ISO/TS 25138
(Main)Surface chemical analysis — Analysis of metal oxide films by glow discharge optical emission spectrometry
Surface chemical analysis — Analysis of metal oxide films by glow discharge optical emission spectrometry
This document describes a glow-discharge optical-emission spectrometric method for the determination of the thickness, mass per unit area and chemical composition of metal oxide films. This method is applicable to oxide films 1 nm to 10 000 nm thick on metals. The metallic elements of the oxide can include one or more from Fe, Cr, Ni, Cu, Ti, Si, Mo, Zn, Mg, Mn, Zr and Al. Other elements that can be determined by the method are O, C, N, H, P and S.
Analyse chimique des surfaces — Analyse de films d'oxyde de métal par spectrométrie d'émission optique à décharge luminescente
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ISO/DTS 25138
ISO/TC 201/SC 8
Surface chemical analysis —
Secretariat: JISC
Analysis of metal oxide films by
Voting begins on:
glow discharge optical emission
2024-11-26
spectrometry
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2025-01-21
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ISO/DTS 25138:2024(en) © ISO 2024
FINAL DRAFT
ISO/DTS 25138:2024(en)
Technical
Specification
ISO/DTS 25138
ISO/TC 201/SC 8
Surface chemical analysis —
Secretariat: JISC
Analysis of metal oxide films by
Voting begins on:
glow discharge optical emission
spectrometry
Voting terminates on:
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
AND TO PROVIDE SUPPOR TING DOCUMENTATION.
© ISO 2024
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
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Phone: +41 22 749 01 11
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Published in Switzerland Reference number
ISO/DTS 25138:2024(en) © ISO 2024
ii
ISO/DTS 25138:2024(en)
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
5.1 Glow discharge optical emission spectrometer .2
5.1.1 General .2
5.1.2 Selection of spectral lines.2
5.1.3 Selection of glow discharge source type .2
6 Adjusting the glow discharge spectrometer system settings . 3
6.1 General .3
6.2 Setting the parameters of a DC source .4
6.2.1 Constant applied current and voltage .4
6.2.2 Constant applied current and pressure .5
6.2.3 Constant voltage and pressure .5
6.3 Setting the discharge parameters of an RF source .6
6.3.1 General .6
6.3.2 Constant applied voltage and pressure .6
6.3.3 Constant applied power and DC bias voltage .7
6.3.4 Constant effective power and RF voltage.7
6.4 Minimum performance requirements .7
6.4.1 General .7
6.4.2 Minimum repeatability .8
6.4.3 Detection limit .8
6.4.4 Control of lamp cleanliness and start-up performance .9
7 Sampling .11
8 Calibration .11
8.1 General .11
8.2 Calibration samples .11
8.2.1 General .11
8.2.2 Low alloy iron or steel samples . 12
8.2.3 Stainless-steel samples . 12
8.2.4 Nickel alloy samples . 12
8.2.5 Copper alloy samples . 12
8.2.6 Titanium alloy samples . 12
8.2.7 Silicon samples . 12
8.2.8 Aluminium alloy samples . 12
8.2.9 High-oxygen samples . 12
8.2.10 High-carbon samples . 12
8.2.11 High-nitrogen samples . 12
8.2.12 High-hydrogen samples . . 13
8.2.13 High-purity copper samples . 13
8.3 Validation samples . 13
8.3.1 General . 13
8.3.2 Hot-rolled low-alloy steel . 13
8.3.3 Oxidized silicon wafers. 13
8.3.4 TiN-coated samples. 13
8.3.5 Anodized Al O samples . 13
2 3
8.3.6 TiO -coated samples . 13
8.4 Determination of the sputtering rate of calibration and validation samples . 13
8.5 Emission intensity measurements of calibration samples . 15
iii
ISO/DTS 25138:2024(en)
8.6 Calculation of calibration formulae . 15
8.7 Validation of the calibration . 15
8.7.1 General . 15
8.7.2 Checking analytical accuracy using bulk reference materials .16
8.7.3 Checking analytical accuracy using metal oxide reference materials .16
8.8 Verification and drift correction .16
9 Analysis of test samples . 17
9.1 Adjusting discharge parameters .17
9.2 Setting of measuring time and data acquisition rate .17
9.3 Quantifying depth profiles of test samples .17
10 Expression of results .18
10.1 Expression of quantitative depth profile .18
10.2 Determination of metal oxide mass per unit area .18
10.3 Determination of the average mass fractions of the elements in the oxide .
...
