ASTM E2735-13

Standard Guide for Selection of Calibrations Needed for X-ray Photoelectron Spectroscopy (XPS) Experiments

SIGNIFICANCE AND USE
4.1 The purpose of this guide is assist users and analysts in selecting the standardization procedures relevant to a defined XPS experiment. These experiments may be based, for example, upon material failure analysis, the determination of surface chemistry of a solid, or the composition profile of a thin film or coating. A series of options will be summarized giving the standards that are related to specific information requirements. ISO 15470 and ISO 10810 also aid XPS users in experiment design for typical samples. ASTM Committee E42 and ISO TC201 are in a continuous process of updating and adding standards and guides. It is recommended to refer to the ASTM and ISO websites for a current list of standards.
SCOPE
1.1 This guide describes an approach to enable users and analysts to determine the calibrations and standards useful to obtain meaningful surface chemistry data with X-ray photoelectron spectroscopy (XPS) and to optimize the instrument for specific analysis objectives and data collection time.  
1.2 This guide offers an organized collection of information or a series of options and does not recommend a specific course of action. This guide cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this guide will be applicable in all circumstances.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this document be applied without consideration of a project’s many unique aspects. The word “Standard” in the title of this document means only that the document has been approved through the ASTM consensus process.    
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 14-Jan-2013
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: E42 - Surface Analysis
• Drafting Committee: E42.03 - Auger Electron Spectroscopy and X-Ray Photoelectron Spectroscopy

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E2735 − 13
StandardGuide for
Selection of Calibrations Needed for X-ray Photoelectron
Spectroscopy (XPS) Experiments
This standard is issued under the fixed designation E2735; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Profiling of Solid Surfaces (Withdrawn 2012)
E995 Guide for Background Subtraction Techniques in Au-
1.1 This guide describes an approach to enable users and
ger Electron Spectroscopy and X-Ray Photoelectron
analysts to determine the calibrations and standards useful to
Spectroscopy
obtain meaningful surface chemistry data with X-ray photo-
E996 Practice for Reporting Data in Auger Electron Spec-
electronspectroscopy(XPS)andtooptimizetheinstrumentfor
troscopy and X-ray Photoelectron Spectroscopy
specific analysis objectives and data collection time.
E1016 Guide for Literature Describing Properties of Elec-
1.2 This guide offers an organized collection of information
trostatic Electron Spectrometers
oraseriesofoptionsanddoesnotrecommendaspecificcourse
E1078 Guide for Specimen Preparation and Mounting in
of action. This guide cannot replace education or experience
Surface Analysis
and should be used in conjunction with professional judgment.
E1127 Guide for Depth Profiling in Auger Electron Spec-
Not all aspects of this guide will be applicable in all circum-
troscopy
stances.
E1217 Practice for Determination of the Specimen Area
Contributing to the Detected Signal in Auger Electron
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this Spectrometers and Some X-Ray Photoelectron Spectrom-
eters
standard.
E1523 Guide to Charge Control and Charge Referencing
1.4 This standard is not intended to represent or replace the
Techniques in X-Ray Photoelectron Spectroscopy
standard of care by which the adequacy of a given professional
E1577 Guide for Reporting of Ion Beam Parameters Used in
service must be judged, nor should this document be applied
Surface Analysis
without consideration of a project’s many unique aspects. The
E1634 Guide for Performing Sputter Crater Depth Measure-
word “Standard” in the title of this document means only that
ments
the document has been approved through the ASTM consensus
E1636 Practice for Analytically Describing Depth-Profile
process.
and Linescan-Profile Data by an Extended Logistic Func-
1.5 This standard does not purport to address all of the
tion
safety concerns, if any, associated with its use. It is the
E1829 Guide for Handling Specimens Prior to Surface
responsibility of the user of this standard to establish appro-
Analysis
priate safety and health practices and determine the applica-
E2108 Practice for Calibration of the Electron Binding-
bility of regulatory limitations prior to use.
Energy Scale of an X-Ray Photoelectron Spectrometer
2.2 ISO Standards:
2. Referenced Documents
ISO 10810 Surface Chemical Analysis—Depth Profiling—
2.1 ASTM Standards:
Measurement of Sputtered Depth
E684 Practice for Approximate Determination of Current
ISO 14606 Surface Chemical Analysis—Sputter Depth
Density of Large-Diameter Ion Beams for Sputter Depth
Profiling—Optimisation Using Layered Systems as Ref-
erence Materials
ISO 14701 Surface Chemical Analysis—X-ray Photoelec-
This guide is under the jurisdiction of ASTM Committee E42 on Surface
tronSpectroscopy—MeasurementofSiliconOxideThick-
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
ness
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved Jan. 15, 2013. Published January 2013. DOI: 10.1520/
E2735-13.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM www.astm.org.
