E42.03 - Auger Electron Spectroscopy and X-Ray Photoelectron Spectroscopy

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.

SIGNIFICANCE AND USE
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.  
4.2 AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1)4 or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.  
4.3 This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.  
4.4 Guide E1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
SCOPE
1.1 This guide covers specimen preparation and mounting prior to, during, and following surface analysis and applies to the following surface analysis disciplines:  
1.1.1 Auger electron spectroscopy (AES),  
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA), and  
1.1.3 Secondary ion mass spectrometry (SIMS).  
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will also apply to many surface sensitive analysis methods, such as ion scattering spectrometry, low energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface sensitive measurements.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
1.4 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.

SIGNIFICANCE AND USE
5.1 The analyst may use this document to obtain information on the properties of electron spectrometers and instrumental aspects associated with quantitative surface analysis.
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with some of the relevant literature describing the physical properties of modern electrostatic electron spectrometers.  
1.2 This guide is intended to apply to electron spectrometers generally used in Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).  
1.3 The values stated in inch-pound units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
1.5 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.

SIGNIFICANCE AND USE
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.  
4.2 AES, XPS, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations from improper specimen handling  (1).4  
4.3 This guide describes methods to minimize the effects of specimen handling on the results obtained using surface-sensitive analytical techniques. It is intended for the specimen owner or the purchaser of surface analytical services and the surface analyst. Because of the wide range of types of specimens and desired information, only broad guidelines and general examples are presented here. The optimum handling procedures will be dependent on the particular specimen and the needed information. It is recommended that the specimen supplier consult the surface analyst as soon as possible with regard to specimen history, the specific problem to be solved or information needed, and the particular specimen preparation or handling procedures required. The surface analyst also is referred to Guide E1078 that discusses additional procedures for preparing, mounting, and analysis of specimens.
SCOPE
1.1 This guide covers specimen handling and preparation prior to surface analysis and applies to the following surface analysis disciplines:  
1.1.1 Auger electron spectroscopy (AES),  
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA), and  
1.1.3 Secondary ion mass spectrometry (SIMS).  
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods may also apply to many surface-sensitive analysis methods, such as ion scattering spectrometry, low-energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface-sensitive measurements.  
1.2 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.  
1.3 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.

SIGNIFICANCE AND USE
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.
SCOPE
1.1 This guide outlines the types of chemical effects and matrix effects which are observed in Auger electron spectroscopy.  
1.2 Guidelines are given for the reporting of chemical and matrix effects in Auger spectra.  
1.3 Guidelines are given for utilizing Auger chemical effects for identification or characterization.  
1.4 This guide is applicable to both electron excited and X-ray excited Auger electron spectroscopy.  
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.

SIGNIFICANCE AND USE
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.  
5.2 This practice is intended as a means for determining the observed specimen area for selected conditions of operation of the electron energy analyzer. The observed specimen area depends on whether or not the electrons are retarded before energy analysis, the analyzer pass energy or retarding ratio if the electrons are retarded before energy analysis, the size of selected slits or apertures, and the value of the electron energy to be measured. The observed specimen area depends on these selected conditions of operation and also can depend on the adequacy of alignment of the specimen with respect to the electron energy analyzer.  
5.3 Any changes in the observed specimen area as a function of measurement conditions, for example, electron energy or analyzer pass energy, may need to be known if the specimen materials in regular use have lateral inhomogeneities with dimensions comparable to the dimensions of the specimen area viewed by the analyzer.  
5.4 This practice can give useful information on the imaging properties of the electron energy analyzer for particular conditions of operation. This information can be helpful in comparing analyzer performance with manufacturer's specifications.  
5.5 Information about the shape and size of the area viewed by the analyzer can also be employed to predict the signal intensity in XPS experiments when the sample is rotated and to assess the axis of rotation of the sample manipulator.  
5.6 Examples of the application of the methods described in this practice have been publis...
SCOPE
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”).  
1.2 This practice is recommended as a useful means for determining the specimen area viewed by the analyzer for different conditions of spectrometer operation, for verifying adequate specimen and beam alignment, and for characterizing the imaging properties of the electron energy analyzer.  
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 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.  
1.5 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 Recomm...

SIGNIFICANCE AND USE
5.1 Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.  
5.2 Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
SCOPE
1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.  
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.  
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 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.  
1.5 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.

SIGNIFICANCE AND USE
4.1 When electron beam excitation is used in AES, the incident electron beam can interact with the specimen material causing physical and chemical changes. In general, these effects are a hindrance to AES analysis because they cause localized specimen modification (1-4).5  
4.2 With specimens that have poor electrical conductivity the electron beam can stimulate the development of localized charge on the specimen surface. This effect is a hindrance to AES analysis because the potentials associated with the charge can either adversely affect the integrity of Auger data or make Auger data collection difficult (5, 6).
SCOPE
1.1 This guide outlines the origins and manifestations of unwanted electron beam effects in Auger electron spectroscopy (AES).  
1.2 Some general guidelines are provided concerning the electron beam parameters which are most likely to produce these effects and suggestions are offered on how to minimize them.  
1.3 General classes of materials are identified which are most likely to exhibit unwanted electron beam effects. In addition, a tabulation of some specific materials which have been observed to undergo electron damage effects is provided.  
1.4 A simple method is outlined for establishing the existence and extent of these effects during routine AES analysis.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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.

