1、BS EN ISO4499-1:2010ICS 77.040.99; 77.160NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDHardmetals Metallographicdetermination ofmicrostructurePart 1: Photomicrographs anddescription (ISO 4499-1:2008)This British Standard was published under the authority of th
2、e Standards Policy and Strategy Committee on 30 June 2010 BSI 2010ISBN 978 0 580 69609 1Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 4499-1:2010National forewordThis British Standard is the UK implementation of EN ISO 4499-1:2010. It is identical to ISO 4499-1:2008. Together
3、with BS EN ISO 4499-2:2010, it supersedes BS EN 24499:1993 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee ISE/65, Sintered metal components.A list of organizations represented on this committee can be obtained on request to its secretary.This publicat
4、ion does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4499-1 May 2010 ICS 77.040.99; 77.1
5、60 Supersedes EN 24499:1993English Version Hardmetals - Metallographic determination of microstructure - Part 1: Photomicrographs and description (ISO 4499-1:2008) Mtaux-durs - Dtermination mtallographique de la microstructure - Partie 1: Prises de vue photomicrographiques et description (ISO 4499-1
6、:2008) Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 1: Gefgebilder und Beschreibung (ISO 4499-1:2008) This European Standard was approved by CEN on 30 April 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for givin
7、g this 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 CEN Management Centre or to any CEN member. This European Standard exists in three official vers
8、ions (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 CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium
9、, Bulgaria, Croatia, 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 COMMITT
10、EE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4499-1:2010: EBS EN ISO 4499-1:2010E
11、N ISO 4499-1:2010 (E) 3 Foreword The text of ISO 4499-1:2008 has been prepared by Technical Committee ISO/TC 119 “Powder metallurgy” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 4499-1:2010. This European Standard shall be given the status of a nation
12、al standard, either by publication of an identical text or by endorsement, at the latest by November 2010, and conflicting national standards shall be withdrawn at the latest by November 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of pate
13、nt rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 24499:1993. ISO 4499-1, together with ISO 4499-2, cancels and replaces ISO 4499:1978, which has been technically revised. In ISO 4499-2, a new section has been added
14、 for the quantitative measurement of the WC grain size of hardmetals. ISO 4499-3 and ISO 4499-4 are additional parts that will deal with the microstructures of hardmetals containing cubic carbides and Ti (C, N)-based hardmetals, and miscellaneous microstructural features, such as defects and non-sto
15、ichiometric phases (e.g. carbon and eta-phase). ISO 4499-3 and ISO 4499-4 are currently in development. In standard WC/Co hardmetals the density is generally controlled so that only two phases WC and Co are present. The Co phase is an alloy and contains some W and C in solid solution. The WC phase i
16、s stoichiometric. If the composition is either high or low in total carbon content then it is possible to see a third phase in the structure. For a high C content this is graphite; for a low C content it is eta phase (), typically an M6C or M12C carbide where M is (CoxWy). Metallographic determinati
17、on of these phases will be outlined in ISO 4499-3. ISO 4499 consists of the following parts, under the general title Hardmetals Metallographic determination of microstructure: Part 1: Photomicrographs and description Part 2: Measurement of WC grain size According to the CEN/CENELEC Internal Regulati
18、ons, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
19、 Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 4499-1:2008 has been approved by CEN as a EN ISO 4499-1:2010 without any modification. BS EN ISO 4499-1:2010ISO 4499-1:2008(E) ISO 2008 All right
20、s reserved iiiContents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Terms and definitions .1 4 Apparatus .1 5 Preparation of testpiece section 2 6 Procedure .2 7 Test report 8 Bibliography 9 BS EN ISO 4499-1:2010ISO 4499-1:2008(E) iv ISO 2008 All rights reservedForeword ISO (the Internation
21、al Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been e
22、stablished has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standard
23、ization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for vo
24、ting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all su
25、ch patent rights. ISO 4499-1 was prepared by Technical Committee ISO/TC 119, Powder metallurgy, Subcommittee SC 4, Sampling and testing methods for hardmetals. ISO 4499-1, together with ISO 4499-2, cancels and replaces ISO 4499:1978, which has been technically revised. In ISO 4499-2, a new section h
26、as been added for the quantitative measurement of the WC grain size of hardmetals. ISO 4499-3 and ISO 4499-4 are additional parts that will deal with the microstructures of hardmetals containing cubic carbides and Ti (C, N)-based hardmetals, and miscellaneous microstructural features, such as defect
27、s and non-stoichiometric phases (e.g. carbon and eta-phase). ISO 4499-3 and ISO 4499-4 are currently in development. In standard WC/Co hardmetals the density is generally controlled so that only two phases WC and Co are present. The Co phase is an alloy and contains some W and C in solid solution. T
28、he WC phase is stoichiometric. If the composition is either high or low in total carbon content then it is possible to see a third phase in the structure. For a high C content this is graphite; for a low C content it is eta phase (), typically an M6C or M12C carbide where M is (CoxWy). Metallographi
29、c determination of these phases will be outlined in ISO 4499-3. ISO 4499 consists of the following parts, under the general title Hardmetals Metallographic determination of microstructure: Part 1: Photomicrographs and description Part 2: Measurement of WC grain size BS EN ISO 4499-1:2010INTERNATIONA
