ISO 16413:2020
(Main)Evaluation of thickness, density and interface width of thin films by X-ray reflectometry — Instrumental requirements, alignment and positioning, data collection, data analysis and reporting
Evaluation of thickness, density and interface width of thin films by X-ray reflectometry — Instrumental requirements, alignment and positioning, data collection, data analysis and reporting
This document specifies a method for the evaluation of thickness, density and interface width of single layer and multi-layered thin films which have thicknesses between approximately 1 nm and 1 μm, on flat substrates, by means of X-Ray Reflectometry (XRR). This method uses a monochromatic, collimated beam, scanning either an angle or a scattering vector. Similar considerations apply to the case of a convergent beam with parallel data collection using a distributed detector or to scanning wavelength, but these methods are not described here. While mention is made of diffuse XRR, and the requirements for experiments are similar, this is not covered in the present document. Measurements may be made on equipment of various configurations, from laboratory instruments to reflectometers at synchrotron radiation beamlines or automated systems used in industry. Attention should be paid to an eventual instability of the layers over the duration of the data collection, which would cause a reduction in the accuracy of the measurement results. Since XRR, performed at a single wavelength, does not provide chemical information about the layers, attention should be paid to possible contamination or reactions at the specimen surface. The accuracy of results for the outmost layer is strongly influenced by any changes at the surface. NOTE 1 Proprietary techniques are not described in this document.
Évaluation de l'épaisseur, de la densité et de la largeur de l'interface des films fins par réflectrométrie de rayons X — Exigences instrumentales, alignement et positionnement, rassemblement des données, analyse des données et rapport
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INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 16413
ISO/TC 201
Evaluation of thickness, density
Secretariat: JISC
and interface width of thin films by
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20200311 X-ray reflectometry — Instrumental
requirements, alignment and
Voting terminates on:
20200506
positioning, data collection, data
analysis and reporting
Évaluation de l'épaisseur, de la densité et de la largeur de l'interface
des films fins par réflectrométrie de rayons X — Exigences
instrumentales, alignement et positionnement, rassemblement des
données, analyse des données et rapport
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ISO/FDIS 16413:2020(E)
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©
NATIONAL REGULATIONS. ISO 2020
ISO/FDIS 16413:2020(E)
© ISO 2020
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
CH1214 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 2020 – All rights reserved
ISO/FDIS 16413:2020(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions, symbols and abbreviated terms . 1
3.1 Symbols and abbreviated terms. 3
4 Instrumental requirements, alignment and positioning guidelines .4
4.1 Instrumental requirements for the scanning method . 4
4.1.1 Schematic diagrams . 4
4.1.2 Incident beam — Requirements and recommendations . 5
4.1.3 Specimen — Requirements and recommendations . 7
4.1.4 Goniometer — Requirements . 8
4.1.5 Detector — Requirements . 8
4.2 Instrument alignment . 9
4.3 Specimen alignment . 9
5 Data collection and storage .11
5.1 Preliminary remarks .11
5.2 Data scan parameters .11
5.3 Dynamic range.11
5.4 Step size (peak definition) .12
5.4.1 Fixed intervals scan .12
5.4.2 Continuous scan .12
5.5 Collection time (accumulated counts) .12
5.6 Segmented data collection .12
5.7 Reduction of noise .13
5.8 Detectors .13
5.9 Environment .13
5.10 Data storage .13
5.10.1 Data output format .13
5.10.2 Headers .13
6 Data analysis .14
6.1 Preliminary data treatment .14
6.2 Specimen modelling .14
6.2.1 General.14
6.2.2 Interface width models .15
6.3 Simulation of XRR data .16
6.4 General examples .16
6.5 Data fitting .22
7 Information required when reporting XRR analysis .24
7.1 General .24
7.2 Experimental details .24
7.3 Analysis (simulation and fitting) procedures .25
7.4 Methods for reporting XRR curves .26
7.4.1 Independent and dependent variables .26
7.4.2 Graphical plotting of XRR data .26
Annex A (informative) Example of report for an oxynitrided silicon wafer .29
Bibliography .32
ISO/FDIS 16413:2020(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso .org/
iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis.
This second edition cancels and replaces the first edition (ISO 16413:2013), of which it constitutes a
minor revision. The changes compared to the previous edition are as follows:
— editorial changes, mainly for a more precise description, e.g. ‘incidence angle’ has been replaced by
‘grazing incidence angle’, ‘intensity’ has been replaced in the appropriate diagrams by ‘reflectivity’ etc.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
ISO/FDIS 16413:2020(E)
Introduction
X-Ray Reflectometry (XRR) is widely applicable to the measurement of thickness, density and interface
width of single layer and multi-layered thin films which have thicknesses between approximately 1 nm
and 1 μm, on flat substrates, provided that the layer, equipment and X-ray wavelength are appropriate.
