Metallic and oxide coatings - Measurement of coating thickness - Microscopical method (ISO 1463:2021)

This document specifies a method for the measurement of the local thickness of metallic coatings, oxide
layers, and porcelain or vitreous enamel coatings, by the microscopical examination of cross-sections
using an optical microscope.

Metall- und Oxidschichten - Schichtdickenmessung - Mikroskopisches Verfahren (ISO 1463:2021)

Dieses Dokument legt ein Verfahren zur Messung der örtlichen Schichtdicke von metallischen Überzügen, Oxidschichten und Emailschichten durch Untersuchung der Querschnittflächen mit einem Lichtmikroskop fest.
WARNUNG Die Anwendung dieser Norm kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Ausrüstungen mit sich bringen. Diese Norm erhebt nicht den Anspruch, auf alle Sicherheitsprobleme hinzuweisen, die mit ihrer Anwendung verbunden sind. Es liegt in der Verantwortung des Anwenders dieser Norm, vor ihrer Anwendung geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz des Personals zu ergreifen und dafür Sorge zu tragen, dass behördliche und gesetzliche Maßnahmen eingehalten werden.

Revêtements métalliques et couches d'oxyde - Mesurage de l'épaisseur de revêtement - Méthode par coupe micrographique (ISO 1463:2021)

Kovinske in oksidne prevleke - Merjenje debeline prevleke - Mikroskopska metoda (ISO 1463:2021)

General Information

Status
Published
Public Enquiry End Date
04-Sep-2020
Publication Date
14-Jun-2021
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
03-Jun-2021
Due Date
08-Aug-2021
Completion Date
15-Jun-2021

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SLOVENSKI STANDARD
SIST EN ISO 1463:2021
01-julij-2021
Nadomešča:
SIST EN ISO 1463:2004
Kovinske in oksidne prevleke - Merjenje debeline prevleke - Mikroskopska metoda
(ISO 1463:2021)

Metallic and oxide coatings - Measurement of coating thickness - Microscopical method

(ISO 1463:2021)

Metall- und Oxidschichten - Schichtdickenmessung - Mikroskopisches Verfahren (ISO

1463:2021)

Revêtements métalliques et couches d'oxyde - Mesurage de l'épaisseur de revêtement -

Méthode par coupe micrographique (ISO 1463:2021)
Ta slovenski standard je istoveten z: EN ISO 1463:2021
ICS:
25.220.20 Površinska obdelava Surface treatment
25.220.40 Kovinske prevleke Metallic coatings
SIST EN ISO 1463:2021 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN ISO 1463:2021
---------------------- Page: 2 ----------------------
SIST EN ISO 1463:2021
EN ISO 1463
EUROPEAN STANDARD
NORME EUROPÉENNE
May 2021
EUROPÄISCHE NORM
ICS 25.220.20; 25.220.40 Supersedes EN ISO 1463:2004
English Version
Metallic and oxide coatings - Measurement of coating
thickness - Microscopical method (ISO 1463:2021)

Revêtements métalliques et couches d'oxyde - Metall- und Oxidschichten - Schichtdickenmessung -

Mesurage de l'épaisseur de revêtement - Méthode par Mikroskopisches Verfahren (ISO 1463:2021)

coupe micrographique (ISO 1463:2021)
This European Standard was approved by CEN on 17 April 2021.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 1463:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 1463:2021
EN ISO 1463:2021 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

---------------------- Page: 4 ----------------------
SIST EN ISO 1463:2021
EN ISO 1463:2021 (E)
European foreword

This document (EN ISO 1463:2021) has been prepared by Technical Committee ISO/TC 107 "Metallic

and other inorganic coatings" in collaboration with Technical Committee CEN/TC 262 “Metallic and

other inorganic coatings, including for corrosion protection and corrosion testing of metals and alloys”

the secretariat of which is held by BSI.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by November 2021, and conflicting national standards

shall be withdrawn at the latest by November 2021.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 1463:2004.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 1463:2021 has been approved by CEN as EN ISO 1463:2021 without any modification.