30、L STANDARD ISO 4499-1:2008(E) ISO 2008 All rights reserved 1Hardmetals Metallographic determination of microstructure Part 1: Photomicrographs and description 1 Scope This part of ISO 4499 specifies the methods of metallographic determination of the microstructure of hardmetals using photomicrograph
31、s. 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. ISO 3878:1983, Hardmeta
32、ls Vickers hardness test ISO 4499-2, Hardmetals Metallographic determination of microstructure Part 2: Measurement of WC grain size 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 -phase tungsten carbide 3.2 -phase binder phase (for example,
33、based on Co, Ni, Fe) 3.3 -phase carbide having a cubic lattice (for example, TiC, Tac) which may contain other carbides (for example WC) in solid solution 4 Apparatus 4.1 Metallographic microscope, permitting observations at magnifications up to 1 500 . 4.2 Scanning electron microscope for magnifica
34、tion over 1 500 . 4.3 Equipment for preparation of testpiece sections. BS EN ISO 4499-1:2010ISO 4499-1:2008(E) 2 ISO 2008 All rights reserved5 Preparation of testpiece section The testpiece section shall be prepared as for metallographic examination, and the surface to be examined shall be free from
35、 grinding and polishing marks. Care shall be taken to avoid tearing-out of particles, which may lead to a wrong evaluation of microstructure. NOTE There are several methods for preparation of hardmetal surfaces for metallographic examination. Firstly, careful coarse grinding is carried out to remove
36、 sufficient material to ensure that the true structure is revealed. After grinding with fine diamond-grit wheels, polishing is effected by using diamond paste or diamond powders, of progressively finer grain size down to 1 m, on rigidly supported laps of, for example, thin plastic, thin felt or pape
37、r. A Good Practice Guide1has been written by the UK National Physical Laboratory that gives detailed guidelines on microstructural preparation. Key points from the Good Practice Guide are included in 6.1. ASTM has also prepared a thorough standard on sample preparation that merits study (ASTM B665)2
38、. 6 Procedure 6.1 Metallographic preparation 6.1.1 General Good metallographic preparation is essential to produce a plane polished sample that when etched reveals the true microstructure of the hardmetal. Bad preparation can lead to grain tear-out, uneven etching and misleading detail in the micros
39、tructure which will affect any subsequent measurement. Preparation and etching procedures may require toxic or dangerous chemicals. Personnel should be adequately trained, and facilities and precautions as laid down in the relevant safety guidelines in place at the laboratory concerned should be obs
40、erved. 6.1.2 Sectioning In many cases, the hardmetal sample may have to be sectioned into smaller samples for metallographic preparation. Diamond tooling is normally required to cut hardmetals into smaller samples. There is a wide variety of cut-off machines which use blades with diamond embedded on
41、 the rim of the disc. Fast cutting times are easily achieved. Wire-cutting machines, in which diamond is embedded in a wire, offer a cheaper method. Very fine slices can be obtained using this method but only at a relatively slow rate of cutting. A faster method is electro-discharge machining, but s
42、ufficiently fast machines are not generally suited to a metallographic preparation facility. 6.1.3 Mounting Mounting of the sample into a resin has several advantages: it is more suitable for automatic preparation, the sample is easier to handle, and the specimen codes or identification can be inscr
43、ibed or written onto the mount. Cold-setting and thermo-setting resins are available. Thermo-setting powders (such as phenolic or diallyl phthalate powders) require a mounting press in which the sample is placed in a chamber, resin is then added, and is melted under pressure. The cycle time for thes
44、e machines can be quite slow. The advantage is that hazardous chemicals are not used and the resin has an unlimited shelf life. Cold-setting resins (such as epoxy, acrylic or polyester resins) do not require additional equipment apart from the moulds in which the sample is placed and the resin is po
45、ured on top. The resins normally consist of two parts, a monomer and a catalyst. Occasionally a third filler material is used; this may be to increase the hardness or to act as a conductive medium. Various types are available which set in minutes or hours; the quicker-setting material reaches relati
46、vely high temperatures while the slow-setting resin remains cool. Mounting of samples in “quick-setting resins” is faster, whilst cold-setting resin is more economical for batches. However, a drawback is that these resins usually have an associated chemical risk, they have a limited shelf-life and t
47、hey shall be stored in cool conditions. BS EN ISO 4499-1:2010ISO 4499-1:2008(E) ISO 2008 All rights reserved 3A further consideration is that, following metallographic preparation of a flat surface, the hardmetal sample may have to be removed from the mount before etching or placing in the SEM. Cold
48、-setting resins can be quite difficult to remove and may require grinding away from the sample. 6.1.4 Grinding Whichever method is used to obtain a section of a hardmetal sample, it will have considerable surface and subsurface damage that shall be removed. Diamond grinding discs are available from
49、all the main suppliers of metallographic equipment. These come in a range of diamond abrasive sizes and can produce very high rates of material removal from the surface of the sample. They should be used in order of decreasing abrasive size to both remove surface and subsurface damage and to obtain the plane section of the hardmetal sample which is to be polished. At each stage of grinding, the process should be continued until the surface damage (observed by optical examination without magnification) from the previous stage
