Surface chemical analysis — X-ray photoelectron spectroscopy — Guidelines for analysis

This document is intended to aid the operators of X-ray photoelectron spectrometers in their analysis of typical samples. It takes the operator through the analysis from the handling of the sample and the calibration and setting-up of the spectrometer to the acquisition of wide and narrow scans and also gives advice on quantification and on preparation of the final report.

Analyse chimique des surfaces — Spectroscopie de photoélectrons par rayons X — Lignes directrices pour l'analyse

General Information

Status
Published
Publication Date
21-Aug-2019
Current Stage
9020 - International Standard under periodical review
Start Date
15-Jul-2024
Completion Date
15-Jul-2024
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ISO 10810:2019 - Surface chemical analysis — X-ray photoelectron spectroscopy — Guidelines for analysis Released:8/22/2019
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INTERNATIONAL ISO
STANDARD 10810
Second edition
2019-08
Surface chemical analysis — X-ray
photoelectron spectroscopy —
Guidelines for analysis
Analyse chimique des surfaces — Spectroscopie de photoélectrons par
rayons X — Lignes directrices pour l'analyse
Reference number
©
ISO 2019
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviations . 1
5 Overview of sample analysis . 2
6 Specimen characterization . 4
6.1 General . 4
6.2 Specimen forms . 5
6.2.1 General. 5
6.2.2 Single crystal . 5
6.2.3 Adsorbed or segregated layers, films and residues . 5
6.2.4 Interfaces and multilayered samples . 6
6.2.5 Non-porous . 6
6.2.6 Porous . 6
6.2.7 Powder . . 6
6.2.8 Fibres and textiles . 6
6.2.9 Internal interface . 6
6.3 Material types . 6
6.3.1 General. 6
6.3.2 Metals and alloys . 6
6.3.3 Polymers . 7
6.3.4 Semiconductors . 7
6.3.5 Magnetic materials . 7
6.3.6 Ceramics . 7
6.3.7 Catalysts . 7
6.3.8 Glass and insulators . 7
6.3.9 Biological . 7
6.3.10 Nanoparticles . 7
6.4 Handling and mounting of specimens . 7
6.5 Specimen treatments . 8
6.5.1 General. 8
6.5.2 Heating and cooling . 8
6.5.3 Scraping and fracture . . 8
6.5.4 Ion bombardment for analysing thin films . 8
6.5.5 Exposure to gases and liquids . 8
[8]
7 Instrument characterization . 8
7.1 General . 8
7.2 Instrument checks . 9
[9]
7.2.1 System health check . 9
7.2.2 Mechanical . 9
7.2.3 Sample holder . 9
7.2.4 Vacuum . 9
7.3 Instrument calibration .10
7.3.1 Calibration of binding energy scale .10
7.3.2 Intensity repeatability and intensity/energy response function (IERF).11
7.3.3 Linearity of intensity scale test .12
7.3.4 Lateral resolution .13
[21][22]
7.3.5 Depth resolution .13
7.3.6 Charge correction .16
7.4 Instrument set-up.16
7.4.1 Optimum settings .16
7.4.2 System configuration .17
8 The wide-scan spectrum .17
8.1 Data acquisition .17
8.1.1 General.17
8.1.2 Sample loading .18
8.1.3 Energy resolution .18
8.1.4 Energy range, step size and acquisition mode .18
8.1.5 X-ray source and conditions .18
8.1.6 Charge correction .19
8.1.7 Spectrum acquisition .19
8.1.8 X-ray degradation .19
8.1.9 Thin surface layer .19
8.2 Data analysis .19
8.2.1 Calibration of the binding energy scale .19
8.2.2 Peak table .20
8.2.3 Quantification .20
8.2.4 Assessment of the composition employing the Tougaard extrinsic
[42]
background  .21
8.2.5 Requirement for narrow scans .21
9 The narrow scan .21
9.1 General .
...


INTERNATIONAL ISO
STANDARD 10810
Second edition
2019-08
Surface chemical analysis — X-ray
photoelectron spectroscopy —
Guidelines for analysis
Analyse chimique des surfaces — Spectroscopie de photoélectrons par
rayons X — Lignes directrices pour l'analyse
Reference number
©
ISO 2019
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviations . 1
5 Overview of sample analysis . 2
6 Specimen characterization . 4
6.1 General . 4
6.2 Specimen forms . 5
6.2.1 General. 5
6.2.2 Single crystal . 5
6.2.3 Adsorbed or segregated layers, films and residues . 5
6.2.4 Interfaces and multilayered samples . 6
6.2.5 Non-porous . 6
6.2.6 Porous . 6
6.2.7 Powder . . 6
6.2.8 Fibres and textiles . 6
6.2.9 Internal interface . 6
6.3 Material types . 6
6.3.1 General. 6
6.3.2 Metals and alloys . 6
6.3.3 Polymers . 7
6.3.4 Semiconductors . 7
6.3.5 Magnetic materials . 7
6.3.6 Ceramics . 7
6.3.7 Catalysts . 7
6.3.8 Glass and insulators . 7
6.3.9 Biological . 7
6.3.10 Nanoparticles . 7
6.4 Handling and mounting of specimens . 7
6.5 Specimen treatments . 8
6.5.1 General. 8
6.5.2 Heating and cooling . 8
6.5.3 Scraping and fracture . . 8
6.5.4 Ion bombardment for analysing thin films . 8
6.5.5 Exposure to gases and liquids . 8
[8]
7 Instrument characterization . 8
7.1 General . 8
7.2 Instrument checks . 9
[9]
7.2.1 System health check . 9
7.2.2 Mechanical . 9
7.2.3 Sample holder . 9
7.2.4 Vacuum . 9
7.3 Instrument calibration .10
7.3.1 Calibration of binding energy scale .10
7.3.2 Intensity repeatability and intensity/energy response function (IERF).11
7.3.3 Linearity of intensity scale test .12
7.3.4 Lateral resolution .13
[21][22]
7.3.5 Depth resolution .13
7.3.6 Charge correction .16
7.4 Instrument set-up.16
7.4.1 Optimum settings .16
7.4.2 System configuration .17
8 The wide-scan spectrum .17
8.1 Data acquisition .17
8.1.1 General.17
8.1.2 Sample loading .18
8.1.3 Energy resolution .18
8.1.4 Energy range, step size and acquisition mode .18
8.1.5 X-ray source and conditions .18
8.1.6 Charge correction .19
8.1.7 Spectrum acquisition .19
8.1.8 X-ray degradation .19
8.1.9 Thin surface layer .19
8.2 Data analysis .19
8.2.1 Calibration of the binding energy scale .19
8.2.2 Peak table .20
8.2.3 Quantification .20
8.2.4 Assessment of the composition employing the Tougaard extrinsic
[42]
background  .21
8.2.5 Requirement for narrow scans .21
9 The narrow scan .21
9.1 General .
...

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