ASTM E2735-14(2020)
(Guide)Standard Guide for Selection of Calibrations Needed for X-ray Photoelectron Spectroscopy (XPS) Experiments
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E2735 − 14 (Reapproved 2020)
Standard Guide 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This guide describes an approach to enable users and
E995 Guide for Background Subtraction Techniques in Au-
analysts to determine the calibrations and standards useful to
ger Electron Spectroscopy and X-Ray Photoelectron
obtain meaningful surface chemistry data with X-ray photo-
Spectroscopy
electron spectroscopy (XPS) and to optimize the instrument for
E996 Practice for Reporting Data in Auger Electron Spec-
specific analysis objectives and data collection time.
troscopy and X-ray Photoelectron Spectroscopy
1.2 This guide offers an organized collection of information
E1078 Guide for Specimen Preparation and Mounting in
or a series of options and does not recommend a specific course
Surface Analysis
of action. This guide cannot replace education or experience
E1127 Guide for Depth Profiling in Auger Electron Spec-
and should be used in conjunction with professional judgment.
troscopy
Not all aspects of this guide will be applicable in all circum-
E1217 Practice for Determination of the Specimen Area
stances.
Contributing to the Detected Signal in Auger Electron
Spectrometers and Some X-Ray Photoelectron Spectrom-
1.3 The values stated in SI units are to be regarded as
eters
standard. No other units of measurement are included in this
E1523 Guide to Charge Control and Charge Referencing
standard.
Techniques in X-Ray Photoelectron Spectroscopy
1.4 This standard is not intended to represent or replace the
E1577 Guide for Reporting of Ion Beam Parameters Used in
standard of care by which the adequacy of a given professional
Surface Analysis (Withdrawn 2020)
service must be judged, nor should this document be applied
E1634 Guide for Performing Sputter Crater Depth Measure-
without consideration of a project’s many unique aspects. The
ments
word “Standard” in the title of this document means only that
E1636 Practice for Analytically Describing Depth-Profile
the document has been approved through the ASTM consensus
and Linescan-Profile Data by an Extended Logistic Func-
process. 3
tion (Withdrawn 2019)
E1829 Guide for Handling Specimens Prior to Surface
1.5 This standard does not purport to address all of the
Analysis
safety concerns, if any, associated with its use. It is the
E2108 Practice for Calibration of the Electron Binding-
responsibility of the user of this standard to establish appro-
Energy Scale of an X-Ray Photoelectron Spectrometer
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 2.2 ISO Standards:
ISO 10810 Surface Chemical Analysis—Depth Profiling—
1.6 This international standard was developed in accor-
Measurement of Sputtered Depth
dance with internationally recognized principles on standard-
ISO 14606 Surface Chemical Analysis—Sputter Depth
ization established in the Decision on Principles for the
Profiling—Optimisation Using Layered Systems as Ref-
Development of International Standards, Guides and Recom-
erence Materials
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This guide is under the jurisdiction of ASTM Committee E42 on Surface Standards volume information, refer to the standard’s Document Summary page on
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron the ASTM website.
Spectroscopy and X-Ray Photoelectron Spectroscopy. The last approved version of this historical standard is referenced on
Current edition approved Dec. 1, 2020. Published December 2020. Originally www.astm.org.
approved in 2013. Last previous edition approved in 2014 as E2735–14. DOI: Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/E2735-14R20. 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 − 14 (2020)
ISO 14701 Surface Chemical Analysis—X-ray Photoelec- XPS experiment. These experiments may be based, for
tron Spectroscopy—Measurement of Silicon Oxide Thick- example, upon material failure analysis, the determination of
ness surface chemistry of a solid, or the composition profile of a thin
ISO 14976 Surface Chemical Analysis—Data Transfer For- film or coating. A series 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 Microscopy
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 Chemical Analysis—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
temperature operation, some instruments may include a sample
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 Chemical Analysis—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 required to obtain meaningful data
Intensity Scale
or to optimize the instrument for the best data in the time
ISO 22335 Surface Chemical Analysis—Depth Profiling—
available. Also included are the ASTM and ISO standards for
Measurement of Sputtering Rate: Mesh-Replica Method
checking the parameter. In the table, an X indicates applica-
Using a Mechanical Stylus Profilometer
tions where a calibration is required. Additionally, the calibra-
ISO 24237 Surface Chemical Analysis—X-ray Photoelec-
tions are ranked with X = generally important and XX =
tron Spectroscopy—Repeatability and Constancy of In-
generally very important calibrations for a given task.
tensity Scale
5.2.2 General System Check—The analyst should perform a
3. Terminology general system health check (including mechanical
components, sample holders, vacuum level, and performance
3.1 Definitions—For definitions of surface analysis terms
check) as recommended by the instrument manufacturer. Many
used in this guide, see ISO 18115-1 and ISO 18115-2.