SIGNIFICANCE AND USE
5.1 Background subtraction techniques in AES were originally employed as a method of enhancement of the relatively weak Auger signals to distinguish them from the slowly varying background of secondary and backscattered electrons. Interest in obtaining useful information from the Auger peak line shape, concern for greater quantitative accuracy from Auger spectra, and improvements in data gathering techniques, have led to the development of various background subtraction techniques.  
5.2 Similarly, the use of background subtraction techniques in XPS has evolved mainly from the interest in the determination of chemical states (from the binding-energy values for component peaks that may often overlap), greater quantitative accuracy from the XPS spectra, and improvements in data acquisition. Post-acquisition background subtraction is normally applied to XPS data.  
5.3 The procedures outlined in Section 7 are popular in XPS and AES; less popular procedures and rarely used procedures are described in Sections 8 and 9, respectively. General reviews of background subtraction methods and curve-fitting techniques have been published elsewhere (1-5).6  
5.4 Background subtraction is commonly performed prior to peak fitting, although it can be assessed (fitted) during peak fitting (active approach  (6, 7)). Some commercial data analysis packages require background removal before peak fitting. Nevertheless, a measured spectral region consisting of one or more peaks and background intensities due to inelastic scattering, Bremsstrahlung (for XPS with unmonochromated X-ray sources), and scattered primary electrons (for AES) can often be satisfactorily represented by applying peak functions for each component with parameters for each one determined in a single least-squares fit. The choice of the background to be removed, if required or desired, before or during peak fitting is suggested by the experience of the analysts, the capabilities of the peak fitting software, and the p...
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with the principal background subtraction techniques presently in use together with the nature of their application to data acquisition and manipulation.  
1.2 This guide is intended to apply to background subtraction in electron, X-ray, and ion-excited Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS).  
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 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.

SIGNIFICANCE AND USE
5.1 X-ray photoelectron spectroscopy is used extensively for the surface analysis of materials. Elements (with the exception of hydrogen and helium) are identified from comparisons of the binding energies determined from photoelectron spectra with tabulated values. Information on chemical state can be derived from the chemical shifts of measured photoelectron and Auger-electron features with respect to those measured for elemental solids.  
5.2 Calibrations of the BE scales of XPS instruments are required for four principal reasons. First, meaningful comparison of BE measurements from two or more XPS instruments requires that the BE scales be calibrated, often with an uncertainty of about 0.1 eV to 0.2 eV. Second, identification of chemical state is based on measurement of chemical shifts of photoelectron and Auger-electron features, again with an uncertainty of typically about 0.1 eV to 0.2 eV; individual measurements, therefore, should be made and literature sources need to be available with comparable or better accuracies. Third, the availability of databases (3) of measured BEs for reliable identification of elements and determination of chemical states by computer software requires that published data and local measurements be made with uncertainties of about 0.1 eV to 0.2 eV. Finally, the growing adoption of quality management systems, such as, ISO 9001:2015, in many analytical laboratories has led to requirements that the measuring and test equipment be calibrated and that the relevant measurement uncertainties be known.  
5.3 The actual uncertainty of a BE measurement depends on instrument properties and stability, measurement conditions, and the method of data analysis. This practice makes use of tolerance limits ±δ (chosen, for example, at the 95 % confidence level) that represent the maximum likely uncertainty of a BE measurement, associated with the instrument in a specified time interval following a calibration (ISO 15472:2010). A user should select a...
SCOPE
1.1 This practice describes a procedure for calibrating the electron binding-energy (BE) scale of an X-ray photoelectron spectrometer that is to be used for performing spectroscopic analysis of photoelectrons excited by unmonochromated aluminum or magnesium Kα X-rays or by monochromated aluminum Kα X-rays.  
1.2 The calibration of the BE scale is recommended after the instrument is installed or modified in any substantive way. Additional checks and, if necessary, recalibrations are recommended at intervals chosen to ensure that BE measurements are statistically unlikely to be made with an uncertainty greater than a tolerance limit, specified by the analyst, based on the instrumental stability and the analyst’s needs. Information is provided by which the analyst can select an appropriate tolerance limit for the BE measurements and the frequency of calibration checks.  
1.3 This practice is based on the assumption that the BE scale of the spectrometer is sufficiently close to linear to allow for calibration by measurements of reference photoelectron lines having BEs near the extremes of the working BE scale. In most commercial instruments, X-ray sources with aluminum or magnesium anodes are employed and BEs are typically measured at least over the 0–1200 eV range. This practice can be used for the BE range from 0 eV to 1040 eV.  
1.4 The assumption that the BE scale is linear is checked by a measurement made with a reference photoelectron line or Auger-electron line that appears at an intermediate position. A single check is a necessary but not sufficient condition for establishing linearity of the BE scale. Additional checks can be made with specified reference lines on instruments equipped with magnesium or unmonochromated aluminum X-ray sources, with secondary BE standards, or by following the procedures of the instrument manufacturer. Deviations from BE-scale linearity can occur because of mechanical misalignments, ...

SIGNIFICANCE AND USE
5.1 The acquisition of chemical information from variations in the energy position of peaks in the XPS spectrum is of primary interest in the use of XPS as a surface analytical tool. Surface charging acts to shift spectral peaks independent of their chemical relationship to other elements on the same surface. The desire to eliminate the influence of surface charging on the peak positions and peak shapes has resulted in the development of several empirical methods designed to assist in the interpretation of the XPS peak positions, determine surface chemistry, and allow comparison of spectra of conducting and non-conducting systems of the same element. It is assumed that the spectrometer is generally working properly for non-insulating specimens (see Practice E902).  
5.2 Although highly reliable methods have now been developed to stabilize surface potentials during XPS analysis of most materials (5, 6), no single method has been developed to deal with surface charging in all circumstances (10, 11). For insulators, an appropriate choice of any control or referencing system will depend on the nature of the specimen, the instruments, and the information needed. The appropriate use of charge control and referencing techniques will result in more consistent, reproducible data. Researchers are strongly urged to report both the control and referencing techniques that have been used, the specific peaks and binding energies used as standards (if any), and the criteria applied in determining optimum results so that the appropriate comparisons may be made.
SCOPE
1.1 This guide acquaints the X-ray photoelectron spectroscopy (XPS) user with the various charge control and charge shift referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens and provides information needed for reporting the methods used to customers or in the literature.  
1.2 This guide is intended to apply to charge control and charge referencing techniques in XPS and is not necessarily applicable to electron-excited systems.  
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 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.