ISO TC201 SC8
ISO /DTS 25138 (ed.3):xxxx(E)
ISO /TC 201/SC 8
Secretariat: JISC
Surface chemical analysis — Analysis of metal oxide films by glow
discharge optical emission spectrometry
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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
EmailE-mail: copyright@iso.org
Website: www.iso.orgwww.iso.org
Published in Switzerland
© ISO 2024 – All rights reserved
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ISO CD TS/DTS 25138-#:####(X:(en)
Contents
Foreword . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
6 Adjusting the glow discharge spectrometer system settings . 4
7 Sampling . 12
8 Calibration . 13
9 Analysis of test samples . 19
10 Expression of results . 20
11 Precision . 22
12 Test report . 22
Annex A (informative) Calculation of calibration constants and quantitative evaluation ofdepth
profiles . 24
Annex B (informative) Suggested spectral lines for determination of given elements . 37
Annex C (informative) Examples of oxide density and the corresponding quantity ρ . 39
O
Annex D (informative) Report on interlaboratory testing of metal oxide films . 40
Bibliography . 47
Foreword . v
Introduction .vii
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
5.1 Glow discharge optical emission spectrometer . 2
6 Adjusting the Glow discharge spectrometer system settings . 4
6.1 General . 4
6.2 Setting the parameters of a DC source . 5
6.3 Setting the discharge parameters of an RF source . 7
6.4 Minimum performance requirements . 9
7 Sampling . 12
8 Calibration . 13
8.1 General . 13
8.2 Calibration samples. 13
8.3 Validation samples . 15
8.4 Determination of the sputtering rate of calibration and validation samples . 15
iv © ISO 2024 – All rights reserved
iv
ISO CD TS25138-#:####(X/DTS 25138:(en)
8.5 Emission intensity measurements of calibration samples . 17
8.6 Calculation of calibration formulae . 17
8.7 Validation of the calibration . 18
8.8 Verification and drift correction . 19
9 Analysis of test samples . 19
9.1 Adjusting discharge parameters . 19
9.2 Setting of measuring time and data acquisition rate . 19
9.3 Quantifying depth profiles of test samples . 20
10 Expression of results . 20
10.1 Expression of quantitative depth profile . 20
10.2 Determination of metal oxide mass per unit area . 21
10.3 Determination of the average mass fractions of the elements in the oxide . 22
11 Precision . 22
12 Test report . 22
Annex A (informative) Calculation of calibration constants and quantitative evaluation of depth
profiles . 23
A.1 Symbols . 23
A.2 Calculation of calibration constants using relative sputtering rates . 24
A.3 Calculation of calibration constants using absolute sputtering rates . 26
A.4 Correction of elemental intensities and sputtered mass for variations in discharge
parameters . 27
A.5 Correction of emission yields due to the influence of hydrogen . 29
A.6 Calculation of mass fractions and sputtered mass using relative sputtering rates. 30
A.7 Calculation of mass fractions and sputtered mass using absolute sputtering rates . 32
A.8 Calculation of sputtered depth . 33
Annex B (informative) Suggested spectral lines for determination of given elements . 36
Annex C (informative) Examples of oxide density and the corresponding quantity ρ . 38
O
Annex D (informative) Report on interlaboratory testing of metal oxide films . 39
D.1 General . 39
D.2 Description of samples included in the trial . 39
D.3 Determination of oxide film thickness. 40
Bibliography . 46
© ISO 2024 – All rights reserved
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ISO CD TS/DTS 25138-#:####(X:(en)
Foreword
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This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee
SC 8, Glow discharge spectroscopy.
This third edition cancels and replaces the second edition (ISO/TS 25138:2019), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— — Theupdated listed types of array detectors have been updated.;
— A note stating that pulsed mode now is available in several commercially available instruments.
— — The anode size 2.,5 mm has been added to those commonly offered in commercial instruments.;
— — Checkingverifying that test specimens and other sa
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