16: Vacuum panel with V2 open.
56
9.10 Ion Pump Cold Trap
The ion pump cold trap should be kept full if the SAC contains samples which outgas a lot. Fill the ion
pump cold trap as follows. Wear safety glasses and insulating gloves.
Figure 9-17: Liquid nitrogen dewar connected to ion pump cold trap fill line.
1) Below the load lock there is a white plastic tube with a white coupling. Attach the coupling to the end
of the siphon in the liquid nitrogen (LN2) dewar (Figure 9-17).
2) Attach the ¼" OD polyethylene tube from the N2 gas cylinder to the small brass valve on the side of
the siphon, using a rubber hose.
57
3) Open the valves on the N2 gas cylinder and ensure that the pressure is set to 8-10 psi. Do not exceed
10 psi static pressure.
4) Open the small brass valve on the LN2 dewar siphon to pressurize the LN2 dewar.
5) Open the large silver valve on the LN2 dewar siphon. LN2 should begin to transfer to the cold trap. Do
not leave the LN2 dewar unattended during LN2 transfer.
6) When the cold trap is full, close the large silver valve on the LN2 dewar outlet tube. LN2 spewing from
the cold trap exhaust hose indicates that the cold trap is full. Do not overfill. The initial fill takes about
10 min.
7) Close the small brass valve on the side of the siphon.
8) Refill the cold trap with LN2 every hour.39
CAUTION
Failure to fill the cold trap with liquid nitrogen every hour may result in increased SAC pressure and con-
tamination of the vacuum chamber. If the SAC pressure is above 5 x 10-8 Torr, the X-ray source must not
be turned on.
When you are finished all LN2 transfers, do the following.
1) Ensure that both valves on the LN2 siphon are closed.

2) Close both shut-off valves on the N2 gas cylinder.
3) Remove the plastic tube from the end of the LN2 siphon.
4) Remove the rubber hose from the ¼" OD polyethylene tube connected to the N2 gas cylinder.
5) Return the LN2 dewar to PVD5.
39
Refill takes about 5 min.
58

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Simon Fraser University 8888 University Drive, Burnaby, B.C.

5 Contact Information ......................................................................................................................... 7

6 X-Ray Safety .................................................................................................................................... 7

7 Software Overview ........................................................................................................................... 8

7.1 Computer Zones ......................................................................................................................... 8

7.2 Vision Instrument Manager......................................................................................................... 9

7.3 Instrument Manual Control Window ........................................................................................... 9

7.4 Vision Processing ..................................................................................................................... 11

7.5 Mouse Operation ..................................................................................................................... 12

8 Manual Acquisition Overview ......................................................................................................... 12

8.1 Types of Spectra ....................................................................................................................... 12

8.1.1 Introduction ...................................................................................................................... 12

8.1.2 Survey Spectrum ................................................................................................................ 12

8.1.3 High Resolution Spectrum .................................................................................................. 15

8.1.4 Snapshot Spectrum............................................................................................................ 18

8.2 Special Sample Considerations.................................................................................................. 21

8.2.1 Insulating Samples ............................................................................................................ 21

8.2.2 Ferromagnetic Samples...................................................................................................... 21

9.1 Samples & Loading ................................................................................................................... 22

9.1.1 Sample Handling and Storage ............................................................................................ 22

9.1.2 Outgassing ........................................................................................................................ 23

9.1.3 Mounting Samples ............................................................................................................ 24

9.1.4 Loading Sample Holders .................................................................................................... 27

9.2 Check of Equipment Status & Log-in ......................................................................................... 27

9.2.1 Visual Inspection ............................................................................................................... 27

9.2.2 X-ray Source & Ion Gun Filament Check ............................................................................. 29

9.2.3 Log-in ............................................................................................................................... 30

9.3 Chiller Alarm ............................................................................................................................ 30

9.4 Focussing ................................................................................................................................. 31

9.4.1 Methods ........................................................................................................................... 31

9.4.2 Manual Sample Height Adjustment .................................................................................... 31

9.5 Acquisition of XPS Spectra ........................................................................................................ 36

9.5.1 Manual Acquisition Panels ................................................................................................. 36

9.5.2 Acquiring Spectra .............................................................................................................. 37

9.5.2.1 Setup ............................................................................................................................................... 37

9.5.2.2 X-Ray Source Warm-up .................................................................................................................. 37

9.5.2.3 Acquisition ....................................................................................................................................... 38

9.5.2.4 Saving Data ..................................................................................................................................... 42

9.6 Wrapping up ............................................................................................................................ 44

9.7 Sample Removal ....................................................................................................................... 45

9.8 Argon Ion Etching in the SAC ................................................................................................... 45

9.8.1 Degassing ......................................................................................................................... 45

9.8.2 Turning On the Ion Gun Gas .............................................................................................. 45

9.8.3 Ion Gun Warm-up ............................................................................................................. 48

9.8.4 Ion Etching ........................................................................................................................ 51

9.8.5 Turning off the Ion Gun & Gas ........................................................................................... 53

9.9 Degassing ................................................................................................................................ 54

9.9.1 X-ray Source...................................................................................................................... 54

9.9.2 SAC Ion Gun ..................................................................................................................... 55

9.10 Ion Pump Cold Trap .............................................................................................................. 57

AES: Auger Electron Spectroscopy

In this document, the following items are italicized.

The following items are underlined.

 Hardware buttons and switches

Text to be typed is shown inside double quotation marks.

 CAUTION indicates a hazard which may cause damage to equipment.

7.1 Computer Zones

 XPS Manager: This zone is reserved for Vision Instrument Manager.

7.2 Vision Instrument Manager

7.3 Instrument Manual Control Window

7.4 Vision Processing

7.5 Mouse Operation

Left mouse button