Advanced technical ceramics - Methods of test for ceramic coatings - Part 6: Determination of the abrasion resistance of coatings by a micro-abrasion wear test

This part of EN 1071 specifies a method for measuring the abrasive wear rate of ceramic coatings by means of a micro-scale abrasion wear test, based on the well known crater grinding technique used for film thickness determination (see EN 1071-2).
This method can provide data on both film and substrate wear rates, either by performing two separate tests or by careful analysis of data from a single test series.
The test method can be applied to samples with planar or non-planar surfaces but the analysis described in clause 9 applies only to flat samples. For non-planar samples, a more complicated analysis, possibly requiring the use of numerical methods, is required.

Hochleistungskeramik - Verfahren zur Prüfung keramischer Schichten - Teil 6: Bestimmung der Beständigkeit gegen Abriebverschleiß von Schichten mittels Mikroabriebprüfung

Dieser Teil von EN 1071 legt ein Verfahren zur Messung der Abriebverschleißrate keramischer Schichten durch eine Mikroabriebprüfung fest, die auf dem von der Bestimmung der Schichtdicke bekannten Kalottenschleifverfahren basiert (siehe EN 1071 2).
Nach diesem Verfahren können Daten zur Bestimmung der Abriebverschleißraten sowohl der Schicht als auch des Grundwerkstoffs ermittelt werden, indem entweder eine Prüfung für die Schicht und eine Prüfung für den Grundwerkstoff oder aber eine Analyse durchgeführt wird, bei der eine sorgfältige Auswertung der aus nur einer einzigen Prüfserie gewonnenen Daten erfolgt.
Das Prüfverfahren kann auf Proben mit ebenen oder nicht ebenen Flächen angewendet werden, während die im Abschnitt 9 beschriebene Analyse nur auf flache Proben anwendbar ist. Für nicht ebene Proben ist eine komplexere Analyse erforderlich, möglicherweise unter Anwendung numerischer Verfahren.

Céramiques techniques avancées - Méthodes d'essai pour revêtements céramiques - Partie 6 : Détermination de la résistance à l'abrasion des revêtements par essai de micro-usure

Sodobna tehnična keramika - Metode za preskušanje keramičnih prevlek - 6. del: Ugotavljanje odpornosti prevlek proti obrabi z mikroabrazivnim preskusom

General Information

Status
Withdrawn
Publication Date
20-Nov-2008
Withdrawal Date
12-May-2016
Technical Committee
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
12-May-2016
Due Date
04-Jun-2016
Completion Date
13-May-2016

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.HVNXVRPHochleistungskeramik - Verfahren zur Prüfung keramischer Schichten - Teil 6: Bestimmung der Beständigkeit gegen Abriebverschleiß von Schichten mittels MikroabriebprüfungCéramiques techniques avancées - Méthodes d'essai pour revêtements céramiques - Partie 6 : Détermination de la résistance à l'abrasion des revêtements par essai de micro-usureAdvanced technical ceramics - Methods of test for ceramic coatings - Part 6: Determination of the abrasion resistance of coatings by a micro-abrasion wear test81.060.30Sodobna keramikaAdvanced ceramics25.220.99Druge obdelave in prevlekeOther treatments and coatingsICS:Ta slovenski standard je istoveten z:EN 1071-6:2007SIST EN 1071-6:2009en,fr,de01-januar-2009SIST EN 1071-6:2009SLOVENSKI
STANDARDSIST ENV 1071-6:20071DGRPHãþD



SIST EN 1071-6:2009



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 1071-6November 2007ICS 81.060.30; 25.220.99; 17.040.20Supersedes ENV 1071-6:2002
English VersionAdvanced technical ceramics - Methods of test for ceramiccoatings - Part 6: Determination of the abrasion resistance ofcoatings by a micro-abrasion wear testCéramiques techniques avancées - Méthodes d'essai pourrevêtements céramiques - Partie 6 : Détermination de larésistance à l'abrasion des revêtements par essai de micro-usureHochleistungskeramik - Verfahren zur Prüfung keramischerSchichten - Teil 6: Bestimmung der Beständigkeit gegenAbriebverschleiß von Schichten mittels MikroabriebprüfungThis European Standard was approved by CEN on 30 September 2007.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: rue de Stassart, 36
B-1050 Brussels© 2007 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 1071-6:2007: ESIST EN 1071-6:2009



EN 1071-6:2007 (E) 2 Contents Page Foreword.3 1 Scope.4 2 Normative references.4 3 Terms and definitions.4 4 Significance and use.4 5 Principle.5 6 Apparatus and materials.5 6.1 Test system.5 6.2 Test balls.7 6.3 Test slurry.7 6.4 Measurement of crater dimensions.8 7 Preparation of test pieces.8 8 Test procedure.9 8.1 Different types of test.9 8.2 Test Type A: No perforation of coating.9 8.3 Test Type B: Perforation of coating.11 9 Analysis of results.13 9.1 Test Type A: no perforation of coating.13 9.2 Test Type B: perforation of coating.13 10 Test reproducibility, repeatability and limits.15 10.1 Reproducibility and repeatability.15 10.2 Limits.16 11 Test report.18 Annex A (normative)
Measurement of coating thickness.19 Bibliography.20
SIST EN 1071-6:2009



