EN 1071-4-2006 en Advanced technical ceramics - Methods of test for ceramic coatings - Part 4 Determination of chemical composition by electron probe microanalysis (EPMA)《先进技术陶瓷 陶瓷.pdf

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1、BRITISH STANDARDBS EN 1071-4:2006Advanced technical ceramics Methods of test for ceramic coatings Part 4: Determination of chemical composition by electron probe microanalysis (EPMA)The European Standard EN 1071-4:2006 has the status of a British StandardICS 81.060.30g49g50g3g38g50g51g60g44g49g42g3g

2、58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 1071-4:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 June 2

3、006 BSI 2006ISBN 0 580 48519 6National forewordThis British Standard is the official English language version of EN 1071-4:2006. It supersedes DD ENV 1071-4:1996 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics, which

4、 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 Catalogue under the section

5、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 application. Compli

6、ance 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 related inte

7、rnational 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 15 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments

8、 issued since publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 1071-4February 2006ICS 81.060.30 Supersedes ENV 1071-4:1995 English VersionAdvanced technical ceramics - Methods of test for ceramiccoatings - Part 4: Determination of chemical composition byelectron pro

9、be microanalysis (EPMA)Cramiques techniques avances - Mthodes dessaispour revtements cramiques - Partie 4 : Dtermination dela composition chimique avec analyse par microsondelectronique (EPMA)Hochleistungskeramik - Verfahren zur Prfung keramischerSchichten - Teil 4: Bestimmung der chemischenZusammen

10、setzung durch Elektronenstrahl-Mikrobereichsanalyse (ESMA)This European Standard was approved by CEN on 30 December 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

11、 any alteration. 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 b

12、y translationunder 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

13、, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Cent

14、re: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 1071-4:2006: EEN 1071-4:2006 (E) 2 Contents Page Foreword 3 1 Scope. 5 2 Normative references. 5 3 Terms and definitions 5 3.1 General 5 3.2

15、 Terms used in electron probe microanalysis. 6 4 Principle 7 5 Apparatus and materials 8 5.1 General 8 5.2 Scanning electron microscope 8 5.3 Electron probe microanalyser . 9 5.4 Energy dispersive spectrometer . 9 5.5 Wavelength dispersive spectrometer . 9 6 Preparation of test piece 9 6.1 General 9

16、 6.2 Surface roughness . 9 6.3 Surface conduction 10 7 Test procedure 11 7.1 General 11 7.2 Instrument conditions 11 7.3 Analysis of thin coatings . 11 7.4 Analysis of thick coatings . 12 7.5 Analysis of multilayer coatings. 12 8 Accuracy and interferences. 13 9 Test report. 13 Bibliography 15 EN 10

17、71-4:2006 (E) 3 Foreword This European Standard (EN 1071-4:2006) 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

18、text or by endorsement, at the latest by August 2006, and conflicting national standards shall be withdrawn at the latest by August 2006. EN 1071 Advanced technical ceramics Methods of test for ceramic coatings consists of 11 Parts: Part 1: Determination of coating thickness by contact probe profilo

19、meter 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: Determi

20、nation 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 adhesion Part 9: Determination of fracture strain Part 10: Determination of coating

21、 thickness by cross sectioning Part 11: Determination of internal stress by the Stoney formula Parts 7 to 11 are Technical Specifications. This European Standard supersedes ENV 1071-4:1995. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following count

22、ries 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, Romania, Slovakia, Slovenia, Spain, Sweden,

23、 Switzerland and United Kingdom. EN 1071-4:2006 (E) 4 Introduction Electron probe microanalysis (EPMA) is a commonly used analytical technique which is applicable to a wide range of materials in bulk form. While international standards for this procedure have been developed under ISO/TC 202 Microbea

24、m analysis, currently no European or international standard considers the application of EPMA to ceramic coating analysis. Terms and definitions, including those used in this European Standard that are not specific to this standard are given in ISO 18115 and in ISO 23833. The composition of a coatin

25、g is a critical factor determining the performance of a product, so this analytical procedure can be used in quality control, coating development, characterisation and for design data acquisition purposes. Reference works on electron probe microanalysis are listed in the Bibliography 1, 2. EN 1071-4

26、:2006 (E) 5 1 Scope This European Standard describes methods for chemical analysis of ceramic coatings by means of electron probe microanalysis (EPMA) using a scanning electron microscope (SEM) or an electron probe microanalyser. The methods described are limited to the examination of single layer c

27、oatings when the analysis is carried out normal to the sample surface, but graded and multilayer coatings may also be analysed in cross-section if the thickness of the individual layers or gradations are greater than the maximum width of the volume of material within which characteristic or fluoresc

28、ent X-rays are generated. NOTE This method can also be used for the analysis of bulk materials. 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 e

29、dition of the referenced document (including any amendments) applies. EN 623-4, Advanced technical ceramics Monolithic ceramics General and textural properties Part 4: Determination of surface roughness EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories

30、 (ISO/IEC 17025:2005) ISO 14594, Microbeam analysis Electron probe microanalysis Guidelines for the determination of experimental parameters for wavelength dispersive spectroscopy ISO 15632, Microbeam analysis Instrumental specification for energy dispersive X-ray spectrometers with semiconductor de

