1、 DEUTSCHE NORMMay 2006DIN EN 1071-4 ICS 81.060.30 Supersedes DIN V ENV 1071-4:1995-11 Advanced technical ceramics Methods of test for ceramic coatings Part 4: Determination of chemical composition by electron probe microanalysis (EPMA) English version of DIN EN 1071-4:2006-05 Hochleistungskeramik Ve
2、rfahren zur Prfung keramischer Schichten Teil 4: Bestimmung der chemischen Zusammensetzung durch Elektronenstrahl-Mikrobereichsanalyse (ESMA) Englische Fassung DIN EN 1071-4:2006-05 Document comprises 17 pages No part of this standard may be reproduced without prior permission of DIN Deutsches Insti
3、tut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-Normen). English price group 9 www.din.de www.beuth.de !,nh“10.06 9756994DIN EN 1071-4:2006-05 2 National foreword This standard has been prepared by CEN/TC 184 Advanced
4、technical ceramics (Secretariat: United Kingdom), Working Group WG 5 Testing of ceramic coatings. The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee). However, at present a DIN committee does not exist for this standa
5、rd since the parties concerned have not shown any interest in work on the subject. Amendments This standard differs from DIN V ENV 1071-4, November 1995 edition, as follows: a) The standard has been revised in form and substance. Previous editions DIN V ENV 1071-4: 1995-11 EUROPEAN STANDARD NORME EU
6、ROPENNE EUROPISCHE NORM EN 1071-4 February 2006 ICS 81.060.30 Supersedes ENV 1071-4:1995 English Version Advanced technical ceramics - Methods of test for ceramic coatings - Part 4: Determination of chemical composition by electron probe microanalysis (EPMA) Cramiques techniques avances - Mthodes de
7、ssais pour revtements cramiques - Partie 4 : Dtermination de la composition chimique avec analyse par microsonde lectronique (EPMA) Hochleistungskeramik - Verfahren zur Prfung keramischer Schichten - Teil 4: Bestimmung der chemischen Zusammensetzung durch Elektronenstrahl-Mikrobereichsanalyse (ESMA)
8、 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 European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical r
9、eferences 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 (English, French, German). A version in any other language made by translation under the responsibility of a CEN membe
10、r 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithu
11、ania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2006
12、 CEN All rights of exploitation in any form and by any means reserved worldwide 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 Terms used in electron probe microanal
13、ysis 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 6.2 Surface roughness 9 6.3 Surface
14、 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 1071-4:2006 (E) 3 Foreword This Europe
15、an 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 text or by endorsement, at the lates
16、t 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 profilometer Part 2: Determination of coati
17、ng 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
18、 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 thickness by cross sectioning Part
19、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 countries are bound to implement this Eur
20、opean 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, Switzerland and United Kingdom. EN
21、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 Microbeam analysis, currently no European or
22、 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 coating is a critical factor determining t
23、he 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 1071-4:2006 (E) 5 1 Scope This European St
24、andard 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 coatings when the analysis is carried
25、 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 fluorescent X-rays are generated. NOTE This
26、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 edition of the referenced document (i
27、ncluding 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 (ISO/IEC 17025:2005) ISO 14594, Mic
28、robeam 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 detectors 3 Terms and definitions For
29、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 thickness 20 m 3.1.2 thin coating coa
30、ting 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-ray spectrometer due to photoelectri
31、c 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 analytical volume 3.2.3 backscattered electro
32、ns 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 using a Faraday cup near the positi
33、on 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 ionise an atom from a specific electron s
34、hell, 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 time interval 3.2.9 electron beam ene
35、rgy 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 volume with micrometer to sub-microme
36、ter 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 by X-ray photons of higher energy 3
37、.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 quantitative electron probe X-ray m
38、icroanalysis 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 cannot be resolved by the detector 3.2.
39、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 topography. 3.2.17 take off angle angle, in
40、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 Braggs law, n = 2dsin , where is the
41、 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 operated in the proportional response r
42、egime 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 beam striking the sample and characteri
43、zation 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 lower energy shell (see Figure 1). For
44、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-ray spectrometers (EDS) or wavelengt
45、h 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 microscope or a purpose built electron mi
46、croprobe 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 dispersive spectrometer shall conform to the
47、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 ima
48、ging 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 obtained are evaluated using proprietary software. 5.2 Scanning electron microscope An electron beam is generated un
49、der vacuum by an electron gun and focussed using electro-magnetic lenses. The electron beam is scanned across the surface of a specimen and thereby generates secondary electrons, backscattered electrons or X-rays. The electrons interact only with a very small volume of material that depends on energy of the electron beam and material EN 1071-4:2006 (E) 9 characteristics such as atomic number and density, but generally this volume is 1-3 m3. The SEM is usually equipped with an energy dispersive spectrometer