---------------------- Page: 5 ----------------------
SIST EN ISO 1463:2021
---------------------- Page: 6 ----------------------
SIST EN ISO 1463:2021
INTERNATIONAL ISO
STANDARD 1463
Fourth edition
2021-05
Metallic and oxide coatings —
Measurement of coating thickness —
Microscopical method
Revêtements métalliques et couches d'oxyde — Mesurage de
l'épaisseur de revêtement — Méthode par coupe micrographique
Reference number
ISO 1463:2021(E)
ISO 2021
---------------------- Page: 7 ----------------------
SIST EN ISO 1463:2021
ISO 1463:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

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 2021 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 1463:2021
ISO 1463:2021(E)
Contents Page

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 1

5 Factors relating to measurement uncertainty ....................................................................................................................... 1

5.1 Surface roughness ................................................................................................................................................................................ 1

5.2 Taper of cross-section ....................................................................................................................................................................... 2

5.3 Deformation of coating .................................................................................................................................................................... 2

5.4 Rounding of edge of coating ........................................................................................................................................................ 2

5.5 Overplating ................................................................................................................................................................................................. 2

5.6 Etching ........................................................................................................................................................................................................... 2

5.7 Smearing ....................................................................................................................................................................................................... 2

5.8 Magnification ............................................................................................................................................................................................ 2

5.9 Calibration of stage micrometer .............................................................................................................................................. 2

5.10 Calibration of the microscope’s length measuring device ................................................................................. 2

5.10.1 Micrometer eyepiece .................................................................................................................................................... 2

5.10.2 Digital image processing ........................................................................................................................................... 3

5.11 Uniformity of magnification ........................................................................................................................................................ 3

5.12 Lens quality ................................................................................................................................................................................................ 3

5.13 Orientation of measuring lines ................................................................................................................................................. 3

5.14 Tube length ................................................................................................................................................................................................ 3

6 Preparation of cross-sections ................................................................................................................................................................. 4

7 Measurement ........................................................................................................................................................................................................... 4

8 Measurement uncertainty .......................................................................................................................................................................... 4

9 Test report ................................................................................................................................................................................................................... 4

Annex A (informative) Guidance on the preparation and measurement of cross-sections ........................6

Annex B (informative) Taper of cross-section and measurement of tooth-constructed coatings ........9

Annex C (informative) Some typical etchants for use at room temperature ...........................................................12

Bibliography .............................................................................................................................................................................................................................13

© ISO 2021 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 1463:2021
ISO 1463:2021(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,

in collaboration with the European Committee for Standardization (CEN) Technical Committee CEN/

TC 262, Metallic and other inorganic coatings, including for corrosion protection and corrosion testing of

metals and alloys, in accordance with the Agreement on technical cooperation between ISO and CEN

(Vienna Agreement).

This fourth edition cancels and replaces the third edition (ISO 1463:2003), which has been technically

revised.
The main changes compared with the previous edition are as follows:
— digital image processing for light microscopes has been added;

— further hints and methods for the preparation of microsections have been added;

— one hazardous etching recipe has been removed from Annex C.

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 2021 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 1463:2021
INTERNATIONAL STANDARD ISO 1463:2021(E)
Metallic and oxide coatings — Measurement of coating
thickness — Microscopical method

WARNING — The use of this document can involve hazardous materials, operations and

equipment. This document does not purport to address all of the safety problems associated

with its use. It is the responsibility of users of this document to take appropriate measures to

ensure the safety and health of personnel prior to the application of the document.

1 Scope

This document specifies a method for the measurement of the local thickness of metallic coatings, oxide

layers, and porcelain or vitreous enamel coatings, by the microscopical examination of cross-sections

using an optical microscope.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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/
3.1
local thickness

mean of the thickness measurements, of which a specified number is made within a reference area

[SOURCE: ISO 2064:1996, 3.4]
4 Principle

A portion of the test specimen is cut out and mounted. The mounted cross-section is prepared by

suitable techniques of grinding, polishing and etching. The thickness of the coating cross-section is

measured by means of a calibrated scale.

NOTE These techniques will be familiar to experienced metallographers, but some guidance is given in

Clause 5 and in Annex A for less experienced operators.
5 Factors relating to measurement uncertainty
5.1 Surface roughness

If the coating or its substrate has a rough surface, one or both of the interfaces bounding the coating

cross-section could be too irregular to permit accurate measurement (see A.6).
© ISO 2021 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 1463:2021
ISO 1463:2021(E)
5.2 Taper of cross-section

If the plane of the cross-section is not perpendicular to the plane of the coating, the measured thickness

will be greater than the true thickness, e.g. an inclination of 10° to the perpendicular will contribute a

1,5 % uncertainty.
NOTE B.1 provides guidance on the taper of a cross-section.
5.3 Deformation of coating

Detrimental deformation of the coating can be caused by excessive temperature or pressure during

mounting and preparation of cross-sections of soft coatings or coatings that melt at a low temperature,

and also by excessive abrasion of brittle materials during preparation of cross-sections.

