ISO/TS 25138:2019
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.
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Foreword
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Apparatus
5.1 Glow-discharge optical-emission spectrometer
5.1.1 General
5.1.2 Selection of spectral lines
5.1.3 Selection of glow-discharge source type
6 Adjusting the glow-discharge spectrometer system settings
6.1 General
6.2 Setting the parameters of a DC source
6.2.1 Constant applied current and voltage
6.2.2 Constant applied current and pressure
6.2.3 Constant voltage and pressure
6.3 Setting the discharge parameters of an RF source
6.3.1 General
6.3.2 Constant applied voltage and pressure
6.3.3 Constant applied power and DC bias voltage
6.3.4 Constant effective power and RF voltage
6.4 Minimum performance requirements
6.4.1 General
6.4.2 Minimum repeatability
6.4.3 Detection limit
7 Sampling
8 Calibration
8.1 General
8.2 Calibration samples
8.2.1 General
8.2.2 Low alloy iron or steel samples
8.2.3 Stainless-steel samples
8.2.4 Nickel alloy samples
8.2.5 Copper alloy samples
8.2.6 Titanium alloy samples
8.2.7 Silicon samples
8.2.8 Aluminium alloy samples
8.2.9 High-oxygen samples
8.2.10 High-carbon samples
8.2.11 High-nitrogen samples
8.2.12 High-hydrogen samples
8.2.13 High-purity copper samples
8.3 Validation samples
8.3.1 General
8.3.2 Hot-rolled low-alloy steel
8.3.3 Oxidized silicon wafers
8.3.4 TiN-coated samples
8.3.5 Anodized Al2O3 samples
8.3.6 TiO2-coated samples
8.4 Determination of the sputtering rate of calibration and validation samples
8.5 Emission intensity measurements of calibration samples
8.6 Calculation of calibration formulae
8.7 Validation of the calibration
8.7.1 General
8.7.2 Checking analytical accuracy using bulk reference materials
8.7.3 Checking analytical accuracy using metal oxide reference materials
8.8 Verification and drift correction
9 Analysis of test samples
9.1 Adjusting discharge parameters
9.2 Setting of measuring time and data acquisition rate
9.3 Quantifying depth profiles of test samples
10 Expression of results
10.1 Expression of quantitative depth profile
10.2 Determination of metal oxide mass per unit area
10.3 Determination of the average mass fractions of the elements in the oxide
11 Precision
12 Test report
Annex A (informative) Calculation of calibration constants and quantitative evaluation ofdepth profiles
Annex B (informative) Suggested spectral lines for determination of given elements
Annex C (informative) Examples of oxide density and the corresponding quantity ρO
Annex D (informative) Report on interlaboratory testing of metal oxide films
Bibliography
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Foreword
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Apparatus
5.1 Glow-discharge optical-emission spectrometer
5.1.1 General
5.1.2 Selection of spectral lines
5.1.3 Selection of glow-discharge source type
6 Adjusting the glow-discharge spectrometer system settings
6.1 General
6.2 Setting the parameters of a DC source
6.2.1 Constant applied current and voltage
6.2.2 Constant applied current and pressure
6.2.3 Constant voltage and pressure
6.3 Setting the discharge parameters of an RF source
6.3.1 General
6.3.2 Constant applied voltage and pressure
6.3.3 Constant applied power and DC bias voltage
6.3.4 Constant effective power and RF voltage
6.4 Minimum performance requirements
6.4.1 General
6.4.2 Minimum repeatability
6.4.3 Detection limit
7 Sampling
8 Calibration
8.1 General
8.2 Calibration samples
8.2.1 General
8.2.2 Low alloy iron or steel samples
8.2.3 Stainless-steel samples
8.2.4 Nickel alloy samples
8.2.5 Copper alloy samples
8.2.6 Titanium alloy samples
8.2.7 Silicon samples
8.2.8 Aluminium alloy samples
8.2.9 High-oxygen samples
8.2.10 High-carbon samples
8.2.11 High-nitrogen samples
8.2.12 High-hydrogen samples
8.2.13 High-purity copper samples
8.3 Validation samples
8.3.1 General
8.3.2 Hot-rolled low-alloy steel
8.3.3 Oxidized silicon wafers
8.3.4 TiN-coated samples
8.3.5 Anodized Al2O3 samples
8.3.6 TiO2-coated samples
8.4 Determination of the sputtering rate of calibration and validation samples
8.5 Emission intensity measurements of calibration samples
8.6 Calculation of calibration formulae
8.7 Validation of the calibration
8.7.1 General
8.7.2 Checking analytical accuracy using bulk reference materials
8.7.3 Checking analytical accuracy using metal oxide reference materials
8.8 Verification and drift correction
9 Analysis of test samples
9.1 Adjusting discharge parameters
9.2 Setting of measuring time and data acquisition rate
9.3 Quantifying depth profiles of test samples
10 Expression of results
10.1 Expression of quantitative depth profile
10.2 Determination of metal oxide mass per unit area
10.3 Determination of the average mass fractions of the elements in the oxide
11 Precision
12 Test report
Annex A (informative) Calculation of calibration constants and quantitative evaluation ofdepth profiles
Annex B (informative) Suggested spectral lines for determination of given elements
Annex C (informative) Examples of oxide density and the corresponding quantity ρO
Annex D (informative) Report on interlaboratory testing of metal oxide films
Bibliography