EN 1071-6:2007 (E) 3 Foreword This document (EN 1071-6:2007) 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 May 2008, and conflicting national standards shall be withdrawn at the latest by May 2008. 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 ENV 1071-6:2002. EN 1071 'Advanced technical ceramics - Methods of test for ceramic coatings' was prepared in 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 by electron probe microanalysis (EPMA) 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 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 5, a European pre-standard, was withdrawn in 2007. Part 7, a Technical Specification, was withdrawn in 2007, following publication of EN ISO 14577-4. At the time of publication of this document, Parts 8 to 11 were Technical Specifications. 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 1071-6:2009



EN 1071-6:2007 (E) 4 1 Scope This part of EN 1071 specifies a method for measuring the abrasive wear rate of ceramic coatings by means of a micro-scale abrasion wear test, based on the well known crater grinding technique used for film thickness determination (see EN 1071-2). This method can provide data on both film and substrate wear rates, either by performing two separate tests or by careful analysis of data from a single test series. The test method can be applied to samples with planar or non-planar surfaces but the analysis described in clause 9 applies only to flat samples. For non-planar samples, a more complicated analysis, possibly requiring the use of numerical methods, is required. 2 Normative references The following referenced documents are 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.
EN ISO 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) ISO 3290, Rolling bearings — Balls — Dimensions and tolerances 3 Terms and definitions For the purposes of this European Standard, the following term and definition applies. 3.1 abrasive wear rate, K abrasive wear coefficient volume of material removed in unit sliding distance under a normal contact load of 1 N 4 Significance and use Although few protective coatings are subject to single wear processes, the abrasive wear resistance of such coatings can play a decisive role in their performance. Hence knowledge of the abrasive wear resistance of ceramic coatings can help in the proper selection of coatings for applications where abrasion plays a major role in their degradation. Although techniques exist to measure the abrasive wear behaviour of bulk materials and thick films (see [1 – 3]), these techniques are not easily applied to thin films and are difficult to interpret when used on curved surfaces.
The purpose of this European Standard is to provide a method for measuring the abrasion resistance of both thin and thick coatings and of bulk materials. The test can be performed on flat surfaces or surfaces with a known radius of curvature, and requires only a few mm2 of sample. However, the analysis described in clause 9 applies only to flat samples, and is applicable to homogeneous single layer coatings only; errors may occur if the test is used on in-homogeneous coatings. [4] and [5] give details of analytical treatments for determining the wear rate for coatings on curved surfaces.
By proper treatment of the results, as indicated in 9.2, where the test produces penetration of the coating it can provide abrasive wear coefficients for both the coating and substrate from a single test series.
SIST EN 1071-6:2009



EN 1071-6:2007 (E) 5 Although the test is designed to enable quantitative measurement of abrasive wear coefficients, it can be adapted as a quality control test for use on real components. 5 Principle In the test, a ball is rotated while being pressed against the sample and an abrasive slurry is fed into the contact zone. A spherical depression is produced and the size of this depression is measured. Where perforation of the coating has not occurred, the wear rate of the coating can be obtained from a single crater. When perforation of the coating occurs, by making a series of such craters and measuring their dimensions, the wear rate of both the coating and the substrate can be calculated. 6 Apparatus and materials 6.1 Test system A ball that can be rotated and pressed against the coated sample shall be used. Two variants of the ball system are shown in Figure 1, where either the sample, mounted on a dead-weight loaded lever, is pressed against a directly driven ball, or the ball’s own weight presses it against the sample. NOTE The results obtained with free-ball systems [6] (see Figure 1a) - can vary depending on the precise system geometry. In particular, it has been found that the tilt angle of the sample holder and the width of the groove in the drive shaft that supports the ball can have an important influence on the results. A tilt angle of 60 ° to 75 º and a shaft groove width of 10 mm have been found to result in the smallest variability under typical conditions [6]. The test system shall be constructed so that the rotational speed of the ball remains constant throughout any test and is reproducible to better than +/-10 % of the nominal value between tests. The drive shaft shall have a total run-out of less than 20 µm at its points of contact with the ball.
SIST EN 1071-6:2009



EN 1071-6:2007 (E) 6
(a)(b)1245343125 Key for a) 1
ball 2
sample 3
drive shaft 4
sample support 5
load cell Key for b) 1
ball 2
sample 3
weight 4
pivot point 5
lever
Figure 1 — Two different types of a ball cratering system: a) free-ball, b) fixed-ball
SIST EN 1071-6:2009



