BS EN ISO 9220-1989 Metallic coatings - Measurement of coating thickness - Scanning electron microscope method《金属镀层 镀层厚度测量 扫描电子显微镜法》.pdf

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1、BRITISH STANDARD BS EN ISO 9220:1995 Incorporating Amendment No.1 Metallic coatings Measurement of coating thickness Scanning electron microscope method The European Standard ENISO9220:1994 has the status of a British StandardBSENISO9220:1995 This British Standard, having been prepared under the dir

2、ectionof the Surface Coatings(other than Paints) Standards Policy Committee, waspublished under the authorityof the Board of BSIandcomes into effect on 29September1989 BSI 03-2000 The following BSI references relate to the work on this standard: Committee referenceSRC/14 Draft for comment87/53727DC

3、ISBN 0 580 17640 1 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Surface Coatings (other than Paints) Standards Policy Committee (SRC/-) to Technical CommitteeSRC/14, upon which the following bodies were represented: Aluminium Federati

4、on Association of Manufacturers of Domestic Electrical Appliances Association of Metal Sprayers British Anodising Association British Industrial Fasteners Federation British Jewellers Association British Telecommunications plc Department of Trade and Industry (National Physical Laboratory) Institute

5、 of Metal Finishing Institution of Corrosion Science and Technology Metal Finishing Association Ministry of Defence NDT Trade Association Society of Motor Manufacturers and Traders Limited Amendments issued since publication Amd. No. Date of issue Comments 8499 April1995 Indicated by a sideline in t

6、he marginBSENISO9220:1995 BSI 03-2000 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 1 Scope 3 2 Normative references 3 3 Definition 3 4 Principle 3 5 Instrumentation 3 6 Factors influencing the measurement results 3 7 Preparation of cross-sections 4 8 Cali

7、bration of instruments 4 9 Procedure 5 10 Measurement uncertainty 5 11 Expression of results 5 12 Test report 5 Annex A (informative) General guidance on the preparation and measurement of cross-sections 6 Annex ZA (normative) Normative references to international publications with their relevant Eu

8、ropean publications 9 Publications referred to Inside back coverBSENISO9220:1995 ii BSI 03-2000 National foreword This Part of BS5411 has been prepared under the direction of the Surface Coatings (other than Paints) Standards Policy Committee. It is identical withISO9220:1988 “Metallic coatings Meas

9、urement of coating thickness Scanning electron microscope method”, which was prepared by Technical Committee107, Metallic and other non-organic coatings, of the International Organization for Standardization (ISO), with the active participation and approval of the UK. In 1994 the European Committee

10、for Standardization (CEN) acceptedISO9220:1989 as European Standard ENISO9220:1994. As a consequence of implementing the European Standard this British Standard is renumbered asBSENISO9220 and any reference toBS5411-16 should be read as a reference toBSENISO9220. Other Parts of BS5411 have been publ

11、ished as follows: Part 1: Definitions and conventions concerning the measurement of thickness; Part 2: Review of methods of measurement of thickness; Part 3: Eddy current method for measurement of coating thickness of non-conductive coatings on non-magnetic basis metals; Part 4: Coulometric method f

12、or the measurement of coating thickness; Part 5: Measurement of local thickness of metal and oxide coatings by the microscopical examination of cross-sections; Part 6: Vickers and Knoop microhardness tests; Part 7: Profilometric method for measurement of coating thickness; Part 8: Measurement of coa

13、ting thickness of metallic coatings: X-ray spectrometric methods 1) ; Part 9: Measurement of coating thickness of electrodeposited nickel coatings on magnetic and non-magnetic substrates: magnetic method; Part 10: Review of methods available for testing adhesion of electrodeposited and chemically de

14、posited metallic coatings on metallic substrates; Part 11: Measurement of coating thickness of non-magnetic metallic and vitreous or porcelain enamel coatings on magnetic basis metals: magnetic method; Part 12: Beta backscatter method for measurement of thickness; Part 13: Chromate conversion coatin

15、gs on zinc and cadmium; Part 14: Gravimetric method for determination of coating mass per unit area of conversion coatings on metallic materials; Part 15: Review of methods of measurement of ductility. 1) Withdrawn. Cross-references InternationalStandard Corresponding British Standard BS 5411 Method

16、s of test for metallic and related coatings ISO 1463:1982 a Part 5:1984 Measurement of local thickness of metal and oxide coatings by the microscopical examination of cross-sections (Identical) ISO 2064:1980 Part 1:1980 Definitions and conventions concerning the measurement of thickness (Identical)

17、a Referred to for information only.BSENISO9220:1995 BSI 03-2000 iii Additional information. For clarity, read8.3.2 as “Repeat the measurement at three or more different locations a minimum of3mm apart on the photograph to determine the average spacing.” ISO 1463 is not a normative reference, but app

18、ears under that heading. This Part describes methods of test only and should not be used or quoted as a specification. Reference to this Part should state that the method of test used is in accordance withBS5411-16. A British Standard does not purport to include all the necessary provisions of a con

19、tract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi toiv, theENISO title page, pages2to10,

20、an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.iv blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 9220 October1994 ICS 25.220.40

21、 Descriptors: Coatings, metal coatings, tests, determination, thickness, thickness measurement English version Metallic coatings Measurement of coating thickness Scanning electron microscope method (ISO9220:1988) Revtements mtalliques Mesurage de lpaisseur de revtement Mthode au microscope lectroniq

22、ue balayage (ISO9220:1988) Metallische berzge Messung der Schichtdicke Verfahren mit Rasterelektronenmikroskop (ISO9220:1988) This European Standard was approved by CEN on1994-10-26. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving t

