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 published (1-7).55.7 There are different ways to define the spectrometer analysis area. An ISO Technical Report provides guidance on determinations of lateral resolution, analysis area, and sample area viewed by the analyzer in AES and XPS(8), and ISO 18516:2006 describes three methods for determination of lateral resolution in AES and XPS. Baer and Engelhard have used well-defined ‘dots’ of a material on a substrate to determine the area of a specimen contributing to the measured signal of a ‘small-area’ XPS measurement (9). This area could be as much as ten times the area estimated simply from the lateral resolution of the instrument. The amount of intensity in ‘fringe’ or ‘tail’ regions could also be highly dependent on lens operation and the adequacy of specimen alignment. Scheithauer described an alternative technique in which Pt apertures of varying diameters were utilized to determine the fraction of ‘long-tail’ X-ray contributions outside each aperture on the measured Pt photoelectron signal compared to that on a Pt foil (10). In test measurements on a commercial XPS instrument with a focused X-ray beam and a nominal lateral resolution of 10 μm (as determined from the distance between the positions for 20 %  and 80 % of maximum signal when scans were made across an edge), it was found that aperture diameters of about 100 μm and 450 μm were required to reduce the photoelectron signals to 10 % and 1 %, respectively, of the maximum value (10). Knowledge of the effective analysis area is important when making tradeoffs between lateral resolution and detectability. In scanning Auger microscopy, the area of analysis is determined more by the radial extent of backscattered electrons than by the radius of the primary beam (11, 12, 13).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 Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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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.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.

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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 value of δ based on the needs of the analytical work to be undertaken, the likely measurement and data-analysis conditions, the stability of the instrument, and the cost of calibrations. This practice gives information on the various sources of uncertainty in BE measurements and on measurements of instrumental stability. The analyst should initially choose some desired value for δ and then make tests, as described in 8.14 to determine from subsequent checks of the calibration whether BE measurements are made within the limits ±δ. Information is given in Appendix X1 on how to evaluate for a material of interest the uncertainty of a BE measurement that is associated with the uncertainty of the calibration procedure. This information is provided for four common analytical situations. It is important to note that some BE measurements may have uncertainties larger than δ as a result of poor counting statistics, large peak widths, uncertainties associated with peak fitting, and effects of surface charging.5.4 Instrument settings typically selected for analysis should be used with this practice. Separate calibrations should be made if key operating conditions, such as choices of analyzer pass energy, aperture sizes, or X-ray source, are varied. Settings not specified in this practice are at the discretion of the user, but those same settings should be recorded and consistently used whenever this practice is repeated in order that the current results will be directly comparable to the previous results.5.5 All of the operations described in Section 8 should be performed the first time that the BE scale is calibrated or after any substantial modification of the instrument. For later checks of the calibration, to be performed on a regular schedule, only the operations in 8.2 – 8.5, 8.10, 8.11, and 8.14 need to be performed. While the measurements described in 8.7 – 8.9 for the first calibration require moderate time and effort, they are essential for ensuring that realistic tolerance limits ±δ have been chosen. The control chart, described in 8.14, is a simple and effective means of demonstrating and documenting that the BE scale of the instrument is in calibration, that is, within the tolerance limits, for a certain period of time.5.6 The average energy of the X-rays incident on the specimen for instruments equipped with a monochromated Al X-ray source will generally be slightly higher, by up to about 0.2 eV, than the average X-ray energy for instruments equipped with an unmonochromated Al X-ray source (4). The actual energy difference depends on the alignment and thermal stability of the X-ray monochromator. An optional procedure is given in Appendix X2 to determine this energy difference from measurements of the Cu L3VV Auger-electron peak. This information is needed for the determination of modified Auger parameters and Auger-electron kinetic energies on instruments with the monochromated Al X-ray source.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, 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 but simply verifies the linearity of the BE scale.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. 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 above 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 Kα 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.9 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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This practice should first be used to establish the operating characteristics of a particular X-ray photoelectron spectrometer at a time when the spectrometer performance is known to be optimum. Hence, the spectrometer settings in Section 5 and the expected performance figures given in Section 7 are to be taken only as guides, to be supplanted by the behavior of the user’actual spectrometer. Subsequently, this practice should be used as a routine check, performed at frequent intervals with the same instrument settings, and the results compared with those obtained in 4.1. Significant deviation from optimum performance may indicate that the spectrometer requires recalibration or other maintenance. Typical analysis settings should be used with this practice. The use of settings not specified by this practice is left to the discretion of the user, however, the settings should be recorded in accordance with Practice E 996 and the same settings should be used consistently whenever this practice is repeated, so that the results obtained will be directly comparable to previous results.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 repeatability of intensity measurements and the drift of the intensities with time. This practice may be conducted at the same time as the spectrometer energy calibration using Practice E 2108.1.2 LimitationsThis 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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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.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.

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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).65.4 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 peak complexity as noted above.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.

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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.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.

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