SIGNIFICANCE AND USE
5.1 Auger electron spectroscopy yields information concerning the chemical and physical state of a solid surface in the near surface region. Nondestructive depth profiling is limited to this near surface region. Techniques for measuring the crater depths and film thicknesses are given in (1).5  
5.2 Ion sputtering is primarily used for depths of less than the order of 1 μm.  
5.3 Angle lapping or mechanical cratering is primarily used for depths greater than the order of 1 μm.  
5.4 The choice of depth profiling methods for investigating an interface depends on surface roughness, interface roughness, and film thickness (2).  
5.5 The depth profile interface widths can be measured using a logistic function which is described in Practice E1636.
SCOPE
1.1 This guide covers procedures used for depth profiling in Auger electron spectroscopy.  
1.2 Guidelines are given for depth profiling by the following:    
Section  
Ion Sputtering  
6  
Angle Lapping and Cross-Sectioning  
7  
Mechanical Cratering  
8  
Mesh Replica Method  
9  
Nondestructive Depth Profiling  
10  
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 does not purport to address all of the safety problems, 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.

SIGNIFICANCE AND USE
4.1 When electron beam excitation is used in AES, the incident electron beam can interact with the specimen material causing physical and chemical changes. In general, these effects are a hindrance to AES analysis because they cause localized specimen modification (1-4).4  
4.2 With specimens that have poor electrical conductivity the electron beam can stimulate the development of localized charge on the specimen surface. This effect is a hindrance to AES analysis because the potentials associated with the charge can either adversely affect the integrity of Auger data or make Auger data collection difficult (5, 6).
SCOPE
1.1 This guide outlines the origins and manifestations of unwanted electron beam effects in Auger electron spectroscopy (AES).  
1.2 Some general guidelines are provided concerning the electron beam parameters which are most likely to produce these effects and suggestions are offered on how to minimize them.  
1.3 General classes of materials are identified which are most likely to exhibit unwanted electron beam effects. In addition, a tabulation of some specific materials which have been observed to undergo electron damage effects is provided.  
1.4 A simple method is outlined for establishing the existence and extent of these effects during routine AES analysis.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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.

SIGNIFICANCE AND USE
5.1 Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.  
5.2 Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
SCOPE
1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.  
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.  
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 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.  
1.5 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.

SIGNIFICANCE AND USE
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.  
4.2 AES, XPS, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations from improper specimen handling  (1).4  
4.3 This guide describes methods to minimize the effects of specimen handling on the results obtained using surface-sensitive analytical techniques. It is intended for the specimen owner or the purchaser of surface analytical services and the surface analyst. Because of the wide range of types of specimens and desired information, only broad guidelines and general examples are presented here. The optimum handling procedures will be dependent on the particular specimen and the needed information. It is recommended that the specimen supplier consult the surface analyst as soon as possible with regard to specimen history, the specific problem to be solved or information needed, and the particular specimen preparation or handling procedures required. The surface analyst also is referred to Guide E1078 that discusses additional procedures for preparing, mounting, and analysis of specimens.
SCOPE
1.1 This guide covers specimen handling and preparation prior to surface analysis and applies to the following surface analysis disciplines:  
1.1.1 Auger electron spectroscopy (AES),  
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA), and  
1.1.3 Secondary ion mass spectrometry (SIMS).  
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods may also apply to many surface-sensitive analysis methods, such as ion scattering spectrometry, low-energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface-sensitive measurements.  
1.2 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.

SIGNIFICANCE AND USE
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.  
4.2 AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1)4 or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.  
4.3 This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.  
4.4 Guide E1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
SCOPE
1.1 This guide covers specimen preparation and mounting prior to, during, and following surface analysis and applies to the following surface analysis disciplines:  
1.1.1 Auger electron spectroscopy (AES),  
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA), and  
1.1.3 Secondary ion mass spectrometry (SIMS).  
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will also apply to many surface sensitive analysis methods, such as ion scattering spectrometry, low energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface sensitive measurements.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.

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.

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.

SIGNIFICANCE AND USE
The analyst may use this document to obtain information on the properties of electron spectrometers and instrumental aspects associated with quantitative surface analysis.
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1.1 The purpose of this guide is to familiarize the analyst with some of the relevant literature describing the physical properties of modern electrostatic electron spectrometers.  
1.2 This guide is intended to apply to electron spectrometers generally used in Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).  
1.3 The values stated in inch-pound units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.

SIGNIFICANCE AND USE
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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1.1 This guide outlines the types of chemical effects and matrix effects which are observed in Auger electron spectroscopy.  
1.2 Guidelines are given for the reporting of chemical and matrix effects in Auger spectra.  
1.3 Guidelines are given for utilizing Auger chemical effects for identification or characterization.  
1.4 This guide is applicable to both electron excited and X-ray excited Auger electron spectroscopy.  
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.

