EN 1071-3-2005 en Advanced technical ceramics - Methods of test for ceramic coatings - Part 3 Determination of adhesion and other mechanical failure modes by a scratch test《先进技术陶瓷 .pdf

1、BRITISH STANDARDBS EN 1071-3:2005Advanced technical ceramics Methods of test for ceramic coatings Part 3: Determination of adhesion and other mechanical failure modes by a scratch testThe European Standard EN 1071-3:2005 has the status of a British StandardICS 81.060.30g49g50g3g38g50g51g60g44g49g42g

2、3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 1071-3:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 4 Janua

3、ry 2006 BSI 4 January 2006ISBN 0 580 47358 9National forewordThis British Standard is the official English language version of EN 1071-3:2005. It supersedes DD ENV 1071-3:1994 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical c

4、eramics, which has the responsibility to:A list of organizations represented on this committee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogueunder

5、the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct applica

6、tion.Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor r

7、elated international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 47 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued

8、.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 1071-3August 2005ICS 81.060.30 Supersedes ENV 1071-3:1994English VersionAdvanced technical ceramics - Methods of test for ceramiccoatings - Part 3: Determination of adhesion and othermechanica

9、l failure modes by a scratch testCramiques techniques avances - Mthodes dessai pourrevtements cramiques - Partie 3 : Dtermination deladhrence et autres modes de dfaillance mcanique paressai de rayureHochleistungskeramik - Verfahren zur Prfung keramischerSchichten - Teil 3: Bestimmung der Haftung und

10、 Formendes mechanischen Versagens mit dem RitztestThis European Standard was approved by CEN on 27 June 2005.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 alterat

11、ion. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translatio

12、nunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, I

13、celand, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart,

14、36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 1071-3:2005: EEN 1071-3:2005 (E) 2Contents pageForeword 3Introduction . 41 Scope. 52 Normative references. 53 Principle 54 Apparatus and materials 74.1 Scratch t

15、ester 74.2 Diamond stylus. 75 Preparation of the test piece 95.1 General requirements. 95.2 Surface roughness, waviness and levelling. 95.3 Specimen cleaning . 95.4 Coating-substrate specific parameters. 96 Test procedure 106.1 General 106.2 Equipment preparation 106.3 Environmental conditions 106.4

16、 Scratching procedure. 116.5 Scratch evaluation and critical load determination . 116.6 Microscope observation 126.7 Acoustic emission (AE) and frictional force (FF) recording 127 Repeatability and limits 158 Test report. 15Annex A (normative) Procedure for calibration of a scratch testing system 17

17、A.1 Introduction. 17A.2 Scope. 17A.3 Principle 17A.4 Apparatus 17A.5 Calibration procedures 18A.6 Recording results . 24Annex B (informative) Typical failure modes obtained in scratch testing. 25B.1 Introduction. 25B.2 Experimental. 25B.3 Results 25B.4 Conclusions 25B.5 The scratch test atlas of fai

18、lure modes. 26Bibliography 47EN 1071-3:2005 (E) 3Foreword This European Standard (EN 1071-3:2005) 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, eithe

19、r by publication of an identical text or by endorsement, at the latest by February 2006, and conflicting national standards shall be withdrawn at the latest by February 2006. This European Standard supersedes ENV 1071-3:1994. EN 1071 Advanced technical ceramics Methods of test for ceramic coatings h

20、as eleven 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 e

21、lectron 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 Youngs modulus by instrumented indentation testing Part 8: Rockwell indentation test for evaluation of

22、 adhesion Part 9: Determination of fracture strain Part 10: Determination of coating thickness by cross sectioning Part 11: Measurement of internal stress with the Stoney formula Parts 7 to 11 are Technical Specifications. According to the CEN/CENELEC Internal Regulations, the national standards org

23、anizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,

24、Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 1071-3:2005 (E) 4IntroductionThe test method in this Part of EN 1071 consists of drawing a loaded stylus across a coated surface. The load on the stylus is increased until failure of the coating/substrate system occurs. Alternatively repeti

25、tive scratching at a fixed load can be used to promote failure. The normal load on the stylus at which a particular failure mode initiates is recorded and is referred to as the critical load, Lc, for that mode of failure. Failure events are detected by the use of microscopic examination, acoustic em

26、ission and/or friction force measurement. Knowledge of the failure mode is essential to assess the mechanical behaviour of coated surfaces. Only some of the observed failure events in scratch testing are related to detachment at the coating-substrate interface and are thus relevant as a measure of a

27、dhesion. Other failures, such as cracks and cohesive damage within the coating or substrate may be equally important to determine the behaviour of a coated component in a particular application. EN 1071-3:2005 (E) 51 Scope This Part of EN 1071 describes a method of testing ceramic coatings by scratc

28、hing with a loaded diamond stylus so as to promote adhesive and/or cohesive failure of the coating-substrate system. The test is suitable for evaluating ceramic coatings up to a thickness of 20 m and can also be suitable for evaluating other coating types and thicknesses. The test is intended for us

29、e with specimens of limited surface roughness. This European Standard is intended for use in the macro (1 N 100 N) load range. The procedures can also be applicable to other load ranges. However, appropriate calibration is essential if the normal loads at which failure events occur are to be quantif

