FprEN ISO 1463

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

Metall- und Oxidschichten - Schichtdickenmessung - Mikroskopisches Verfahren (ISO/FDIS 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 dieses Dokumentes kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Ausrüstungen mit sich bringen. Dieses Dokument erhebt nicht den Anspruch, auf alle Sicherheits-probleme hinzuweisen, die mit ihrer Anwendung verbunden sind. Es liegt in der Verantwortung des Anwenders dieses Dokumentes, vor ihrer Anwendung geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz des Personals zu ergreifen.

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

Kovinske in oksidne prevleke - Merjenje debeline prevleke - Mikroskopska metoda (ISO/DIS 1463:2020)

Standards Content (sample)

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.

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oSIST prEN ISO 1463:2020
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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
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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

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ii © ISO 2020 – All rights reserved
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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
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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
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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.
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oSIST prEN ISO 1463:2020
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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.
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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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