SIGNIFICANCE AND USE
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.
This practice is intended as a means for determining the observed specimen area for selected conditions of operation of the electron energy analyzer. The observed specimen area depends on whether or not the electrons are retarded before energy analysis, the analyzer pass energy or retarding ratio if the electrons are retarded before energy analysis, the size of selected slits or apertures, and the value of the electron energy to be measured. The observed specimen area depends on these selected conditions of operation and also can depend on the adequacy of alignment of the specimen with respect to the electron energy analyzer.
Any changes in the observed specimen area as a function of measurement conditions, for example, electron energy or analyzer pass energy, may need to be known if the specimen materials in regular use have lateral inhomogeneities with dimensions comparable to the dimensions of the specimen area viewed by the analyzer.
This practice can give useful information on the imaging properties of the electron energy analyzer for particular conditions of operation. This information can be helpful in comparing analyzer performance with manufacturer's specifications.
Information about the shape and size of the area viewed by the analyzer can also be employed to predict the signal intensity in XPS experiments when the sample is rotated and to assess the axis of rotation of the sample manipulator.
Examples of the application of the methods described in this practice have been published (1-7).  
There are diffe...
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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”).
1.2 This practice is recommended as a useful means for determining the specimen area viewed by the analyzer for different conditions of spectrometer operation, for verifying adequate specimen and beam alignment, and for characterizing the imaging properties of the electron energy analyzer.
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 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.

SIGNIFICANCE AND USE
Background subtraction techniques in AES were originally employed as a method of enhancement of the relatively weak Auger signals to distinguish them from the slowly varying background of secondary and backscattered electrons. Interest in obtaining useful information from the Auger peak line shape, concern for greater quantitative accuracy from Auger spectra, and improvements in data gathering techniques, have led to the development of various background subtraction techniques.
Similarly, the use of background subtraction techniques in XPS has evolved mainly from the interest in the determination of chemical states (from the binding-energy values for component peaks that may often overlap), greater quantitative accuracy from the XPS spectra, and improvements in data acquisition. Post-acquisition background subtraction is normally applied to XPS data.
The procedures outlined in Section 7 are popular in XPS and AES; less popular procedures and rarely used procedures are described in Sections 8 and 9, respectively. General reviews of background subtraction methods and curve-fitting techniques have been published (1-5).  
Background subtraction is usually done before peak fitting. Some commercial systems require background removal. Nevertheless, a measured spectral region consisting of one or more peaks and background intensities due to inelastic scattering, Bremsstrahlung (for XPS with unmonochromated X-ray sources), and scattered primary electrons (for AES) can often be satisfactorily represented by choosing functions for each intensity component with parameters for each component determined in a single least-squares fit. The choice of the background to be removed if required or desired before peak fitting is suggested by the experience of the analysts and the peak complexity as noted above.
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1.1 The purpose of this guide is to familiarize the analyst with the principal background subtraction techniques presently in use together with the nature of their application to data acquisition and manipulation.
1.2 This guide is intended to apply to background subtraction in electron, X-ray, and ion-excited Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS).
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 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.

SIGNIFICANCE AND USE
When electron beam excitation is used in AES, the incident electron beam can interact with the specimen material causing physical and chemical changes. In general, these effects are a hindrance to AES analysis because they cause localized specimen modification (1-4).  
With specimens that have poor electrical conductivity the electron beam can stimulate the development of localized charge on the specimen surface. This effect is a hindrance to AES analysis because the potentials associated with the charge can either adversely affect the integrity of Auger data or make Auger data collection difficult (5, 6).
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1.1 This guide outlines the origins and manifestations of unwanted electron beam effects in Auger electron spectroscopy (AES).
1.2 Some general guidelines are provided concerning the electron beam parameters which are most likely to produce these effects and suggestions are offered on how to minimize them.
1.3 General classes of materials are identified which are most likely to exhibit unwanted electron beam effects. In addition, a tabulation of some specific materials which have been observed to undergo electron damage effects is provided.
1.4 A simple method is outlined for establishing the existence and extent of these effects during routine AES analysis.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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.

SIGNIFICANCE AND USE
Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.
Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
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1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.
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 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.

SIGNIFICANCE AND USE
X-ray photoelectron spectroscopy is used extensively for the surface analysis of materials. Elements (with the exception of hydrogen and helium) are identified from comparisons of the binding energies determined from photoelectron spectra with tabulated values. Information on chemical state can be derived from the chemical shifts of measured photoelectron and Auger-electron features with respect to those measured for elemental solids.
Calibrations of the BE scales of XPS instruments are required for four principal reasons. First, meaningful comparison of BE measurements from two or more XPS instruments requires that the BE scales be calibrated, often with an uncertainty of about 0.1 eV to 0.2 eV. Second, identification of chemical state is based on measurement of chemical shifts of photoelectron and Auger-electron features, again with an uncertainty of typically about 0.1 eV to 0.2 eV; individual measurements, therefore, should be made and literature sources need to be available with comparable or better accuracies. Third, the availability of databases (3) of measured BEs for reliable identification of elements and determination of chemical states by computer software requires that published data and local measurements be made with uncertainties of about 0.1 eV to 0.2 eV. Finally, the growing adoption of quality management systems, such as, ISO 9001:2000, in many analytical laboratories has led to requirements that the measuring and test equipment be calibrated and that the relevant measurement uncertainties be known.
The actual uncertainty of a BE measurement depends on instrument properties and stability, measurement conditions, and the method of data analysis. This practice makes use of tolerance limits ±δ (chosen, for example, at the 95 % confidence level) that represent the maximum likely uncertainty of a BE measurement, associated with the instrument in a specified time interval following a calibration (ISO 15472:2001). A user should select a value of δ ba...
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1.1 This practice describes a procedure for calibrating the electron binding-energy (BE) scale of an X-ray photoelectron spectrometer that is to be used for performing spectroscopic analysis of photoelectrons excited by unmonochromated aluminum or magnesium Kα X-rays or by monochromated aluminum Kα X-rays.
1.2 The calibration of the BE scale is recommended after the instrument is installed or modified in any substantive way. Additional checks and, if necessary, recalibrations are recommended at intervals chosen to ensure that BE measurements are statistically unlikely to be made with an uncertainty greater than a tolerance limit, specified by the analyst, based on the instrumental stability and the analyst's needs. Information is provided by which the analyst can select an appropriate tolerance limit for the BE measurements and the frequency of calibration checks.
1.3 This practice is based on the assumption that the BE scale of the spectrometer is sufficiently close to linear to allow for calibration by measurements of reference photoelectron lines having BEs near the extremes of the working BE scale. In most commercial instruments, X-ray sources with aluminum or magnesium anodes are employed and BEs are typically measured over the 0–1000 eV range. This practice can be used for the BE range from 0 eV to 1040 eV.
1.4 The assumption that the BE scale is linear is checked by a measurement made with a reference photoelectron line or Auger-electron line that appears at an intermediate position. A single check is a necessary but not sufficient condition for establishing linearity of the BE scale. Additional checks can be made with specified reference lines on instruments equipped with magnesium or unmonochromated aluminum X-ray sources, with secondary BE standards, or by following the procedures of the instrument manufacturer. Deviations from BE-scale linearity can occur because of mechanical misalignments, excessive ma...