30、ied. 2 Normative references The following referenced documents are indispensable for the application of this European Standard. For dated references, only the edition cited applies. For undated references the latest edition of the referenced document (including any amendments) applies. EN ISO 4287,

31、Geometrical product specifications (GPS) - Surface texture: Profile method - Terms, definitions and surface texture parameters (ISO 4287:1997) EN ISO 6508-2, Metallic materials - Rockwell hardness test - Part 2: Verification and calibration of testing machines (scales A, B, C, D, E, F, G, H, K, N, T

32、) (ISO 6508-2:1999)EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:1999)3 Principle The scratch test is designed for the assessment of the mechanical integrity of coated surfaces. The test method consists of generating scratches with a

33、 stylus of defined shape (usually diamond with a Rockwell C geometry) by drawing it across the surface of the coating-substrate system to be tested, either under constant or progressive load (see Figure 1). Failure events are detected by direct microscopic observation of the scratch and sometimes by

34、 using acoustic emission and/or friction force measurement. The driving forces for the failure of the coating-substrate system in the scratch test are a combination of elastic-plastic indentation stresses, frictional stresses and the residual internal stress present in the coating. The normal load a

35、t which failure occurs is called the critical load Lc.NOTE 1 In a scratch test, a number of consecutive coating failure events may be observed at increasing critical load values. Failure by cracking through the coating thickness (through-thickness cracking) usually occurs at lower loads than detachm

36、ent of the coating. Therefore, it is quite common to characterise the onset of cracking by the critical normal load Lc1, while the onset of coating detachment defines the critical normal load Lc2. In general, a series of failure modes are observed and used to study the mechanical behaviour of the co

37、ated surface, where the onset of the nthfailure mode defines the critical load Lcn(see Annex B). NOTE 2 The critical loads at which the failure events appear depend not only on the coating adhesion strength but also on other parameters, such as loading rate, traverse speed, diamond tip wear, substra

38、te and coating roughness, some of which are directly related to the test itself, while others are related to the coating-substrate system. EN 1071-3:2005 (E) 6(a) (b) KeyX Time Y Normal load Z Indenter traverse distance Figure 1 Sketches illustrating the normal load and traverse distance versus time

39、 in (a) the progressive load, and (b) the constant load operation modes EN 1071-3:2005 (E) 74 Apparatus and materials 4.1 Scratch testerA scratch tester is an instrument used to rigidly hold the stylus and to apply both the normal load and the driving force to produce scratches. A schematic of a typ

40、ical arrangement is shown in Figure 2. NOTE 1 In general, spring deformation controlled normal load instruments are used, in which the deformation of a spring is used to achieve the chosen loading programme. Magnetically driven assemblies are also available. Where required, the scratch tester can be

41、 equipped with acoustic emission (AE) and/or friction force (FF) transducers. NOTE 2 Although it is attractive to use such methods for the on-line automatic quality control of coated parts, these techniques cannot discriminate between cohesive and adhesive failures nor do they always detect the firs

42、t occurrence of failure. Hence, AE and FF signals cannot be used as a reliable means for determining scratch test critical loads. These techniques can at best be used as a warning system in the quality control of coated components and then only after a large series of experiments on the same coating

43、 type to establish the statistics of correlation with a certain failure mode. Inspection of the scratch track by microscopic observation remains the only reliable means of associating a failure event with a measured critical normal load. To meet the requirements of this European Standard, scratch te

44、sters shall comply with the calibration requirements of Annex A. 4.2 Diamond stylus This consists of a rigidly mounted diamond normally having a Rockwell C geometry compliant with the requirements of EN ISO 6508-2. The stylus shall be inspected regularly to check for contamination and changes in geo

45、metry. If damage is observed at 200x or lower magnification then the stylus shall be changed (see 1) and if either damage or contamination is observed, the test results since the last inspection shall be disregarded. If during constant load operation the friction force increases, it should be presum

46、ed that the stylus has been contaminated. NOTE 1 Uncertainties in the Rockwell C stylus tip shape and manufacturing defects are a major source of error for the scratch test method. The use of an imperfect stylus may result in different values of critical load when the stylus is rotated in its holder

47、. Control of the stylus shape is imperative, in the as-received condition as well as during usage, to detect wear at the tip. Wear usually occurs in the form of ring cracks or crater wear which is easily visible under a reflected light microscope (magnification 100:1). NOTE 2 A certified reference m

48、aterial, BCR-6921), which presents three repeatable failure events at known critical load intervals is available for verification purposes. This can provide a good indication of overall performance, including stylus condition and calibration. 1)European Commission Directorate-General Joint Research

49、Centre, Institute for Reference Materials and Measurement (IRMM), Retieseweg 111, B-2440 Geel, Belgium. EN 1071-3:2005 (E) 82435 7 861Key1 Stylus shaft 2 Vertical load transducer 3 Upper support assembly 4 Base reference 5 XY stage to manoeuvre 6 XY stage drive arrangement 7 Low friction sample table 8 Horizontal force transducer Figure 2 Schematic diagram of a typical scratch tester EN 1071-3:2005 (E) 95 Preparation of the test piece 5.1 General requirementsA representative specimen of the product to be tested shall be used. The substrate, inte