EN 1071-6:2007 (E) 7 6.2 Test balls The balls used are typically 25 mm diameter hardened steel, e.g. UNS G52986 (SAE52100, [7]) and shall, prior to any conditioning, conform to the requirements of ISO 3290. NOTE 1 Balls can be used in a polished condition but it has been found [8] that the test behaviour is erratic and poor results are obtained if balls are used without conditioning.
The recommended conditioning treatment consists of running the new test ball for at least 300 revolutions on a non-critical part of the sample, or other suitable surface, under normal test conditions and repeating this for at least 5 different orientations of the ball before starting the test programme. NOTE 2 A flat, ground steel coupon with a hardness of between 200 and 800 HV 30 has been found to be suitable for conditioning the ball. NOTE 3 Following conditioning, balls have been found to be usable for around 50 individual craters, depending on the precise conditions used.
The performance of balls shall be subject to regular performance checks to ensure that they continue to produce acceptable craters. Balls shall be replaced if such a check indicates any abnormal cratering behaviour. NOTE 4 Performance checks can be made using any representative test piece, such as hardened and tempered high speed steel, or a well characterized titanium nitride or other coating deposited on a stable substrate material. 6.3 Test slurry In all cases, a slurry of silicon carbide (SiC) or other suitable abrasive in a suitable liquid, normally water, shall be used. Other liquids may be used where their use is suggested by matching conditions to a particular application. In this respect the wetting properties and viscosity of the fluid are important parameters to consider. NOTE 1 The abrasive is normally F1200 SiC, but F1200 alumina or other fine abrasive can be used. The average size of the abrasive should not exceed 5µm.
The use of different abrasive media will produce different wear rates, and only results produced from craters under identical conditions should be compared. A homogeneous slurry shall be used throughout the test. This can be done by stirring the slurry continuously, or by adding stabilizers. NOTE 2 If testing is to be on coatings deposited onto steel substrates that are susceptible to corrosion, it is recommended that sodium nitrite (NaNO2) should be added to the slurry at the rate of 1 g for each
100 cm3 of water to prevent corrosion of craters before they can be measured. An abrasive slurry shall be made from the abrasive powder and the chosen liquid in the required proportions. As the mode of wear that is observed can depend critically on the concentration of the abrasive slurry, two concentrations are recommended. These are: 1) Dilute (promotes grooving wear) Concentration of 2 % v/v. For SiC, for example, with a density of 3,2 gcm-3, this is achieved by mixing 6,4 g of SiC to 98 ml of distilled or de-ionized water. SIST EN 1071-6:2009



EN 1071-6:2007 (E) 8 2) Concentrated (promotes rolling wear) Concentration of 20 % v/v. For SiC, for example, with a density of 3,2 gcm-3, this is achieved by mixing 80 g of SiC in 100 cm-3 of distilled or de-ionized water.
NOTE 3 The type of wear promoted depends both on the concentration of the slurry and the type of abrasive as well as on the material being tested. For example, it has been found that micro-grain (submicron) rutile can promote rolling wear even at concentrations as low as 3 % by volume. As an alternative to mixing slurries, ready mixed abrasive slurries can be used. If this is done all details of the supplier and makeup of the slurry shall be reported. NOTE 4 Preliminary testing should be undertaken to ensure that the slurry concentration chosen produces the wear mode(s) of interest during the test.
6.4 Measurement of crater dimensions Crater dimensions may be measured with any suitable equipment, e.g. a microscope with calibrated graticule, provided that the calibration used is traceable to national standards. Where measurements are made from photographically capture images, it is essential that fiducial (reference) marks of known dimensions are incorporated in the images to ensure that any shrinkage of the photographic film after development or during storage can be eliminated. Alternatively, automatic measurement using an electronically captured image may be used provided that the measurement system is fully calibrated, the procedure used being traceable to national standards. NOTE 1 In some cases, e.g. rolling wear with relatively large abrasive particles, it may be difficult to identify the edge of craters, particularly at the outer surface of the coating. In such cases the use of profilometry, a change in illumination angle, or substrate etching (for craters that penetrate the coating) can help.
NOTE 2 Profilometry may lead to different results than optical microscopy evaluation of crater size, due to rounded crater edges. Results of tests evaluated by different measurement methods should not be compared to each other. 7 Preparation of test pieces 7.1 Coated samples shall have a flat area large enough to perform the necessary series of experiments. In all cases the coating thickness shall be larger than 1 µm. NOTE Samples with non-flat surfaces can also be tested but the analysis required determining the wear rate of coating and substrate will be different to that given in this standard – see [4] and [5].
7.2 The accuracy with which crater diameters can be measured depends on the surface finish of the sample and the type of abrasive used. Although it is possible to improve the surface finish of the coating by polishing prior to testing, this is not the case with the substrate, and the surface finish of the substrate affects the accuracy with which the interface between coating and substrate can be located. Therefore, wherever possible, coatings should be deposited onto polished substrates to allow accurate location of the base of the coating. Where necessary, the surface of the coating may be polished to improve the surface finish.
NOTE To avoid damaging the surface of the coating or affecting its wear rate, it is recommended that any polishing should be done with the smallest diamond abrasive and lowest pressure commensurate with achieving the surface finish required. Polishing should therefore commence with, for example, 1µm diamond abrasive and this should only be increased if the required finish cannot be achieved.
SIST EN 1071-6:2009



EN 1071-6:
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