SIST EN 1071-10:2009
(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
Dieses Dokument legt ein Messverfahren für die Schichtdicke keramischer Beschichtungen fest, bei dem ein
metallographisch angefertigter Querschliff der Beschichtigung mit einem kalibrierten Licht- oder
Rasterelektronenmikroskop untersucht wird. Es lehnt sich eng an EN ISO 9220 [8] an, jedoch wurden alle
erforderlichen Anpassungen und Aktualisierungen vorgenommen, um keramischen Beschichtungen und der
derzeitig besten Praxis zu entsprechen.
Céramiques techniques avancées - Méthodes d'essai pour les revêtements céramiques - Partie 10: Détermination de l'épaisseur du revêtement par découpage transverse
Le présent document définit une méthode de mesurage de l’épaisseur des revêtements céramiques qui
comprend l’examen par microscope optique ou électronique à balayage étalonné d’une section transversale
du revêtement préparée métallographiquement. Il est largement inspiré du document EN ISO 9220 [8], mais a
été modifié et mis à jour conformément aux exigences pour pouvoir être appliqué aux revêtements
céramiques et aux bonnes pratiques actuelles.
Sodobna tehnična keramika - Metode za preskušanje keramičnih prevlek - 10. del: Ugotavljanje debeline prevleke s prečnim prerezom
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Hochleistungskeramik - Verfahren zur Prüfung keramischer Schichten - Teil 10: Bestimmung der Schichtdicke mittels QuerschliffCéramiques techniques avancées - Méthodes d'essai pour les revêtements céramiques - Partie 10: Détermination de l'épaisseur du revêtement par découpage transverseAdvanced technical ceramics - Methods of test for ceramic coatings - Part 10: Determination of coating thickness by cross sectioning81.060.30Sodobna keramikaAdvanced ceramics25.220.99Druge obdelave in prevlekeOther treatments and coatingsICS:Ta slovenski standard je istoveten z:EN 1071-10:2009SIST EN 1071-10:2009en,fr,de01-november-2009SIST EN 1071-10:2009SLOVENSKI
STANDARDSIST-TS CEN/TS 1071-10:20051DGRPHãþD
SIST EN 1071-10:2009
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 1071-10July 2009ICS 81.060.30Supersedes CEN/TS 1071-10:2004
English VersionAdvanced technical ceramics - Methods of test for ceramiccoatings - Part 10: Determination of coating thickness by crosssectioningCéramiques techniques avancées - Méthodes d'essai pourles revêtements céramiques - Partie 10: Détermination del'épaisseur du revêtement par découpage transverseHochleistungskeramik - Verfahren zur Prüfung keramischerSchichten - Teil 10: Bestimmung der Schichtdicke mittelsQuerschliffThis European Standard was approved by CEN on 19 June 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre:
Avenue Marnix 17,
B-1000 Brussels© 2009 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 1071-10:2009: ESIST EN 1071-10:2009
EN 1071-10:2009 (E) 2 Contents Page Foreword . 3 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 8.3 Measurement . 10 8.4 Thickness calculation . 10 8.5 Correction procedures . 11 9 Measurement uncertainty . 11 10 Expression of results. 11 11 Report . 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 A.4 Grinding and polishing . 14 A.5 Use of the scanning electron microscope. 14 Bibliography . 15 SIST EN 1071-10:2009
EN 1071-10:2009 (E) 3 Foreword This document (EN 1071-10:2009) has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics”, 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 January 2010, and conflicting national standards shall be withdrawn at the latest by January 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document supersedes CEN/TS 1071-10:2004. EN 1071 Advanced technical ceramics — Methods of test for ceramic coatings consists of the following 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 by electron probe microanalysis (EPMA) Part 5: Determination of porosity [withdrawn] 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 [withdrawn] Part 8: Rockwell indentation test for evaluation of adhesion Part 9: Determination of fracture strain Part 10: Determination of coating thickness by cross sectioning Part 11: Determination of internal stress by the Stoney formula Part 12: Reciprocating wear test 1) Part 13: Determination of wear rate by the pin-on-disk method 1) Parts 7, 8 and 11 are Technical Specifications. Part 7 was withdrawn shortly after publication of EN ISO 14577-4:2007.