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2735 − 13
ISO 14976 Surface Chemical Analysis—Data Transfer For- film or coating.Aseries of options will be summarized giving
mat the standards that are related to specific information require-
ISO 15470 Surface Chemical Analysis—X-ray Photoelec- ments. ISO 15470 and ISO 10810 also aid XPS users in
tron Spectroscopy—Description of Selected Instrumental experiment design for typical samples.ASTM Committee E42
Performance Parameters and ISO TC201 are in a continuous process of updating and
ISO 15472 Surface Chemical Analysis—X-ray Photoelec- adding standards and guides. It is recommended to refer to the
tron Spectrometers—Calibration of Energy Scales ASTM and ISO websites for a current list of standards.
ISO/TR 15969 Surface Chemical Analysis—Depth
5. Procedure
Profiling—Measurement of Sputtered Depth
ISO 18115-1 Surface Chemical Analysis—Vocabulary—
5.1 General Sample Characterization:
Part 1: General Terms and Terms Used in Spectroscopy
5.1.1 Sample History—The analyst should obtain a sum-
ISO 18115-2 Surface Chemical Analysis—Vocabulary—
mary of the background information of the sample, including
Part 2: Terms Used in Scanning-Probe
descriptors, history, sample cleaning and handling, existing
ISO 18116 Surface Chemical Analysis—Guidelines for
application data, bulk composition, and any prior analysis that
Preparation and Mounting of Specimens for Analysis
has been conducted. The sample history, especially handling,
ISO 18117 Surface ChemicalAnalysis—Handling of Speci-
packing and storage, can impact the approach needed to obtain
mens Prior to Analysis
the desired information. Because inadequate sample collection
ISO 18118 Surface Chemical Analysis—Auger Electron
can sometimes destroy or minimize the ability to collect the
Spectroscopy and X-ray Photoelectron Spectroscopy—
desired information, it is often necessary to identify the needed
Guide to the Use of Experimentally Determined Relative
information and establish the procedures to be used (5.2)
Sensitivity Factors for the Quantitative Analysis of Ho-
before the surface analysis is performed.
mogeneous Materials
5.1.2 Vacuum Compatibility—The compatibility of sample
ISO/TR 18392 Surface Chemical Analysis—X-ray Photo-
with instrument vacuum should be considered.Although some
electron Spectroscopy—Procedures for Determining
samples have inappropriately high vapor pressures for ambient
Backgrounds
temperatureoperation,someinstrumentsmayincludeasample
ISO 18516 Surface Chemical Analysis—Auger Electron
cooling stage, which allows these types of materials to be
Spectroscopy and X-ray Photoelectron Spectroscopy—
analyzed. Additionally, newer XPS systems often have im-
Determination of Lateral Resolution
proved vacuum pumps coupled with monochromatic X-ray
ISO 19318 Surface Chemical Analysis—X-ray Photoelec-
sources (that do not heat the sample) and a small X-ray spot
tron Spectroscopy—Reporting of Methods Used for
size (requiring less sample for analysis). As a result, strongly
Charge Control and Charge Correction
outgassing or subliming samples can often be examined.
ISO/TR 19319 Surface ChemicalAnalysis—Auger Electron
5.2 Design of Experiment:
Spectroscopy and X-ray Photoelectron Spectroscopy—
5.2.1 The goal of the experiment should be defined. Experi-
Determination of Lateral Resolution, Analysis Area and
mental goals may include data relating to the surface chemical
Sample Area Viewed by the Analyser
composition and chemical state, surface segregation,
ISO 20903 Surface Chemical Analysis—Auger Electron
quantification, layer thickness, nanostructures, and so forth.
Spectroscopy and X-ray Photoelectron Spectroscopy—
The identification of the specific analysis objectives influences
Methods Used to Determine Peak Intensities and Infor-
sample handling, instrument setup, the approach to data
mation Required when Reporting Results
collection, and finally the methods of data analysis.
ISO 21270 Surface Chemical Analysis—X-ray Photoelec-
5.2.1.1 Table 1 is a summary of possible experiments along
tron and Auger Electron Spectrometers—Linearity of
with different calibrations to be considered. Also included are
Intensity Scale
the ASTM and ISO standards for checking the parameter. In
ISO 22335 Surface Chemical Analysis—Depth Profiling—
the table, an X indicates applications where a calibration is
Measurement of Sputtering Rate: Mesh-Replica Method
required. Additionally, the calibrations are ranked with X =
Using a Mechanical Stylus Profilometer
generally important and XX = generally very important cali-
ISO 24237 Surface Chemical Analysis—X-ray Photoelec-
brations for a given task.
tron Spectroscopy—Repeatability and Constancy of In-
5.2.2 General System Check—The analyst should perform a
tensity Scale
general system health check (including mechanical
components, sample holders, vacuum level, and performance
3. Terminology
check)asrecommendedbytheinstrumentmanufacturer.Many
3.1 Definitions—For definitions of surface analysis terms
analysts have also developed their own methods to verify the
used in this guide, see ISO 18115-1 and ISO 18115-2.
general operational health of an instrument. This might be
4. Significance and Use done, for example, by testing a specimen commonly analyzed
by the instrument to quickly verify the binding energies of few
4.1 The purpose of this guide is assist users and analysts in
selecting the standardization procedures relevant to a defined
XPS experiment. These experiments may be based, for
Castle, J. E., Powell, C. J., Report on the 34th IUVSTAWorkshop, XPS: From
example, upon material failure analysis, the determination of
Spectra to Results—Towards an Expert System, Surface and Interface Analysis,Vol
surfacechemistryofasolid,orthecompositionprofileofathin 26, 2004, pp. 225–237.
