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ASTM E2735-14

(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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
31-Jan-2014
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
Current Stage
Ref Project

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ASTM E2735-14 - Standard Guide for Selection of Calibrations Needed for X-ray Photoelectron Spectroscopy (XPS) ExperimentsASTM E2735-14 - Standard Guide for Selection of Calibrations Needed for X-ray Photoelectron Spectroscopy (XPS) Experiments
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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 − 14
Standard Guide for
Selection of Calibrations Needed for X-ray Photoelectron
1
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 ger Electron Spectroscopy and X-Ray Photoelectron
Spectroscopy
1.1 This guide describes an approach to enable users and
E996 Practice for Reporting Data in Auger Electron Spec-
analysts to determine the calibrations and standards useful to
troscopy and X-ray Photoelectron Spectroscopy
obtain meaningful surface chemistry data with X-ray photo-
E1078 Guide for Specimen Preparation and Mounting in
electronspectroscopy(XPS)andtooptimizetheinstrumentfor
Surface Analysis
specific analysis objectives and data collection time.
E1127 Guide for Depth Profiling in Auger Electron Spec-
1.2 This guide offers an organized collection of information
troscopy
oraseriesofoptionsanddoesnotrecommendaspecificcourse
E1217 Practice for Determination of the Specimen Area
of action. This guide cannot replace education or experience
Contributing to the Detected Signal in Auger Electron
and should be used in conjunction with professional judgment.
Spectrometers and Some X-Ray Photoelectron Spectrom-
Not all aspects of this guide will be applicable in all circum-
eters
stances.
E1523 Guide to Charge Control and Charge Referencing
Techniques in X-Ray Photoelectron Spectroscopy
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this E1577 Guide for Reporting of Ion Beam Parameters Used in
Surface Analysis
standard.
E1634 Guide for Performing Sputter Crater Depth Measure-
1.4 This standard is not intended to represent or replace the
ments
standard of care by which the adequacy of a given professional
E1636 Practice for Analytically Describing Depth-Profile
service must be judged, nor should this document be applied
and Linescan-Profile Data by an Extended Logistic Func-
without consideration of a project’s many unique aspects. The
tion
word “Standard” in the title of this document means only that
E1829 Guide for Handling Specimens Prior to Surface
the document has been approved through the ASTM consensus
Analysis
process.
E2108 Practice for Calibration of the Electron Binding-
1.5 This standard does not purport to address all of the
Energy Scale of an X-Ray Photoelectron Spectrometer
safety concerns, if any, associated with its use. It is the
3
2.2 ISO Standards:
responsibility of the user of this standard to establish appro-
ISO 10810 Surface Chemical Analysis—Depth Profiling—
priate safety and health practices and determine the applica-
Measurement of Sputtered Depth
bility of regulatory limitations prior to use.
ISO 14606 Surface Chemical Analysis—Sputter Depth
Profiling—Optimisation Using Layered Systems as Ref-
2. Referenced Documents
erence Materials
2
2.1 ASTM Standards:
ISO 14701 Surface Chemical Analysis—X-ray Photoelec-
E995 Guide for Background Subtraction Techniques in Au-
tronSpectroscopy—MeasurementofSiliconOxideThick-
ness
ISO 14976 Surface Chemical Analysis—Data Transfer For-
1
This guide is under the jurisdiction of ASTM Committee E42 on Surface
mat
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
ISO 15470 Surface Chemical Analysis—X-ray Photoelec-
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved Feb. 1, 2014. Published February 2014. Originally tron Spectroscopy—Description of Selected Instrumental
approved in 2013. Last previous edition approved in 2013 as E2735–13. DOI:
Performance Parameters
10.1520/E2735-14.
2
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
3
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
1

---------------------- Page: 1 ----------------------
E2735 − 14
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 Characteri
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E2735 − 13 E2735 − 14
Standard Guide for
Selection of Calibrations Needed for X-ray Photoelectron
1
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
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.
2. Referenced Documents
2
2.1 ASTM Standards:
E684 Practice for Approximate Determination of Current Density of Large-Diameter Ion Beams for Sputter Depth Profiling of
3
Solid Surfaces (Withdrawn 2012)
E995 Guide for Background Subtraction Techniques in Auger Electron Spectroscopy and X-Ray Photoelectron Spectroscopy
E996 Practice for Reporting Data in Auger Electron Spectroscopy and X-ray Photoelectron Spectroscopy
E1016 Guide for Literature Describing Properties of Electrostatic Electron Spectrometers
E1078 Guide for Specimen Preparation and Mounting in Surface Analysis
E1127 Guide for Depth Profiling in Auger Electron Spectroscopy
E1217 Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers
and Some X-Ray Photoelectron Spectrometers
E1523 Guide to Charge Control and Charge Referencing Techniques in X-Ray Photoelectron Spectroscopy
E1577 Guide for Reporting of Ion Beam Parameters Used in Surface Analysis
E1634 Guide for Performing Sputter Crater Depth Measurements
E1636 Practice for Analytically Describing Depth-Profile and Linescan-Profile Data by an Extended Logistic Function
E1829 Guide for Handling Specimens Prior to Surface Analysis
E2108 Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer
3
2.2 ISO Standards:
ISO 10810 Surface Chemical Analysis—Depth Profiling—Measurement of Sputtered Depth
ISO 14606 Surface Chemical Analysis—Sputter Depth Profiling—Optimisation Using Layered Systems as Reference Materials
1
This guide is under the jurisdiction of ASTM Committee E42 on Surface Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved Jan. 15, 2013Feb. 1, 2014. Published January 2013February 2014. Originally approved in 2013. Last previous edition approved in 2013 as
E2735–13. DOI: 10.1520/E2735-13.10.1520/E2735-14.
2
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 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
1

---------------------- Page: 1 ----------------------
E2735 − 14
ISO 14701 Surface Chemical Analysis—X-ray Photoelectron Spectroscopy—Measurement of Silicon Oxide Thickness
ISO 14976 Sur
...