5.4 Rounding of edge of coating

If the edge of the coating cross-section is rounded, i.e. if the coating cross-section is not completely flat

up to its edges, the true thickness cannot be observed microscopically. Edge rounding can be caused

by improper mounting, grinding, polishing or etching. It is usually minimized by overplating the test

specimen before mounting (see A.2).
5.5 Overplating

Overplating of the test specimen protects the coating edges during preparation of cross-sections and

thus prevents erroneous measurement. Removal of coating material during surface preparation for

overplating can result in a low thickness measurement.
5.6 Etching

Optimum etching produces a clearly defined and narrow dark line at the interface of two metals.

Excessive etching produces a poorly defined or wide line that can result in erroneous measurement.

5.7 Smearing

Improper polishing or overplating with a softer metal can cause smearing of one metal over the other

metal, obscuring the boundary between the coating and the substrate. This problem can be alleviated

by repeating the preparation of the cross-section of the coated metal until repeatability of the thickness

measurement (see A.3 and A.5) is obtained and also by overplating with a harder metal.

5.8 Magnification

For any given coating thickness, measurement uncertainty generally increases with decreasing

magnification. The magnification should be chosen so that the field of view is between 1,5 × and 3 × the

coating thickness.
5.9 Calibration of stage micrometer

Any uncertainty in calibration of the stage micrometer will be reflected in the measurement of the

specimen. A suitable, traceable length standard shall be used.
5.10 Calibration of the microscope’s length measuring device
5.10.1 Micrometer eyepiece

A filar micrometer eyepiece provides a satisfactory means of making the measurement of the specimen.

The measurement will be no more accurate than the calibration of the eyepiece. As calibration is

operator dependent, the eyepiece shall be calibrated by the person making the measurement.

2 © ISO 2021 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 1463:2021
ISO 1463:2021(E)

Repeated calibrations of the micrometer eyepiece can be reasonably expected to have a spread of less

than 1 %. The distance between the two lines of a stage micrometer used for the calibration shall be

known to within 0,2 µm or 0,1 %, whichever is the greater.

Some image splitting micrometer eyepieces have a nonlinearity that introduces an uncertainty of up to

1 % for short measurement distances.

Uncertainties can be introduced by backlash in the movement of the micrometer eyepiece. To avoid this

uncertainty, ensure that the final motion during alignment of the hairline is always made in the same

direction.
5.10.2 Digital image processing

Microscopes with a triocular tube, camera adapters with projecting lens and digital cameras connected

to a computer with software for image capturing and processing are nowadays state of the art. Similar

to 5.10.1, the measurement will be no more accurate than the adjustment and calibration of the length

measurement function (combination of hardware and software).

For adjustment, digital images from the stage micrometer (in both directions parallel to the x- and y-axis

of the image) are recorded for
...

SLOVENSKI STANDARD
oSIST prEN ISO 1463:2020
01-september-2020
Kovinske in oksidne prevleke - Merjenje debeline prevleke - Mikroskopska metoda
(ISO/DIS 1463:2020)

Metallic and oxide coatings - Measurement of coating thickness - Microscopical method

(ISO/DIS 1463:2020)
Metall- und Oxidschichten - Schichtdickenmessung - Mikroskopisches Verfahren
(ISO/DIS 1463:2020)

Revêtements métalliques et couches d'oxyde - Mesurage de l'épaisseur de revêtement -

Méthode par coupe micrographique (ISO/DIS 1463:2020)
Ta slovenski standard je istoveten z: prEN ISO 1463
ICS:
25.220.20 Površinska obdelava Surface treatment
25.220.40 Kovinske prevleke Metallic coatings
oSIST prEN ISO 1463:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 1463:2020
---------------------- Page: 2 ----------------------
oSIST prEN ISO 1463:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 1463
ISO/TC 107 Secretariat: KATS
Voting begins on: Voting terminates on:
2020-05-15 2020-08-07
Metallic and oxide coatings — Measurement of coating
thickness — Microscopical method