Interface width is a general term; it is typically composed of interface or surface roughness and/or
density grading across an interface. The specimen needs to be laterally uniform under the footprint of
the X-ray beam. In contrast with typical surface chemical analysis methods which provide information
of the amount of substance and need conversion to estimate thicknesses, XRR provides thicknesses
directly traceable to the unit of length. XRR is very powerful method to measure the thickness of thin
film with SI traceability.
The key requirements for equipment suitable for collecting specular X-ray reflectivity data of high
quality, and the requirements for specimen alignment and positioning so that useful, accurate
measurements may be obtained are described in Clause 3.
The key issues for data collection to obtain specular X-ray reflectivity data of high quality, suitable
for data treatment and modelling are described in Clause 4. The collection of the data is traditionally
conducted by running single measurements under direct operator data input. However, recently data
are often collected by instructing the instrument to operate in multiple ru
...
INTERNATIONAL ISO
STANDARD 16413
Second edition
2020-08
Evaluation of thickness, density
and interface width of thin films by
X-ray reflectometry — Instrumental
requirements, alignment and
positioning, data collection, data
analysis and reporting
Évaluation de l'épaisseur, de la densité et de la largeur de l'interface
des films fins par réflectrométrie de rayons X — Exigences
instrumentales, alignement et positionnement, rassemblement des
données, analyse des données et rapport
Reference number
©
ISO 2020
© ISO 2020
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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
3.1 Terms and definitions . 1
3.2 Symbols and abbreviated terms. 3
4 Instrumental requirements, alignment and positioning guidelines .4
4.1 Instrumental requirements for the scanning method . 4
4.1.1 Schematic diagrams . 4
4.1.2 Incident beam — Requirements and recommendations . 6
4.1.3 Specimen — Requirements and recommendations . 7
4.1.4 Goniometer — Requirements . 8
4.1.5 Detector — Requirements . 8
4.2 Instrument alignment . 9
4.3 Specimen alignment . 9
5 Data collection and storage .11
5.1 Preliminary remarks .11
5.2 Data scan parameters .11
5.3 Dynamic range.11
5.4 Step size (peak definition) .12
5.4.1 Fixed intervals scan .12
5.4.2 Continuous scan .12
5.5 Collection time (accumulated counts) .12
5.6 Segmented data collection .12
5.7 Reduction of noise .13
5.8 Detectors .13
5.9 Environment .13
5.10 Data storage .13
5.10.1 Data output format .13
5.10.2 Headers .13
6 Data analysis .14
6.1 Preliminary data treatment .14
6.2 Specimen modelling .14
6.2.1 General.14
6.2.2 Interface width models .15
6.3 Simulation of XRR data .16
6.4 General examples .16
6.5 Data fitting .22
7 Information required when reporting XRR analysis .24
7.1 General .24
7.2 Experimental details .24
7.3 Analysis (simulation and fitting) procedures .25
7.4 Methods for reporting XRR curves .26
7.4.1 Independent and dependent variables .26
7.4.2 Graphical plotting of XRR data .26
Annex A (informative) Example of report for an oxynitrided silicon wafer .29
Bibliography .32
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso .org/
iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis.
This second edition cancels and replaces the first edition (ISO 16413:2013), of which it constitutes a
minor revision. The changes compared to the previous edition are as follows:
— editorial changes, mainly for a more precise description, e.g. ‘incidence angle’ has been replaced by
‘grazing incidence angle’, ‘intensity’ has been replaced in the appropriate diagrams by ‘reflectivity’ etc.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
Introduction
X-Ray Reflectometry (XRR) is widely applicable to the measurement of thickness, density and interface
width of single layer and multi-layered thin films which have thicknesses between approximately 1 nm
and 1 μm, on flat substrates, provided that the layer, equipment and X-ray wavelength are appropriate.
Interface width is a general term; it is typically composed of interface or surface roughness and/or
density grading across an interface. The specimen needs to be laterally uniform under the footprint of
the X-ray beam. In contrast with typical surface chemical analysis methods which provide information
of the amount of substance and need conversion to estimate thicknesses, XRR provides thicknesses
directly traceable to the unit of length. XRR is very powerful method to measure the thickness of thin
film with SI traceability.
The key requirements for equipment suitable for collecting specular X-ray reflectivity data of high
quality, and the requirements for specimen alignment and positioning so that useful, accurate
measurements may be obtained are described in Clause 4.
The key issues for data collection to obtain specular X-ray reflectivity data of high quality, suitable
for data treatment and modelling are described in Clause 5. The collection of the data is traditionally
conducted by running single measurements under direct operator data input. However, recently data
are often collected by instructing the instrument to operate in multiple runs. In addition to the operator
mode, data can be collected making use of automated scripts, when available in the software program
controlling the instrument.
The principles for analysing specular XRR data in order to obtain physically meaningful material
information about the specimen are described in Clause 6. While specular XRR fitting can be a
complex pr
...
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