Determination of modulation period of nano-multilayer coatings by low-angle X-ray methods

This document specifies the substrate conditions and testing of the modulation period (including the principles for low-angle X-ray methods, the requirements of the coatings, the requirements for X-ray measuring apparatus, the calibration of apparatus and samples, and the testing conditions and calculation process) of nano-multilayer coatings by low-angle X-ray methods including X-ray reflectivity (XRR) and glancing incident X-ray diffraction (GIXRD).

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Status
Published
Publication Date
21-Jul-2022
Current Stage
6060 - International Standard published
Due Date
21-Apr-2023
Completion Date
22-Jul-2022
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ISO 24688:2022 - Determination of modulation period of nano-multilayer coatings by low-angle X-ray methods Released:22. 07. 2022
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INTERNATIONAL ISO
STANDARD 24688
First edition
2022-07
Determination of modulation period
of nano-multilayer coatings by low-
angle X-ray methods
Reference number
ISO 24688:2022(E)
© ISO 2022
---------------------- Page: 1 ----------------------
ISO 24688:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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© ISO 2022 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 24688:2022(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction .................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Substrate conditions ........................................................................................................................................................................................1

5 Testing of modulation period ................................................................................................................................................................. 1

5.1 Principle for low-angle X-ray methods .............................................................................................................................. 1

5.1.1 General ........................................................................................................................................................................................ 1

5.1.2 XRR method ............................................................................................................................................................................ 1

5.1.3 GIXRD method ...................................................................................................................................................................... 2

5.1.4 Calculating formula.......................................................................................................................................................... 3

5.2 Specifications concerning the coated sample ............................................................................................................. 4

5.2.1 Size specifications for the coated sample..................................................................................................... 4

5.2.2 Periods specifications for the coated sample ........................................................................................... 4

5.2.3 Surface roughness requirements of the coated sample .................................................................. 4

5.3 Specifications for X-ray measuring apparatus ........................................................................................................... 5

5.3.1 Apparatus configuration ............................................................................................................................................. 5

5.3.2 Beam conversion device .............................................................................................................................................. 5

5.3.3 Radiation sources and filters .................................................................................................................................. 5

5.4 Calibrating of apparatus ................................................................................................................................................................ 5

5.5 Testing conditions ............................................................................................................................................................................... 6

5.6 Test and calculation procedure ............................................................................................................................................... 6

Annex A (informative) Process of determination of modulation period by XRR .................................................7

iii
© ISO 2022 – All rights reserved
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ISO 24688:2022(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

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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

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iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 107, Metallic and other inorganic coatings,

Subcommittee SC 9, Physical vapor deposition coatings.

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.
© ISO 2022 – All rights reserved
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ISO 24688:2022(E)
Introduction

Nano-multilayer coatings by physical vapor deposition (PVD), which possess high coating-substrate

adhesion, high hardness and good wear resistance, corrosion resistance and conductive resistance,

have been widely applied on tools, moulds, microelectronics and other important parts to improve their

service life. Nano-multilayers formed by depositing two materials alternately at nanometer scale have

attracted considerable interest due to their superior physical and chemical properties. The modulation

period refers to the thickness of these two alternate layers.

Based on the chemical compositions, the main nano-multilayer coatings involve metal/metal, metal/

ceramic and ceramic/ceramic systems such as Cu/Ni, Cu/W, Cu/Ag, Ti/TiN, Cr/CrN, Zr/ZrN, TiN/CrN,

CrN/AlCrN, TiC/TiCN and CrAlN/AlCrTiSiN. The key factor influencing the properties of nano-multilayer

coatings was previously the modulation period, which has an important effect on properties including

hardness, toughness, electromagnetic and optical property. For example, as the modulation period

decreases, the hardness of the nano-multilayer coatings increases. At present, the high-resolution

projection electron microscope (HR-TEM) and the X-ray methods including the X-ray reflectivity (XRR)

and glancing incident X-ray diffraction (GIXRD) are the two common methods for determining the

modulation period of the nano-multilayer coatings. X-ray methods are more suitable for determination

of the modulation period due to the advantages of being non-destructive, statistical, convenient and

accurate compared with HR-TEM.

However, there is not yet any standard to qualify the modulation period of these nano-multilayer

coatings, which limits their further development.

Thus, the motivation of this document is to prescribe the calculation of the modulation period of the

nano-multilayer hard coatings and the measurement conditions of X-ray methods. The modulation

period is an important technical indicator of the nano-multilayer coatings, which can also provide the

communication bridge for customers who want to use the coatings, tool coater and analytic service

provider. This document can be used for quality assurance of products with nano-multilayer coatings.

© ISO 2022 – All rights reserved
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INTERNATIONAL STANDARD ISO 24688:2022(E)
Determination of modulation period of nano-multilayer
coatings by low-angle X-ray methods
1 Scope

This document specifies the substrate conditions and testing of the modulation period (including

the principles for low-angle X-ray methods, the requirements of the coatings, the requirements for

X-ray measuring apparatus, the calibration of apparatus and samples, and the testing conditions and

calculation process) of nano-multilayer coatings by low-angle X-ray methods including X-ray reflectivity

(XRR) and glancing incident X-ray dif
...

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