4. Significance and Use
Castle, J. E., Powell, C. J., Report on the 34th IUVSTA Workshop, XPS: From
4.1 The purpose of this guide is assist users and analysts in
Spectra to Results—Towards an Expert System, Surface and Interface Analysis, Vol
selecting the standardization procedures relevant to a defined 26, 2004, pp. 225–237.
E2735 − 14 (2020)
TABLE 1 Recommended XPS Calibrations for Defined Experiments
A
NOTE 1—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
B C
instruments is available from the UK National Physical Laboratory. BCR 261 is a certified reference tantalum oxide/tantalum foil calibration sample
D
and NIST SRM 2135c is a certified nickel/chromium thin-film depth profile standard.
Instrument
ASTM ISO Additional Elemental Chemical Low Level Quantifi- Layer Nano-
Calibrations
Standard Standard Sources Composition State Detection cation Thickness structures
and Checks
General System Check Local Method XX XX XX XX XX XX
Sample Preparation E1829 18116 X X 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 NPL XX X XX
Response Function Software
Linearity of Intensity 21270 X X XX X XX
Scale 18118
Peak Intensities E995 18392 Local Method X X XX X X X
Ion Gun and Sputter E1577 15969 BCR 261 XX XX
Rate E1127 22335
E1634 14606
Depth Resolution E1577 14606 BCR 261 XX XX
E1127 NIST SRM
E1634 2135c
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
Manual from the system manufacturer.
B
National Physical Laboratory (NPL),
http: ⁄ ⁄www.npl.co.uk ⁄science-technology ⁄surface-and-nanoanalysis ⁄services ⁄calibration-software-and-reference-materials-for-electron-spectrometers.
C
European Institute for Reference Materials and Measurements, BCR261, certified reference material.
D
National Institute of Standards and Technology, NIST-SRM 2135c Ni/Cr Thin Film Depth Profile Standard, http://www.nist.gov.
analysts have also developed their own methods to verify the must be to preserve the state of the surface so that the analysis
general operational health of an instrument. This might be remains representative of the original surface. Care must then
done, for example, by testing a specimen commonly analyzed be taken to ensure that no outside agents come in contact with
by the instrument to quickly verify the binding energies of few the surface to be investigated. These agents include: fingers,
photoelectron peaks and overall count rates. Based upon the solvents or cleaning solutions, gases (including compressed
experiment to be performed, the relative importance of the air) or vapors, metals, tissue or other wrapping materials, tape,
parameters in Table 1 should be assessed, including calibration cloth, tools, packing materials or the walls of containers.
of the binding-energy scale, intensity repeatability and Handling of the surface to be analyzed should be eliminated or
constancy, intensity/energy response function (IERF), linearity minimized whenever possible.
test of the intensity scale, energy resolution for the desired 5.2.3.1 Proper preparation and mounting of specimens is
intensity, lateral resolution, charge compensation, depth particularly critical for surface analysis. Improper preparation
resolution, and depth profile rate calibration. of specimens can result in alteration of the surface composition
5.2.3 Sample Transport and Preparation—As a surface and unreliable data. In addition, specimen mounting techniques
analysis technique, X-ray photoelectron spectroscopy (XPS) is have the potential to affect the intended analysis. Guides E1078
sensitive to the outermost few atomic layers of the sample and E1829 and/or ISO 18116 and ISO 18117 describe methods
being characterized. Specimens should be transported to the the surface analyst may need to minimize the effects of
analyst in a container that does not come into direct contact specimen preparation when using any surface-sensitive ana-
with the surface of interest. In most cases, the analysis will be lytical technique. Also described are methods to mount speci-
performed on the as-received specimen; therefore, the goal mens so as to ensure that the desired information is not
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.