SIST-TS CEN/TS 1071-10:2005
(Main)Advanced technical ceramics - Methods of test for ceramic coatings - Part 10: Determination of coating thickness by cross sectioning
Advanced technical ceramics - Methods of test for ceramic coatings - Part 10: Determination of coating thickness by cross sectioning
This document specifies a method of measuring the thickness of ceramic coatings by means of examination of a metallographically prepared cross-section of the coating in a calibrated optical or scanning electron microscope. It draws strongly on EN ISO 9220 [8], modifying and updating as required to be relevant to ceramic coatings and current best practice.
Hochleistungskeramik - Verfahren zur Prüfung keramischer Schichten - Teil 10: Bestimmung der Schichtdicke mittels Querschliff
Céramiques techniques avancées - Méthodes d'essai pour les revetements céramiques - Partie 10: Détermination de l'épaisseur du revetement par découpage transverse
Sodobna tehnična keramika – Metode za preskušanje keramičnih prevlek – 10. del: Ugotavljanje debeline prevleke s prečnim prerezom
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 1071-10:2005
01-januar-2005
6RGREQDWHKQLþQDNHUDPLND±0HWRGH]DSUHVNXãDQMHNHUDPLþQLKSUHYOHN±GHO
8JRWDYOMDQMHGHEHOLQHSUHYOHNHVSUHþQLPSUHUH]RP
Advanced technical ceramics - Methods of test for ceramic coatings - Part 10:
Determination of coating thickness by cross sectioning
Hochleistungskeramik - Verfahren zur Prüfung keramischer Schichten - Teil 10:
Bestimmung der Schichtdicke mittels Querschliff
Céramiques techniques avancées - Méthodes d'essai pour les revetements céramiques -
Partie 10: Détermination de l'épaisseur du revetement par découpage transverse
Ta slovenski standard je istoveten z: CEN/TS 1071-10:2004
ICS:
25.220.99 Druge obdelave in prevleke Other treatments and
coatings
81.060.30 Sodobna keramika Advanced ceramics
SIST-TS CEN/TS 1071-10:2005 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST-TS CEN/TS 1071-10:2005
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 1071-10:2005
TECHNICAL SPECIFICATION
CEN/TS 1071-10
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
July 2004
ICS 17.040.20; 25.220.99; 81.060.30
English version
Advanced technical ceramics - Methods of test for ceramic
coatings - Part 10: Determination of coating thickness by cross
sectioning
Céramiques techniques avancées - Méthodes d'essai pour Hochleistungskeramik - Verfahren zur Prüfung keramischer
les revêtements céramiques - Partie 10: Détermination de Schichten - Teil 10: Bestimmung der Schichtdicke mittels
l'épaisseur du revêtement par découpage transverse Querschliff
This Technical Specification (CEN/TS) was approved by CEN on 2 March 2004 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 1071-10:2004: E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 1071-10:2005
CEN/TS 1071-10:2004 (E)
Contents Page
Foreword. 4
Introduction . 5
1 Scope. 6
2 Normative references . 6
3 Terms and definitions. 6
4 Principle . 6
5 Apparatus . 6
5.1 Scanning electron microscope (SEM) . 6
5.2 Optical microscope. 6
6 Sample preparation. 7
6.1 Cross-section preparation . 7
6.2 Surface roughness. 7
6.3 Taper of cross-section. 7
6.4 Specimen tilt. 7
6.5 Coating damage . 7
6.6 Rounding of edges of the coating. 7
6.7 Overplating . 8
6.8 Etching . 8
6.9 Smearing. 8
7 Calibration of instruments . 8
7.1 Procedure . 8
7.2 Photography . 8
7.3 Measurement . 8
7.4 Calculation of magnification. 8
7.5 Poor contrast. 9
7.6 Magnification. 9
7.7 Uniformity of magnification . 9
7.8 Stability of magnification . 9
8 Test procedure . 9
8.1 General. 9
8.2 Preparation of images . 10
8.2.1 General. 10
8.2.2 Conventional photographic micrograph . 10
8.2.3 Digital images. 10
8.3 Measurement . 10
8.4 Thickness calculation. 10
8.5 Correction procedures . 11
9 Measurement uncertainty . 11
10 Expression of results. 11
11 Reporting of results. 11
Annex A (informative) General guidance on the preparation and measurement of cross-
sections. 13
A.1 Introduction . 13
A.2 Cutting. 13
A.3 Mounting . 13
2
---------------------- Page: 4 ----------------------
SIST-TS CEN/TS 1071-10:2005
CEN/TS 1071-10:2004 (E)
A.4 Grinding and polishing. 14
A.5 Use of the scanning electron microscope. 14
Bibliography . 15
3
---------------------- Page: 5 ----------------------
SIST-TS CEN/TS 1071-10:2005
CEN/TS 1071-10:2004 (E)
Foreword
This document CEN/TS 1071-10:2004 has been prepared by Technical Committee CEN/TC 184
“Advanced technical ceramics”, the secretariat of which is held by BSI.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to announce this Technical Specification: Austria, Belgium, Cyprus,
Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and the United Kingdom.