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4.1 Proper preparation and mounting of specimens is particularly critical for surface analysis. Improper preparation of specimens can result in alteration of the surface composition and unreliable data. Specimens should be handled carefully so as to avoid the introduction of spurious contaminants in the preparation and mounting process. The goal must be to preserve the state of the surface so that the analysis remains representative of the original.  
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4.1 Proper handling and preparation of specimens is particularly critical for analysis. Improper handling of specimens can result in alteration of the surface composition and unreliable data. Specimens should be handled carefully so as to avoid the introduction of spurious contaminants. The goal must be to preserve the state of the surface so that analysis remains representative of the original subject.  
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4.1 Auger electron spectroscopy is often capable of yielding information concerning the chemical and physical environment of atoms in the near-surface region of a solid as well as giving elemental and quantitative information. This information is manifested as changes in the observed Auger electron spectrum for a particular element in the specimen under study compared to the Auger spectrum produced by the same element when it is in some reference form. The differences in the two spectra are said to be due to a chemical effect or a matrix effect. Despite sometimes making elemental identification and quantitative measurements more difficult, these effects in the Auger spectrum are considered valuable tools for characterizing the environment of the near-surface atoms in a solid.
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5.1 This practice is to be used for reporting the experimental and data reduction procedures to be described with the publication of the data.
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5.1 This practice is used for reporting the experimental conditions as specified in Section 6 in the “Methods” or “Experimental” sections of other publications (subject to editorial restrictions).  
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Standard Guide for Performing Sputter Crater Depth Measurements

SIGNIFICANCE AND USE
4.1 Sputter crater depth measurements are performed in order to determine a sputter rate (depth/time) for each matrix sputtered during a sputter depth profile or similar in-depth type analyses. From sputter rate values, a linear depth scale can be calculated and displayed for the sputter depth profile.  
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5.1 Auger electron spectroscopy and X-ray photoelectron spectroscopy are used extensively for the surface analysis of materials. This practice summarizes methods for determining the specimen area contributing to the detected signal (a) for instruments in which a focused electron beam can be scanned over a region with dimensions greater than the dimensions of the specimen area viewed by the analyzer, and (b) by employing a sample with a sharp edge.  
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1.1 This practice describes methods for determining the specimen area contributing to the detected signal in Auger electron spectrometers and some types of X-ray photoelectron spectrometers (spectrometer analysis area) when this area is defined by the electron collection lens and aperture system of the electron energy analyzer. The practice is applicable only to those X-ray photoelectron spectrometers in which the specimen area excited by the incident X-ray beam is larger than the specimen area viewed by the analyzer, in which the photoelectrons travel in a field-free region from the specimen to the analyzer entrance. Some of the methods described here require an auxiliary electron gun mounted to produce an electron beam of variable energy on the specimen (“electron-gun method”). Other experiments require a sample with a sharp edge, such as a wafer covered with a uniform clean layer (for example, gold (Au) or silver (Ag)) and cleaved to obtain a long side (“sharp-edge method”).  
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ASTM E2426-10(2019)(Practice)
Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMS

SIGNIFICANCE AND USE
5.1 Electron multipliers are commonly used in pulse-counting mode to detect ions from magnetic sector mass spectrometers. The electronics used to amplify, detect and count pulses from the electron multipliers always have a characteristic time interval after the detection of a pulse, during which no other pulses can be counted. This characteristic time interval is known as the “dead time.” The dead time has the effect of reducing the measured count rate compared with the “true” count rate.  
5.2 In order to measure count rates accurately over the entire dynamic range of a pulse counting detector, such as an electron multiplier, the dead time of the entire pulse counting system must be well known. Accurate count rate measurement forms the basis of isotopic ratio measurements as well as elemental abundance determinations.  
5.3 The procedure described herein has been successfully used to determine the dead time of counting systems on SIMS instruments.6 The accurate determination of the dead time by this method has been a key component of precision isotopic ratio measurements made by SIMS.
SCOPE
1.1 This practice provides the Secondary Ion Mass Spectrometry (SIMS) analyst with a method for determining the dead time of the pulse-counting detection systems on the instrument. This practice also allows the analyst to determine whether the apparent dead time is independent of count rate.  
1.2 This practice is applicable to most types of mass spectrometers that have pulse-counting detectors.  
1.3 This practice does not describe methods for precise or accurate isotopic ratio measurements.  
1.4 This practice does not describe methods for the proper operation of pulse counting systems and detectors for mass spectrometry.  
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.

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