E2735 − 13
TABLE 1 Recommended XPS Calibrations for Defined Experiments
A
NOTE 1—Calibrations required to obtain meaningful data or to optimize the instrument for the best data in the time available. The X indicates
applications where a calibration is required. X = generally important, XX = generally very important. Local methods are procedures developed by an
individual laboratory or the instrument manufacturer. NPL software for the calibration of the intensity scales of XPS instruments is available from the
B C D
UKNationalPhysicalLaboratory. BCR261 isacertifiedreferencetantalumoxide/tantalumfoilcalibrationsampleandNISTSRM2135c isacertified
nickel/chromium thin-film depth profile standard.
Instrument
ASTM ISO Elemental Chemical Low Level Quantifi- Layer Nano-
Calibrations
Standard Standard Composition State Detection cation Thickness structures
and Checks
General System Check Local Method Local Method XX XX XX XX XX XX
Sample Preparation E1829 18116 XX X X XX X
E1078 18117
Binding Energy E2108 15472 XX XX X X
E1523 19318
Intensity Repeatability 24237 X X XX XX X X
and Constancy
Intensity/Energy Re- NPL XX X XX
sponse Function Software
Linearity of Intensity E1016 21270 XX XX X XX
Scale 18118
Peak Intensities E995, 18392 XX XX X X X
Local Method 20903
Ion Gun and Sputter E684 15969 XX XX
Rate E1577 22335
E1127 BCR 261
E1634 14606
Depth Resolution E684 BCR 261 XX XX
E1577 NIST SRM
E1127 2135c
E1634 14606
E1636
Analysis Area E1217 19319 X X X XX
Lateral Resolution 18516 X X X X
Data Reporting E996 14979 X X X X X X
A
Castle, J. E., Powell, C. J., Report on the 34th IUVSTAWorkshop, XPS: From Spectra to Results—Towards an Expert System, Surface and Interface Analysis, Vol 26,
2004, pp. 225–237.
B
National Physical Laboratory (NPL), http://www.npl.co.uk/server.php?show=ConWebDoc.606.
C
European Institute for Reference Materials and Measurements, BCR261, certified reference material.
D
National Institute of Standards and Technology, NIST-SRM 3125c Ni/Cr Thin Film Depth Profile Standard, http://www.nist.gov/srm.
photoelectron peaks and overall count rates. Based upon the must be to preserve the state of the surface so that the analysis
experiment to be performed, the relative importance of the remains representative of the original surface. Care must then
parameters in Table 1 should be assessed, including calibration be taken to ensure that no outside agents come in contact with
of the binding-energy scale, intensity repeatability and the surface to be investigated. These agents include: fingers,
constancy, intensity/energy response function (IERF), linearity solvents or cleaning solutions, gases (including compressed
test of the intensity scale, energy resolution for the desired air) or vapors, metals, tissue or other wrapping materials, tape,
intensity, lateral resolution, charge compensation, depth cloth, tools, packing materials or the walls of containers.
resolution, and depth profile rate calibration. Handling of the surface to be analyzed should be eliminated or
5.2.3 Sample Transport and Preparation—As a surface minimized whenever possible.
analysis technique, X-ray photoelectron spectroscopy (XPS) is 5.2.3.1 Proper preparation and mounting of specimens is
sensitive to the outermost few atomic layers of the sample particularly critical for surface analysis. Improper preparation
being characterized. Specimens should be transported to the ofspecimenscanresultinalterationofthesurfacecomposition
analyst in a container that does not come into direct contact andunreliabledata.Inaddition,specimenmountingtechniques
with the surface of interest. In most cases, the analysis will be have the potential to affect the intended analysis.
performed on the as-received specimen; therefore, the goal Guides E1078 and E1829 and/or ISO 18116 and ISO 18117
E2735 − 13
describemethodsthesurfaceanalystmayneedtominimizethe of confidence, based on the instrument stability and the
effects of specimen preparation when using any surface- analyst’s needs.Then, BE measurements statistically are likely
to be made within these limits during specified time intervals
sensitive analytical technique. Also described are methods to
mountspecimenssoastoensurethatthedesiredinformationis following a calibration. The instrument is then adjusted or
subsequent BE measurements are corrected. For a routine
not compromised. Because of the wide range of types of
specimens and desired information, only broad guidelines and check of the instrumental c
...