EN 1071 Advanced technical ceramics — Methods of test for ceramic coatings consists of 11 parts:
Part 1: Determination of coating thickness by contact probe profilometer
Part 2: Determination of coating thickness by the crater grinding method
Part 3: Determination of adhesion and other mechanical failure modes by a scratch test
Part 4: Determination of chemical composition
Part 5: Determination of porosity
Part 6: Determination of the abrasion resistance of coatings by a micro-abrasion wear test
Part 7: Determination of hardness and Young's modulus by instrumented indentation testing
1)
Part 8: Rockwell indentation test for evaluation of adhesion
Part 9: Determination of fracture strain
Part 10: Determination of coating thickness by cross sectioning
1)
Part 11: Measurement of internal stress with the Stoney formula
Parts 7 to 11 are Technical Specifications.
This document includes a bibliography.
1) In preparation at the time of publication of this document.
4
---------------------- Page: 6 ----------------------
SIST-TS CEN/TS 1071-10:2005
CEN/TS 1071-10:2004 (E)
Introduction
The thickness of a coating is an important property that controls its functional behaviour. Thickness
determinations are also used as part of quality control in the production of coatings. It is normal to
specify a thickness when defining a coating, so that valid methods of measurement are required. The
method described here is direct, but is destructive, requiring preparation of a metallographic cross-
section. A number of other standard non-destructive methods exist and some of these are listed in the
Bibliography (references [1] to [7]).
5
---------------------- Page: 7 ----------------------
SIST-TS CEN/TS 1071-10:2005
CEN/TS 1071-10:2004 (E)
1 Scope
This document specifies a method of measuring the thickness of ceramic coatings by means of
examination of a metallographically prepared cross-section of the coating in a calibrated optical or
scanning electron microscope. It draws strongly on EN ISO 9220 [8], modifying and updating as
required to be relevant to ceramic coatings and current best practice.
2 Normative references
The following referenced document is indispensable for the application 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.
ENV 13005, Guide to the expression of uncertainty in measurement
3 Terms and definitions
For the purposes of this document, the following term and definition apply.
3.1
local thickness
mean of the thickness measurements, of which a specified number is made within a reference area
[5]
[EN ISO 2064:2000, 3.4]
4 Principle
This test procedure covers the measurement of coating thickness by examination of a cross-section in
an optical or scanning electron microscope. Preparation of the cross-section requires care to ensure
that the total thickness is revealed and that when viewed it is normal to the axis of the microscope.
After proper calibration of the microscope, it is a simple matter to determine the coating thickness
from knowledge of the magnification used. This can be done directly using a modern measuring
microscope, or indirectly from photographic images obtained from an optical or scanning electron
microscope.
5 Apparatus
5.1 Scanning electron microscope (SEM)
The SEM shall have a spatial resolution of 50 nm or better. Suitable instruments are available
commercially.
5.2 Optical microscope
The optical microscope shall have a spatial resolution of 500 nm or better. Suitable instruments are
available commercially.
NOTE 1 Microscopes that incorporate a system to automatically record the XY coordinates are available and
if the stage movement has been calibrated, can be used directly to measure coating thickness without the need
to take photographs. This method is particularly useful where coating thickness variations around a component
are likely.
6
---------------------- Page: 8 ----------------------
SIST-TS CEN/TS 1071-10:2005
CEN/TS 1071-10:2004 (E)
NOTE 2 The choice of instrument will depend on the thickness of the coating to be measured and the
accuracy required.
6 Sample preparation
6.1 Cross-section preparation
Prepare the cross-section so that:
a) it is perpendicular to the plane of the coating;
b) the surface is flat and the entire width of the coating image is simultaneously in focus at the
magnification to be used for measurement;
c) all material damaged by cutting or cross-sectioning is removed;
d) the boundaries of the coating cross-section are sharply defined by no more than contrasting
appearance, or by a narrow well defined line.
NOTE Further guidance is given in Annex A.
6.2 Surface roughness
If the coating or its substrate is rough relative to the coating thickness, one or both of the interfaces
bounding the coating may be too irregular to permit accurate measurement of the average thickness
in the field of view.
6.3 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. For example, an inclination of 10 degrees to the
perpendicular will contribute an error of 1,5 %.
NOTE It is recommended that a cross-section of a reference sample of known thickness be prepared using
the same procedures as the test sample as a check on the accuracy of cutting, mounting and polishing
procedures.
6.4 Specimen tilt
Any tilt of the specimen (plane of cross-section) with respect to the electron beam or optical axis will
result in an inaccurate measurement. This error is compounded if the test specimen tilt is different
from that used during calibration.
6.5 Coating damage
Ceramic coatings are generally brittle, and hence easily damaged during preparation of the
metallographic cross-section.
6.6 Rounding of edges of the 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 observed thickness may differ from the true thickness. Edge rounding can be
caused by improper mounting, grinding, polishing or etching (see 6.8 and Annex A).
7
---------------------- Page: 9 ----------------------
SIST-TS CEN/TS 1071-10:2005
CEN/TS 1071-10:2004 (E)
6.7 Overplating
Overplating of the test specimen serves to protect the coating during preparation of the cross-section
and thus to prevent an inaccurate measurement. Removal of coating material is however possible
during plating and care should be exercised in the choice of plating procedure.
6.8 Etching
Optimum etching will produce a clearly defined and narrow line at the interface between the coating
and substrate. A wide or poorly defined line can result in an inaccurate measurement.
NOTE Many etchants are developed for optical microscopy and do not necessarily enhance contrast in a
SEM.
6.
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.