Revêtements métalliques et couches d'oxyde — Mesurage de l'épaisseur de revêtement — Méthode par

coupe micrographique
ICS: 25.220.20; 25.220.40
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 1463:2020(E)
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 SUPPORTING DOCUMENTATION. ISO 2020
---------------------- Page: 3 ----------------------
oSIST prEN ISO 1463:2020
ISO/DIS 1463:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© 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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 1463:2020
ISO/DIS 1463:2020(E)
Contents Page

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 1

5 Factors relating to measurement uncertainty ....................................................................................................................... 2

5.1 Surface roughness ................................................................................................................................................................................ 2

5.2 Taper of cross-section ....................................................................................................................................................................... 2

5.3 Deformation of coating .................................................................................................................................................................... 2

5.4 Rounding of edge of coating ........................................................................................................................................................ 2

5.5 Overplating ................................................................................................................................................................................................. 2

5.6 Etching ........................................................................................................................................................................................................... 2

5.7 Smearing ....................................................................................................................................................................................................... 2

5.8 Magnification ............................................................................................................................................................................................ 2

5.9 Calibration of stage micrometer .............................................................................................................................................. 2

5.10 Calibration of the microscope’s length measuring device ................................................................................. 3

5.10.1 Micrometer eyepiece .................................................................................................................................................... 3

5.10.2 Digital image processing ........................................................................................................................................... 3

5.11 Uniformity of magnification ........................................................................................................................................................ 3

5.12 Lens quality ................................................................................................................................................................................................ 3

5.13 Orientation of measuring lines ................................................................................................................................................. 4

5.14 Tube length ................................................................................................................................................................................................ 4

6 Preparation of cross-sections ................................................................................................................................................................. 4

7 Measurement ........................................................................................................................................................................................................... 4

8 Measurement uncertainty .......................................................................................................................................................................... 4

9 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Guidance on the preparation and measurement of cross-sections ........................6

Annex B (informative) Taper of cross-section and measurement of tooth-constructed coatings ........9

Annex C (informative) Some typical etchants for use at room temperature ...........................................................12

Bibliography .............................................................................................................................................................................................................................13

© ISO 2020 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 1463:2020
ISO/DIS 1463:2020(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 107, Metallic and other inorganic coatings.

This third fourth edition cancels and replaces the third edition (ISO 1463:2003), which has been

technically revised.
The main changes compared to the previous edition are as follows:
— digital image processing for light microscopes added;
— further hints and methods for the preparation of microsections added;
— some hazardous etching recipes removed from Annex C;
— editorial changes.

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
---------------------- Page: 6 ----------------------
oSIST prEN ISO 1463:2020
DRAFT INTERNATIONAL STANDARD ISO/DIS 1463:2020(E)
Metallic and oxide coatings — Measurement of coating
thickness — Microscopical method
1 Scope

This document specifies a method for the measurement of the local thickness of metallic coatings, oxide

layers, and porcelain or vitreous enamel coatings, by the microscopical examination of cross sections

using an optical microscope.

WARNING — The use of this Standard can involve hazardous materials, operations and

equipment. This Standard does not purport to address all of the safety problems associated with

its use. It is the responsibility of users of this standard to take appropriate measures to ensure

the safety and health of personnel prior to application of the standard, and fulfil statutory and

regulatory requirements for this purpose.
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 2064, Metallic and other inorganic coatings — Definitions and conventions concerning the measurement

of thickness
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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/
3.1
local thickness

the mean of the thickness measurements, of which a specified number is made within a reference area

[SOURCE: ISO 2064:1996, 3.4]
4 Principle

A portion of the test specimen is cut out and mounted. The mounted cross-section is prepared by

suitable techniques of grinding, polishing and etching. The thickness of the coating cross-section is

measured by means of a calibrated scale.

NOTE These techniques will be familiar to experienced metallographers, but some guidance is given in

Clause 5 and in Annex A for less experienced operators.
© ISO 2020 – All rights reserved 1
---------------------- Page: 7 ----------------------
oSIST prEN ISO 1463:2020
ISO/DIS 1463:2020(E)
5 Factors relating to measurement uncertainty
5.1 Surface roughness

If the coating or its substrate has a rough surface, one or both of the interfaces bounding the coating

cross-section may be too irregular to permit accurate measurement (see A.5).
5.2 Taper of cross-section

If the plane of the cross-section is not perpendicular to the plane of the coating, the measured thickness

will be greater than the true thickness; e.g. an inclination of 10° to the perpendicular will contribute a

1,5 % uncertainty.
NOTE B.1 provides guidance on taper cross-section.
5.3 Deformation of coating

Detrimental deformation of the coating can be caused by excessive temperature or pressure during

mounting and preparation of cross-sections of soft coatings or coatings that melt at a low temperature,

and also by excessive abrasion of brittle materials during preparation of cross-sections.