23、his European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions

24、(English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denma

25、rk, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-

26、1050 Brussels 1994 Copyright reserved to CEN members Ref. No. ENISO9220:1994EENISO9220:1994 BSI 03-2000 2 Foreword This European Standard was taken over by the Technical Committee CEN/TC262, Protection of metallic materials against corrosion, from the work ofISO/TC107, Metallic and other inorganic c

27、oatings, of the International Organization for Standardization (ISO). CEN/TC 262 had decided to submit the final draft for formal vote. The result was positive. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at t

28、he latest byApril1995, and conflicting national standards shall be withdrawn at the latest byApril1995. According to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Irel

29、and, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, UnitedKingdom. NOTENormative references to international publications are listed inAnnex ZA (normative).ENISO9220:1994 BSI 03-2000 3 1 Scope This InternationalStandard specifies a method for the measurement of the loc

30、al thickness of metallic coatings by examination of cross-sections with a scanning electron microscope (SEM). It is destructive and has an uncertainty of less than10% or0,14m, whichever is greater. It can be used for thicknesses up to several millimetres, but it is usually more practical to use a li

31、ght microscope (ISO1463) when applicable. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this InternationalStandard. At the time of publication, the editions indicated were valid. All standards are subject to revision

32、, and parties to agreements based on this InternationalStandard are encouraged to investigate the possibility of applying the most recent editions of the standards listed below. Members of IEC and ISO maintain registers of currently valid InternationalStandards. ISO 1463:1982, Metallic and oxide coa

33、tings Measurement of coating thickness Microscopical method. ISO 2064:1980, Metallic and other non-organic coatings Definitions and conventions concerning the measurement of thickness. 3 Definition For the purposes of this InternationalStandard, the following definition applies. local thickness the

34、mean of the thickness measurements, of which a specified number is made within a reference area (SeeISO2064.) 4 Principle A test specimen is cut, ground, and polished from a cross-section of the coating for metallographic examination by a scanning electron microscope. The measurement is made on a co

35、nventional micrograph or on a photograph of the video waveform signal for a single scan across the coating. 5 Instrumentation 5.1 Scanning electron microscope (SEM) The SEM shall have a resolution capability of50nm or better. Suitable instruments are available commercially. 5.2 SEM stage micrometer

36、A stage micrometer or graticule is required for calibration of the magnification of the SEM. The stage micrometer or graticule shall have an uncertainty of less than5% for the magnification employed. Suitable stage micrometers or graticules are available commercially. 6 Factors influencing the measu

37、rement results The following factors may affect the accuracy of a measurement of coating thickness. 6.1 Surface roughness If the coating or its substrate is rough relative to the coating thickness, one or both of the interfaces bounding the coating cross-section may be too irregular to permit accura

38、te measurement of the average thickness in the field of view. 6.2 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. For example, an inclination of10 to the perpendicular will cont

39、ribute a1,5% error. 6.3 Specimen tilt Any tilt of the specimen (plane of cross-section) with respect to the SEM beam may result in an inaccurate measurement. NOTEIf the tilt of the test specimen is different from that used for calibration, inaccuracies may result. 6.4 Coating deformation Detrimental

40、 deformation of the coating can be caused by excessive temperature or pressure during the mounting and preparation of cross-sections of soft coatings or coatings that melt at low temperatures, and by excessive abrasion of brittle materials during preparation of cross-sections. 6.5 Rounding of edges

41、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 (see6.6 and clause

42、A.1). 6.6 Overplating Overplating of the test specimen serves to protect the coating edges during preparation of cross-sections and thus to prevent an inaccurate measurement. Removal of the coating material during surface preparation for overplating can cause a low thickness measurement.ENISO9220:19

43、94 4 BSI 03-2000 6.7 Etching Optimum etching will produce a clearly defined and narrow dark line at the interface between the two metals. A wide or poorly defined line can result in an inaccurate measurement. 6.8 Smearing Polishing may leave smeared metal that obscures the true boundary between two

44、metals and results in an inaccurate measurement. This may occur with soft metals like lead, indium, and gold. To help identify whether or not there is smearing, repeat the polishing, etching, and measurement several times. Any significant variation in readings is an indication of possible smearing.

45、6.9 Poor contrast The visual contrast between metals in an SEM is poor when their atomic numbers are close together. For example, bright and semi-bright nickel layers may not be discriminable unless their common boundary can be brought out sufficiently by appropriate etching and SEM techniques. For

46、some metal combinations, energy dispersive X-ray techniques (seeA.3.5) or backscatter images (seeA.3.6) can be helpful. 6.10 Magnification For a given coating thickness, measurement errors tend to increase with decreasing magnification. If practical, the magnification should be chosen so that the fi

47、eld of view is between1,5 and3times the coating thickness. The magnification readout of an SEM often differs from the actual magnification by more than the5% often quoted and, for some instruments, the magnification has been found to vary by25% across the field. Magnification errors are minimized by

48、 appropriate use of an SEM stage micrometer. 6.11 Uniformity of magnification Because the magnification may not be uniform over the entire field, errors can occur if both the calibration and the measurement are not made over the same portion of the field. These errors can be very significant. 6.12 S

49、tability of magnification 6.12.1 The magnification of an SEM may drift with time. This effect is minimized by mounting the stage micrometer and test specimen side by side on the SEM stage so as to keep the transfer time short. 6.12.2 A change in magnification can occur when adjustments are made with the focusing and other SEM electronic controls; for example the scan rotation, operating voltage and contrast controls. Such a change is prevented by not using the focus controls or other SEM electronic contr