PVD multi-layer hard coatings — Composition, structure and properties

This document specifies the evaluation standard of the composition, structure and properties of multi-layer hard coatings by common physical vapor deposition (PVD), indicating a vacuum deposition method that produces a material source by evaporation, sputtering or related non-chemical ways.

Revêtements durs multicouches déposés par PVD — Composition, structure et propriétés

General Information

Status
Published
Publication Date
29-Oct-2019
Current Stage
6060 - International Standard published
Start Date
30-Oct-2019
Completion Date
30-Oct-2019
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ISO 21874:2019 - PVD multi-layer hard coatings -- Composition, structure and properties
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INTERNATIONAL ISO
STANDARD 21874
First edition
2019-10
PVD multi-layer hard coatings —
Composition, structure and properties
Revêtements durs multicouches déposés par PVD — Composition,
structure et propriétés
Reference number
ISO 21874:2019(E)
ISO 2019
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ISO 21874:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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ii © ISO 2019 – All rights reserved
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ISO 21874:2019(E)
Contents Page

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

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

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

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

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

4 Samples for composition, structure and properties evaluation ......................................................................... 1

5 Testing of composition, structure and properties ............................................................................................................. 1

5.1 Testing of chemical composition ............................................................................................................................................. 1

5.2 Testing of layer structure ............................................................................................................................................................... 2

5.3 Testing of surface deficiency ....................................................................................................................................................... 3

5.4 Testing of thickness ............................................................................................................................................................................. 4

5.5 Testing of properties .......................................................................................................................................................................... 4

5.5.1 Hardness ................................................................................................................................................................................. 4

5.5.2 Friction and wear ............................................................................................................................................................ 6

Annex A (informative) Sample preparation and operation of transmission electron microscopy .....7

Annex B (informative) Example of a surface deficiency rate calculation ....................................................................... 9

© ISO 2019 – All rights reserved iii
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ISO 21874:2019(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 107, Metallic and other inorganic coatings,

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.
iv © ISO 2019 – All rights reserved
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ISO 21874:2019(E)
Introduction

Multi-layer hard coatings by physical vapor deposition (PVD), which possess high coating-substrate

adhesion, high hardness and good wear resistance, are widely applied on tools and machine parts to

improve their service life. Based on the chemical compositions, the mainstream PVD multi-layer hard

coatings in the market involve transition metal nitrides and carbides, such as Ti/TiN, TiN/CrN, CrN/

AlCrN, TiC/TiCN and CrAlN/AlCrTiSiN. To date, there has been no standard to qualify the composition,

structure and properties of these multi-layer hard coatings, which has limited their further

development.

This document defines the measurement and evaluation of the composition, microstructure, surface

quality, thickness, hardness and tribological properties (such as friction and wear performance) of

multi-layer hard coatings. The methods are for the purpose of coating development. Where standards

for quality assurance in production exist, they are referred to in this document.

© ISO 2019 – All rights reserved v
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INTERNATIONAL STANDARD ISO 21874:2019(E)
PVD multi-layer hard coatings — Composition, structure
and properties
1 Scope

This document specifies the evaluation standard of the composition, structure and properties of

multi-layer hard coatings by common physical vapor deposition (PVD), indicating a vacuum deposition

method that produces a material source by evaporation, sputtering or related non-chemical ways.

2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 4545-1, Metallic materials — Knoop hardness test — Part 1: Test method
ISO 6507-1, Metallic materials — Vickers hardness test — Part 1: Test method

ISO 9220, Metallic coatings — Measurement of coating thickness — Scanning electron microscope method

ISO 14577-1, Metallic materials — Instrumented indentation test for hardness and materials parameters

— Part 1: Test method

ISO 20808, Fine ceramics (advanced ceramics, advanced technical ceramics) — Determination of friction

and wear characteristics of monolithic ceramics by ball-on-disc method

ISO 26423, Fine ceramics (advanced ceramics, advanced technical ceramics) — Determination of coating

thickness by crater-grinding method
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Samples for composition, structure and properties evaluation

Samples for the composition, structure and properties evaluation should be coated in the same batch

as the products requiring the composition, structure and properties evaluation. The samples should be

polished to a mirror finish (R < 0,05 μm) before being coated and cleaned using ultrasonic agitation,

which immerses them in the correct solution to remove hydrocarbons and other surface contaminants.

5 Testing of composition, structure and properties
5.1 Testing of chemical composition

The chemical composition of PVD multi-layer hard coatings is decided by many factors, including

the composition of the evaporator source, the energy density of incident atoms/ions, the deposition

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ISO 21874:2019(E)

pressure and the bias voltage. Various elements in the evaporator source can segregate during

deposition, which results in different contents in the coatings. Testing methods that can be used to

characterize the chemical compositions of PVD multi-layer hard coatings are energy dispersive

spectrometer (EDS), electron probe micro analysis (EPMA), X-ray photoelectron spectrometer (XPS),

auger electron spectrometer (AES), secondary ion mass spectrometry (SIMS), X-ray fluorescence (XRF)

and glow discharge optical emission spectroscopy (GDOES). The details are shown in Table 1.

Table 1 — Testing methods of chemical compositions of PVD multi-layer hard coatings

Surface area Cross-sectional area
Testing
Maps and line scans
B, C, N and O B, C, N and O
method
Metal elements Metal elements
elements elements
Recommend-
Recommended Recommended Recommended
ed (monolayer
EDS (excluding Li and (excluding B and (excluding B and Recommended
thickness more
Be) C) C)
than 100 nm)
EPMA Recommended Recommended Recommended Recommended Recommended
Recommended Recommended Recommended
XPS Recommended Recommended
(only by etching) (only by etching) (destructive)
Preferably Preferably
AES Recommended Recommended Recommended
recommended recommended
Preferably Preferably Preferably Preferably Recommended
SIMS
recommended recommended recommended recommended (destructive)
XRF Recommended — — — —
Preferably rec- Preferably rec-
Preferably Preferably Recommended
GDOES ommended (only ommended (only
recommended recommended (destructive)
by etching) by etching)
5.2 Testing of layer structure

Different structures of PVD hard coatings observed by electron microscope, including columnar crystal,

equiaxed crystal and amorphous, lead to different grain or crystallite types, boundary energy and

texture, which influence their hardness, internal stress, toughness and adhesion. Therefore, structure

testing is essential for coating evaluation.

PVD multi-layer hard coatings can be defined in two classes. The first class comprises several different

layers consecutively, including the adhesive layer, transition layer, hard core layer and/or surface

adaptive layer for lubrication, hydrophobicity, electroconductivity, etc, as shown in Figure 1 a). The

other class comprises two kinds of layers, in which every two adjacent layers constitute a unit and the

thickness is called the "modulation period" (Λ = λ + λ ; λ and λ are the thickness of the A layer and

A B A B

B layer, respectively). It is called "nano-layered coating" when Λ is less than 100 nm or "super-lattice

coating", as shown in Figure 1 b).

Methods such as SIMS, scanning electron microscope (SEM) and transmission electron microscope

(TEM) are able to detect and confirm the layer structure of coatings. Detailed information about

analysing the layer structure by TEM is given in Annex A.
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ISO 21874:2019(E)
a) Several d
...

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