SIGNIFICANCE AND USE
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.
AES, XPS, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations from improper specimen handling (1).  
This guide describes methods to minimize the effects of specimen handling on the results obtained using surface-sensitive analytical techniques. It is intended for the specimen owner or the purchaser of surface analytical services and the surface analyst. Because of the wide range of types of specimens and desired information, only broad guidelines and general examples are presented here. The optimum handling procedures will be dependent on the particular specimen and the needed information. It is recommended that the specimen supplier consult the surface analyst as soon as possible with regard to specimen history, the specific problem to be solved or information needed, and the particular specimen preparation or handling procedures required. The surface analyst also is referred to Guide E 1078 that discusses additional procedures for preparing, mounting, and analysis of specimens.
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1.1 This guide covers specimen handling and preparation prior to surface analysis and applies to the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA), and
1.1.3 Secondary ion mass spectrometry (SIMS).
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods may also apply to many surface-sensitive analysis methods, such as ion scattering spectrometry, low-energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface-sensitive measurements.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.

SIGNIFICANCE AND USE
The acquisition of chemical information from variations in the energy position of peaks in the XPS spectrum is of primary interest in the use of XPS as a surface analytical tool. Surface charging acts to shift spectral peaks independent of their chemical relationship to other elements on the same surface. The desire to eliminate the influence of surface charging on the peak positions and peak shapes has resulted in the development of several empirical methods designed to assist in the interpretation of the XPS peak positions, determine surface chemistry, and allow comparison of spectra of conducting and non-conducting systems of the same element. It is assumed that the spectrometer is generally working properly for non-insulating specimens (see Practice E 902).
Although highly reliable methods have now been developed to stabilize surface potentials during XPS analysis of most materials (5, 6), no single method has been developed to deal with surface charging in all circumstances (10, 11). For insulators, an appropriate choice of any control or referencing system will depend on the nature of the specimen, the instruments, and the information needed. The appropriate use of charge control and referencing techniques will result in more consistent, reproducible data. Researchers are strongly urged to report both the control and referencing techniques that have been used, the specific peaks and binding energies used as standards (if any), and the criteria applied in determining optimum results so that the appropriate comparisons may be made.
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1.1 This guide acquaints the X-ray photoelectron spectroscopy (XPS) user with the various charge control and charge shift referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens and provides information needed for reporting the methods used to customers or in the literature.
1.2 This guide is intended to apply to charge control and charge referencing techniques in XPS and is not necessarily applicable to electron-excited systems.
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 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.

SIGNIFICANCE AND USE
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.
AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1) or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.
This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.
Guide E 1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
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1.1 This guide covers specimen preparation and mounting prior to, during, and following surface analysis and applies to the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA), and
1.1.3 Secondary ion mass spectrometry, (SIMS).
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will also apply to many surface sensitive analysis methods, such as ion scattering spectrometry, low energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface sensitive measurements.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.

SIGNIFICANCE AND USE
Auger electron spectroscopy yields information concerning the chemical and physical state of a solid surface in the near surface region. Nondestructive depth profiling is limited to this near surface region. Techniques for measuring the crater depths and film thicknesses are given in (1).  
Ion sputtering is primarily used for depths of less than the order of 1 μm.
Angle lapping or mechanical cratering is primarily used for depths greater than the order of 1 μm.
The choice of depth profiling methods for investigating an interface depends on surface roughness, interface roughness, and film thickness (2).
The depth profile interface widths can be measured using a logistic function which is described in Practice E 1636.
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1.1 This guide covers procedures used for depth profiling in Auger electron spectroscopy.
1.2 Guidelines are given for depth profiling by the following:
Section Ion Sputtering 6 Angle Lapping and Cross-Sectioning 7 Mechanical Cratering 8 Mesh Replica Method9 Nondestructive Depth Profiling 10
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 does not purport to address all of the safety problems, 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.

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1.1 This practice outlines the necessary steps for the identification of elements in a given Auger spectrum obtained using conventional electron spectrometers. Spectra displayed as either the electron energy distribution (direct spectrum) or the first derivative of the electron energy distribution are considered.
1.2 This practice applies to Auger spectra generated by electron or X-ray bombardment of the specimen surface and can be extended to spectra generated by other methods such as ion bombardment.
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 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.