31、tectors 3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. NOTE Definitions of further terms are given in ISO 23833 and the International Vocabulary of basic and general terms in Metrology. 3 3.1 General 3.1.1 thick coating coating with a t

32、hickness 20 m 3.1.2 thin coating coating with a thickness 20 m EN 1071-4:2006 (E) 6 3.2 Terms used in electron probe microanalysis 3.2.1 absorption correction A matrix correction arising from the loss of X-ray intensity of element “A“ while propagating through the specimen in the direction of the X-

33、ray spectrometer due to photoelectric absorption by all elements within the specimen 3.2.2 atomic number correction Z matrix correction for the modification of the X-ray intensity for element “A“ due to electron backscattering and stopping power, which are influenced by all elements in the analytica

34、l volume 3.2.3 backscattered electrons incident beam electrons that have been re-emitted from the specimen surface due to multiple scattering NOTE They are of a high energy (up to the energy of the beam) and can provide atomic number contrast. 3.2.4 beam current electron beam current, in A (measured

35、 using a Faraday cup near the position of the specimen in the instrument) 3.2.5 Bragg angle angle, in degrees, between the diffracting crystal surface and the X-rays being analysed 3.2.6 count rate number of X-ray counts per second 3.2.7 critical excitation energy Ec minimum energy required to ionis

36、e an atom from a specific electron shell, in eV 3.2.8 dead time length of time, in a measurement system that processes one event at a time, during which the system is engaged in processing a photon event (“busy“), such that it is unavailable to process another photon which randomly appears in this t

37、ime interval 3.2.9 electron beam energy Eo energy of the electrons of the beam at the sample, in eV 3.2.10 electron probe microanalysis (EPMA) technique of spatially-resolved elemental analysis based upon electron-excited X-ray spectrometry with a focused electron probe and an electron interaction v

38、olume with micrometer to sub-micrometer dimensions EN 1071-4:2006 (E) 7 3.2.11 energy dispersive X-ray spectrometry (EDS) method for examining the intensity of X-rays as a function of the photon energy 3.2.12 fluorescence correction F correction applied to account for characteristic X-ray excitation

39、 by X-ray photons of higher energy 3.2.13 overvoltage U ratio of the incident beam energy to the critical excitation energy for a particular shell NOTE This factor should be greater than unity for characteristic X-ray production to occur from that atomic shell. 3.2.14 (z) matrix correction method of

40、 quantitative electron probe X-ray microanalysis in which correction factors are calculated from empirical equations developed from fits to experimental data of X-ray production as a function of depth the so-called (z) function 3.2.15 peak overlap merging of peaks of nearly the same energy which can

41、not be resolved by the detector 3.2.16 secondary electron electron of the specimen emitted as a result of inelastic scattering of the primary beam electron with loosely bound valence-level electrons of the specimen NOTE They are of a low energy ( 50 eV) and provide information about surface topograp

42、hy. 3.2.17 take off angle angle, in degrees, between the specimen surface and the line of sight to the centre of the detector 3.2.18 wavelength dispersive X-ray spectrometry (WDS) device for determining X-ray intensity as a function of the wavelength of the radiation, where separation is based upon

43、Braggs law, n = 2dsin , where is the X-ray wavelength, d is the spacing of the atom planes of the crystal or the repeated layers of the synthetic diffractor, and is the angle at which constructive interference takes place NOTE X-rays diffracted at a particular angle are directed to a gas counter ope

44、rated in the proportional response regime where the charge produced is proportional to the photon energy. 3.2.19 working distance distance, in metres, from the principal plane of the objective lens to the cross-over of the focused probe 4 Principle Analysis is carried out by means of an electron bea

45、m striking the sample and characterization of the X-rays subsequently emitted. The incident electrons eject an electron from the K, L or M shell of an EN 1071-4:2006 (E) 8 atom in the sample. X-ray emission occurs when an electron from a higher energy shell replaces the electron ejected from the low

46、er energy shell (see Figure 1). For example a KX-ray is generated when an electron transition from an L to a K shell occurs with consequent release of energy in the form of an X-ray and a KX-ray is generated by an M to K shell transition. The X-rays are detected by use of either energy dispersive X-

47、ray spectrometers (EDS) or wavelength dispersive X-ray spectrometers (WDS). KLMKL M NFigure 1 Spectrum of X-rays that may be generated from a single element 5 Apparatus and materials 5.1 General Various commercial instruments are available which are based on a general-purpose scanning electron micro

48、scope or a purpose built electron microprobe analyser; the former is more commonly used. The instruments deliver a finely focused beam of electrons to the test piece which generates X -rays which are then analysed with either an energy or wavelength dispersive X-ray spectrometer. An energy dispersiv

49、e spectrometer shall conform to the specification detailed in ISO 15632, while a wavelength dispersive spectrometer shall be operated in accordance with ISO 14594. Usually an SEM is used in which high resolution imaging with secondary or backscattered electrons is also possible; an electron probe microanalyser generally has poorer imaging than an SEM but better beam stability and allows more extensive use of wavelength spectrometry, which results in improved analytical sensitivity and resolution. The X-ray spectra