1) In preparation at the time of publication of this European Standard. SIST EN 1071-10:2009
EN 1071-10:2009 (E) 4 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 1071-10:2009
EN 1071-10:2009 (E) 5 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]). SIST EN 1071-10:2009
EN 1071-10:2009 (E) 6 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 EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 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 [EN ISO 2064:2000] [5] 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 SIST EN 1071-10:2009
EN 1071-10:2009 (E) 7 to take photographs. This method is particularly useful where coating thickness variations around a component are likely. 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). SIST EN 1071-10:2009
EN 1071-10:2009 (E) 8 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 no
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Hochleistungskeramik - Verfahren zur Prüfung keramischer Schichten - Teil 10: Bestimmung der Schichtdicke mittels QuerschliffCéramiques techniques avancées - Méthodes d'essai pour les revêtements céramiques - Partie 10: Détermination de l'épaisseur du revêtement par découpage transverseAdvanced technical ceramics - Methods of test for ceramic coatings - Part 10: Determination of coating thickness by cross sectioning81.060.30Sodobna keramikaAdvanced ceramicsICS:Ta slovenski standard je istoveten z:prEN 1071-10kSIST prEN 1071-10:2009en,fr,de01-marec-2009kSIST prEN 1071-10:2009SLOVENSKI
STANDARD
kSIST prEN 1071-10:2009
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMFINAL DRAFTprEN 1071-10December 2008ICS 81.060.30Will supersede CEN/TS 1071-10:2004
English VersionAdvanced technical ceramics - Methods of test for ceramiccoatings - Part 10: Determination of coating thickness by crosssectioningCéramiques techniques avancées - Méthodes d'essai pourles revêtements céramiques - Partie 10: Détermination del'épaisseur du revêtement par découpage transverseHochleistungskeramik - Verfahren zur Prüfung keramischerSchichten - Teil 10: Bestimmung der Schichtdicke mittelsQuerschliffThis draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the TechnicalCommittee CEN/TC 184.If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations whichstipulate the conditions for giving this European Standard the status of a national standard without any alteration.This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other languagemade by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has thesame status as the official versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice andshall not be referred to as a European Standard.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre:
Avenue Marnix 17,
B-1000 Brussels© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. prEN 1071-10:2008: EkSIST prEN 1071-10:2009
prEN 1071-10:2008 (E) 2 Contents Page Foreword.3 Introduction.4 1 Scope.5 2 Normative references.5 3 Terms and definitions.5 4 Principle.5 5 Apparatus.5 5.1 Scanning electron microscope (SEM).5 5.2 Optical microscope.5 6 Sample preparation.6 6.1 Cross-section preparation.6 6.2 Surface roughness.6 6.3 Taper of cross-section.6 6.4 Specimen tilt.6 6.5 Coating damage.6 6.6 Rounding of edges of the coating.6 6.7 Overplating.7 6.8 Etching.7 6.9 Smearing.7 7 Calibration of instruments.7 7.1 Procedure.7 7.2 Photography.7 7.3 Measurement.7 7.4 Calculation of magnification.7 7.5 Poor contrast.8 7.6 Magnification.8 7.7 Uniformity of magnification.8 7.8 Stability of magnification.8 8 Test procedure.8 8.1 General.8 8.2 Preparation of images.9 8.3 Measurement.9 8.4 Thickness calculation.9 8.5 Correction procedures.10 9 Measurement uncertainty.10 10 Expression of results.10 11 Report.10 Annex A (informative)
General guidance on the preparation and measurement of cross-sections.12 A.1 Introduction.12 A.2 Cutting.12 A.3 Mounting.12 A.4 Grinding and polishing.13 A.5 Use of the scanning electron microscope.13 Bibliography.14 kSIST prEN 1071-10:2009
prEN 1071-10:2008 (E) 3 Foreword This document (prEN 1071-10:2008) has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics”, the secretariat of which is held by BSI. This document is currently submitted to the Unique Acceptance Procedure. This document will supersede CEN/TS 1071-10:2004. EN 1071 Advanced technical ceramics — Methods of test for ceramic coatings consists of the following parts: Part 1: Determination of coating thickness by contact probe filometer 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 by electron probe microanalysis (EPMA) Part 5: Determination of porosity [withdrawn] 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 [withdrawn] Part 8: Rockwell indentation test for evaluation of adhesion Part 9: Determination of fracture strain Part 10: Determination of coating thickness by cross sectioning Part 11: Determination of internal stress by the Stoney formula Part 12: Reciprocating wear test 1) Part 13: Determination of wear rate by the pin-on-disk method 1) Parts 7, 8 and 11 are Technical Specifications. Part 7 was withdrawn shortly after publication of EN ISO 14577-4:2007. This part of EN 1071 includes a bibliography.
1) In preparation at the time of publication of this European Standard. kSIST prEN 1071-10:2009
prEN 1071-10:2008 (E) 4 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]). kSIST prEN 1071-10:2009
prEN 1071-10:2008 (E) 5 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 EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 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 [EN ISO 2064:2000] [5] 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 kSIST prEN 1071-10:2009
prEN 1071-10:2008 (E) 6 to take photographs. This method is particularly useful where coating thickness variations around a component are likely. 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). kSIST prEN 1071-10:2009
prEN 1071-10:2008 (E) 7 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. 6.9 Smearing Polishing may leave smeared metal that obscures the true boundary between the coating and the substrate, and/or the overplate and thus results in an inaccurate measurement. To help identify whether or not smearing occurs, repeat the polishing, etching and measurement several times. Any significant variation in readings is an indication of possible smearing. 7 Cal
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