SIGNIFICANCE AND USE
The analyst may use this document to obtain information on the properties of electron spectrometers and instrumental aspects associated with quantitative surface analysis.
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1.1 The purpose of this guide is to familiarize the analyst with some of the relevant literature describing the physical properties of modern electrostatic electron spectrometers.
1.2 This guide is intended to apply to electron spectrometers generally used in Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).
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.

SIGNIFICANCE AND USE
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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1.1 This guide outlines the types of chemical effects and matrix effects which are observed in Auger electron spectroscopy.
1.2 Guidelines are given for the reporting of chemical and matrix effects in Auger spectra.
1.3 Guidelines are given for utilizing Auger chemical effects for identification or characterization.
1.4 This guide is applicable to both electron excited and X-ray excited Auger electron spectroscopy.
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.

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1.1 This practice describes a procedure for calibrating the electron binding-energy (BE) scale of an X-ray photoelectron spectrometer that is to be used for surface analysis with unmonochromated aluminum or magnesium K X-rays or monochromated aluminum K X rays.
1.2 It is recommended that the BE scale be calibrated after the instrument is installed or modified in any substantive way. Also, it is recommended that the instrumental BE scale be checked, and if necessary, recalibrated at intervals chosen to ensure that BE measurements are statistically unlikely to be made with greater uncertainty than a tolerance limit, specified by the analyst, based on the instrumental stability and the analyst's needs. Information is provided by which an analyst can select an appropriate tolerance limit for the BE measurements and the frequency of calibration checks.
1.3 This practice is based on the assumption that the BE scale of the spectrometer is sufficiently close to linear that the BE scale can be calibrated by measurements of reference photoelectron lines made near the extremes of the working BE scale. In most commercial instruments, X-ray sources with aluminum or magnesium anodes are employed and BEs are typically measured over the 0-1000 eV range. This practice can be used for the BE range from 0 eV to 1040 eV.
1.4 The assumption that the BE scale is linear is checked by a measurement made with a reference photoelectron line or Auger-electron line that appears at an intermediate position. A single check is a necessary but not sufficient condition for establishing linearity of the BE scale. Additional checks can be made with specified reference lines on instruments equipped with magnesium or unmonochromated aluminum X-ray sources, with secondary BE standards, or by following the procedures of the instrument manufacturer. Deviations from BE-scale linearity can occur because of mechanical misalignments, excessive magnetic fields in the region of the analyzer, or imperfections or malfunctions in the power supplies. This practice does not check for, nor identify, problems of this type.
1.5 After an initial check of the BE-scale linearity and measurements of the repeatability standard deviation for the main calibration lines for a particular instrument, a simplified procedure is given for routine checks of the calibration at subsequent times.
1.6 This practice is recommended for use with X-ray photoelectron spectrometers operated in the constant-pass-energy or fixed-analyzer-transmission mode and for which the pass energy is less than 200 eV; otherwise, depending on the configuration of the instrument, a relativistic equation could be needed for the calibration equation. The practice should not be used for instruments operated in the constant-retardation-ratio mode at retardation ratios less than 10, for instruments with an energy resolution worse than 1.5 eV, or in applications for which BE measurements are desired with tolerance limits of 0.03 eV or less.
1.7 On instruments equipped with a monochromated aluminum K X-ray source, a measurement of the position of a specified Auger-electron line can be used, if desired, to determine the average energy of the X rays incident on the specimen. This information is needed for the determination of modified Auger parameters.
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.

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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 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, and in which an auxiliary electron gun can be mounted to produce an electron beam of variable energy on the specimen.
1.2 This practice is recommended as a useful means for determining the specimen area viewed by the analyzer for different conditions of spectrometer operation, for verifying adequate specimen and beam alignment, and for characterizing the imaging properties of the electron energy analyzer.
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.

SCOPE
1.1 This guide outlines the origins and manifestations of unwanted electron beam effects in Auger electron spectroscopy (AES).
1.2 Some general guidelines are provided concerning the electron beam parameters which are most likely to produce these effects and suggestions are offered on how to minimize them.
1.3 General classes of materials are identified which are most likely to exhibit unwanted electron beam effects. In addition, a tabulation of some specific materials which have been observed to undergo electron damage effects is provided.
1.4 A simple method is outlined for establishing the existence and extent of these effects during routine AES analysis.
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.

SIGNIFICANCE AND USE
Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.
Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
SCOPE
1.1 Auger and x-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.  
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.  
1.3 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.

SIGNIFICANCE AND USE
Background subtraction techniques in AES were originally employed as a method of enhancement of the relatively weak Auger signals to distinguish them from the slowly varying background of secondary and backscattered electrons. Interest in obtaining useful information from the Auger peak line shape, concern for greater quantitative accuracy from Auger spectra, and improvements in data gathering techniques, have led to the development of various background subtraction techniques.
Similarly, the use of background subtraction techniques in XPS has evolved mainly from the interest in the determination of chemical states (binding energy values), greater quantitative accuracy from the XPS spectra, and improvements in data acquisition. Post-acquisition background subtraction is normally applied to XPS data.
The procedures outlined are popular in XPS and AES. General reviews of background subtraction techniques have been published (1 and 2 ).3
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with the principal background subtraction techniques presently in use together with the nature of their application to data acquisition and manipulation.
1.2 This guide is intended to apply to background subtraction in electron, X-ray, and ion-excited Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS).
1.3 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.