5.4 Rounding of edge of coating

If the edge of the coating cross-section is rounded, i.e. if the coating cross-section is not completely flat

up to its edges, the true thickness cannot be observed microscopically. Edge rounding can be caused

by improper mounting, grinding, polishing or etching. It is usually minimized by overplating the test

specimen before mounting (see A.2).
5.5 Overplating

Overplating of the test specimen protects the coating edges during preparation of cross-sections and

thus prevents erroneous measurement. Removal of coating material during surface preparation for

overplating can result in a low thickness measurement.
5.6 Etching

Optimum etching produces a clearly defined and narrow dark line at the interface of two metals.

Excessive etching produces a poorly defined or wide line that can result in erroneous measurement.

5.7 Smearing

Improper polishing or overplating with a softer metal may cause smearing of one metal over the other

metal, obscuring the boundary between the coating and the substrate. This problem may be alleviated

by repeating the preparation of the cross section of the coated metal until repeatability of the thickness

measurement (see A.3 and A.5) is obtained and also by overplating with a harder metal.

5.8 Magnification

For any given coating thickness, measurement uncertainty generally increases with decreasing

magnification. The magnification should be chosen so that the field of view is between 1,5 × and 3 × the

coating thickness.
5.9 Calibration of stage micrometer

Any uncertainty in calibration of the stage micrometer will be reflected in the measurement of the

specimen. A suitable, traceable length standard shall be used.
2 © ISO 2020 – All rights reserved
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oSIST prEN ISO 1463:2020
ISO/DIS 1463:2020(E)
5.10 Calibration of the microscope’s length measuring device
5.10.1 Micrometer eyepiece

A filar micrometer eyepiece provides a satisfactory means of making the measurement of the specimen.

The measurement will be no more accurate than the calibration of the eyepiece. As calibration is

operator dependent, the eyepiece shall be calibrated by the person making the measurement.

Repeated calibrations of the micrometer eyepiece can be reasonably expected to have a spread of less

than 1 %. The distance between the two lines of a stage micrometer used for the calibration shall be

known to within 0,2 µm or 0,1 %, whichever is the greater.

Some image splitting micrometer eyepieces have a nonlinearity that introduces an uncertainty of up to

1 % for short measurement distances.

Uncertainties can be introduced by backlash in the movement of the micrometer eyepiece. To avoid this

uncertainty, ensure that the final motion during alignment of the hairline is always made in the same

direction.
5.10.2 Digital image processing

Microscopes with triocular tube, camera adapter with projecting lens and digital camera connected to

a computer with a software for image capturing and processing are nowadays state-of-the-art. Similar

to 5.10.1 the measurement will be no more accurate than the adjustment and calibration of the length

measurement function (combination of hard- and software).

For adjustment digital images from the stage micrometer (in both directions parallel to the x- and y-axis

of the image) are recorded for every combination of objective, eventual intermediate magnification

changer, and resolution setting of the camera (full resolution and typical settings of pixel binning). The

length in object space represented by a pixel of the digital image is calculated by measuring a known

distance on the stage micrometer with the respective function of the software and is then saved in

the software. Usually after such an adjustment the images are recorded “calibrated”, i.e. with the µm/

pixel factor assigned to the image, by selecting the objective, the eventual intermediate magnification

changer, and the pixel setting of the camera in the software at the time of capturing the image.

The adjustment and/or calibration are usually stable for long time. Furthermore, they are not operator

dependent as long as no changes are applied to the tube, an eventual intermediate magnification

changer, the camera adapter, or the camera itself and as long as the same resolution of the camera

(number of pixels in x and y direction) is used for adjustment and/or calibration and for measurement.

Normally it is sufficient to record in regular time intervals images from the stage micrometer and

measure known distances; when the deviation between the measured length and the certified length is

less than a reasonably defined uncertainty limit for length measurements, which the laboratory wants

to achieve, e.g. 1 %, the calibration is still vali
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