SIGNIFICANCE AND USE
Auger electron spectroscopy yields information concerning the chemical and physical state of a solid surface in the near surface region. Nondestructive depth profiling is limited to this near surface region. Techniques for measuring the crater depths and film thicknesses are given in (35).
Ion sputtering is primarily used for depths of less than the order of 1 μm.
Angle lapping or mechanical cratering is primarily used for depths greater than the order of 1 μm.
The choice of depth profiling methods for investigating an interface depends on surface roughness, interface roughness, and film thickness (1).3
SCOPE
1.1 This guide covers procedures used for depth profiling in Auger electron spectroscopy.
1.2 Guidelines are given for depth profiling by the following:SectionIon Sputtering6Angle Lapping and Cross-Sectioning7Mechanical Cratering8Nondestructive Depth Profiling9
1.3 This standard does not purport to address all of the safety problems, 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.

SIGNIFICANCE AND USE
The acquisition of chemical information from variations in the energy position of peaks in the XPS spectrum is of primary interest in the use of XPS as a surface analytical tool. Surface charging acts to shift spectral peaks independent of their chemical relationship to other elements on the same surface. The desire to eliminate the influence of surface charging on the peak positions and peak shapes has resulted in the development of several empirical methods designed to assist in the interpretation of the XPS peak positions, determine surface chemistry, and allow comparison of spectra of conducting and nonconducting systems of the same element. It is assumed that the spectrometer is generally working properly for non-insulating specimens (see Practice E 902).
No ideal method has been developed to deal with surface charging (3, 4). For insulators, an appropriate choice of any control or referencing system will depend on the nature of the specimen, the instruments, and the information needed. The appropriate use of charge control and referencing techniques will result in more consistent, reproducible data. Researchers are strongly urged to report both the control and referencing techniques that have been used, the specific peaks and binding energies used as standards (if any), and the criteria applied in determining optimum results so that the appropriate comparisons may be made.
SCOPE
1.1 This guide covers the acquainting of the XPS user with the various charge control and charge shift referencing techniques that are and have been used in the acquisition and interpretation of X-ray photoelectron spectroscopy (XPS) data from surfaces of insulating specimens.
1.2 This guide is intended to apply to charge control and charge referencing techniques in XPS and is not necessarily applicable to electron-excited systems.
1.3 SI units are standard unless otherwise noted.
1.4 This standard does not purport to address all of the safety problems, 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.

SIGNIFICANCE AND USE
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.
Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS or ESCA), and secondary ion mass spectrometry (SIMS) are sensitive to surface layers that are typically a few nanometers (nm) thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1)3 or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.
This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.
Guide E 1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
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1.1 This guide covers specimen preparation and mounting prior to, during, and following surface analysis and applies to the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA), and
1.1.3 Secondary ion mass spectrometry, (SIMS).
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will also apply to many surface sensitive analysis methods, such as ion scattering spectrometry, low energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface sensitive measurements.
1.2 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.

SIGNIFICANCE AND USE
Auger analysis is used to determine the elemental composition of the first few atomic layers, typically 0.5 to 2.0 nm thick, of a specimen surface. In conjunction with inert gas ion sputtering, it is used to determine the sputter depth profile to a depth of a few micrometres.
The specimen is normally a solid conductor, semiconductor, or insulator. For insulators, provisions may be required for control of charge accumulation at the surface (see Guide E 1523). Typical applications include the analysis of thin film deposits or segregated overlayers on metallic or alloy substrates. The specimen topography may vary from a smooth, polished specimen to a rough fracture surface.
Auger analysis of specimens with volatile species that evaporate in the ultra-high vacuum environment of the Auger chamber and substances which are susceptible to electron or X-ray beam damage, such as organic compounds, may require special techniques not covered herein. (See Guide E 983.)
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1.1 This practice outlines the necessary steps for the identification of elements in a given Auger spectrum obtained using conventional electron spectrometers. Spectra displayed as either the electron energy distribution (direct spectrum) or the first derivative of the electron energy distribution are considered.
1.2 This practice applies to Auger spectra generated by electron or X-ray bombardment of the specimen surface and can be extended to spectra generated by other methods such as ion bombardment.
1.3 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.

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1.1 This guide covers specimen handling and preparation prior to surface analysis and applies to the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA), and
1.1.3 Secondary ion mass spectrometry, SIMS.
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods may also apply to many surface-sensitive analysis methods, such as ion scattering spectrometry, low-energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface-sensitive measurements.
1.2 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.

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1.1 This practice outlines the necessary steps for the identification of elements in a given Auger spectrum obtained using conventional electron spectrometers. Spectra displayed as either the electron energy distribution (direct spectrum) or the first derivative of the electron energy distribution are considered.
1.2 This practice applies to Auger spectra generated by electron or X-ray bombardment of the specimen surface and can be extended to spectra generated by other methods such as ion bombardment.
1.3 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.

SIGNIFICANCE AND USE
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.
Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and secondary ion mass spectroscopy (SIMS) are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations from improper specimen handling (1).3  
This guide describes methods to minimize the effects of specimen handling on the results obtained using surface-sensitive analytical techniques. It is intended for the specimen owner or the purchaser of surface analytical services and the surface analyst. Because of the wide range of types of specimens and desired information, only broad guidelines and general examples are presented here. The optimum handling procedures will be dependent on the particular specimen and the needed information. It is recommended that the specimen supplier consult the surface analyst as soon as possible with regard to specimen history, the specific problem to be solved or information needed, and the particular specimen preparation or handling procedures required. The surface analyst also is referred to Guide E 1078 that discusses additional procedures for preparing, mounting, and analysis of specimens.
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1.1 This guide covers specimen handling and preparation prior to surface analysis and applies to the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA), and
1.1.3 Secondary ion mass spectrometry, SIMS.
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods may also apply to many surface-sensitive analysis methods, such as ion scattering spectrometry, low-energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface-sensitive measurements.
1.2 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.

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1.1 This guide outlines the types of chemical effects and matrix effects which are observed in Auger electron spectroscopy.  
1.2 Guidelines are given for the reporting of chemical and matrix effects in Auger spectra.  
1.3 Guidelines are given for utilizing Auger chemical effects for identification or characterization.  
1.4 This guide is applicable to both electron excited and X-ray excited Auger electron spectroscopy.  
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.

SCOPE
1.1 This guide outlines the types of chemical effects and matrix effects which are observed in Auger electron spectroscopy.  
1.2 Guidelines are given for the reporting of chemical and matrix effects in Auger spectra.  
1.3 Guidelines are given for utilizing Auger chemical effects for identification or characterization.  
1.4 This guide is applicable to both electron excited and X-ray excited Auger electron spectroscopy.  
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.

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1.1 This practice describes a procedure for calibrating the electron binding-energy (BE) scale of an X-ray photoelectron spectrometer that is to be used for surface analysis with unmonochromated aluminum or magnesium K X-rays or monochromated aluminum K X rays.
1.2 It is recommended that the BE scale be calibrated after the instrument is installed or modified in any substantive way. Also, it is recommended that the instrumental BE scale be checked, and if necessary, recalibrated at intervals chosen to ensure that BE measurements are statistically unlikely to be made with greater uncertainty than a tolerance limit, specified by the analyst, based on the instrumental stability and the analyst's needs. Information is provided by which an analyst can select an appropriate tolerance limit for the BE measurements and the frequency of calibration checks.
1.3 This practice is based on the assumption that the BE scale of the spectrometer is sufficiently close to linear that the BE scale can be calibrated by measurements of reference photoelectron lines made near the extremes of the working BE scale. In most commercial instruments, X-ray sources with aluminum or magnesium anodes are employed and BEs are typically measured over the 0-1000 eV range. This practice can be used for the BE range from 0 eV to 1040 eV.
1.4 The assumption that the BE scale is linear is checked by a measurement made with a reference photoelectron line or Auger-electron line that appears at an intermediate position. A single check is a necessary but not sufficient condition for establishing linearity of the BE scale. Additional checks can be made with specified reference lines on instruments equipped with magnesium or unmonochromated aluminum X-ray sources, with secondary BE standards, or by following the procedures of the instrument manufacturer. Deviations from BE-scale linearity can occur because of mechanical misalignments, excessive magnetic fields in the region of the analyzer, or imperfections or malfunctions in the power supplies. This practice does not check for, nor identify, problems of this type.
1.5 After an initial check of the BE-scale linearity and measurements of the repeatability standard deviation for the main calibration lines for a particular instrument, a simplified procedure is given for routine checks of the calibration at subsequent times.
1.6 This practice is recommended for use with X-ray photoelectron spectrometers operated in the constant-pass-energy or fixed-analyzer-transmission mode and for which the pass energy is less than 200 eV; otherwise, depending on the configuration of the instrument, a relativistic equation could be needed for the calibration equation. The practice should not be used for instruments operated in the constant-retardation-ratio mode at retardation ratios less than 10, for instruments with an energy resolution worse than 1.5 eV, or in applications for which BE measurements are desired with tolerance limits of 0.03 eV or less.
1.7 On instruments equipped with a monochromated aluminum K X-ray source, a measurement of the position of a specified Auger-electron line can be used, if desired, to determine the average energy of the X rays incident on the specimen. This information is needed for the determination of modified Auger parameters.
1.8 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. ^REFERENCE: ^REFDOCID: E 456^REFDOCTITLE: Terminology Relating to Quality and Statistics^REFDOCID: E 673^REFDOCTITLE: Terminology Relating to Surface Analysis^REFDOCID: E 902^REFDOCTITLE: Practice for Checking the Operating Characteristics of X-Ray Photoelectron Spectrometers^REFDOCID: E 1016^REFDOCTITLE: Guide for Literature Describing Properties of Electrostatic Electron Spe...

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1.1 This practice describes methods for determining the specimen area contributing to the detected signal in X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) when this area is defined by the electron collection lens/aperture system. It is recommended as a useful means of determining the observed specimen area for different conditions of spectrometer operation, verifying adequate specimen alignment, and characterizing the imaging properties of the electron energy analyzer.
1.2 This practice is intended only for spectrometers in which the specimen area excited by X-ray or electron beams is or can be made larger than the specimen area viewed by the analyzer. It is assumed that, under normal conditions of operation, the specimen is excited by a beam of X rays or electrons that can be considered to have a uniform intensity over the specimen area viewed by the analyzer, and the specimen is homogeneous and uniform over the observed area.
1.3 This standard does not purport to address all of the safety problems, 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.

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1.1 This practice covers a procedure for checking some of the operating characteristics of an X-ray photoelectron spectrometer. Tests herein provide checks of the following instrument characteristics: X-ray photoelectron spectroscopy (XPS) signal intensity, background, energy resolution, short-term voltage stability, transmission, and energy scale linearity. It is meant for spectrometers with digital storage of counts in energy channels.
1.2 Limitations -This practice is meant to augment, and not to replace, the calibration procedures recommended by the manufacturer of the spectrometer. This practice is also not meant to be used as a means of comparison between X-ray photoelectron spectrometers, but only as a self-consistent check of the operating characteristics of an individual spectrometer.
1.3 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.

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1.1 Auger and x-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.  
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.  
1.3 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.