1、October 2010 Translation by DIN-Sprachendienst.English price group 10No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC
2、S 77.040.99; 77.160!$kTi“1724970www.din.deDDIN EN ISO 4499-1Hardmetals Metallographic determination of microstructure Part 1: Photomicrographs and description (ISO 4499-1:2008)English translation of DIN EN ISO 4499-1:2010-10Hartmetalle Metallographische Bestimmung der Mikrostruktur Teil 1: Gefgebild
3、er und Beschreibung (ISO 4499-1:2008)Englische bersetzung von DIN EN ISO 4499-1:2010-10Mtaux-durs Dtermination mtallographique de la microstructure Partie 1: Prises de vue photomicrographiques et description (ISO 4499-1:2008)Traduction anglaise de DIN EN ISO 4499-1:2010-10Together with DIN EN ISO449
4、9-2:2010-10,supersedesDIN ISO 4499:1991-07www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 16 pages10.10 DIN EN ISO 4499-1:2010-10 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Co
5、mmittee ISO/TC 119 “Powder metallurgy” (Secretariat: SIS, Sweden) in collaboration with Technical Committee CEN/SS M11 “Powder metallurgy” (Secretariat: CCMC). The responsible German body involved in its preparation was the Normenausschuss Werkstofftechnologie (Technology of Materials Standards Comm
6、ittee), Working Committee NA 145-01-04 AA Probenahme und Prfverfahren fr Hartmetalle. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3878:1983 DIN ISO 3878:1991-07 ISO 4499-2 DIN EN ISO 4499-2 Amendments This standard differs from DIN
7、ISO 4499:1991-07 as follows: a) the standard has been technically revised; b) the apparatus (Clause 4) has been extended; c) in Clause 6 “Procedure”, a new subclause (6.1) relating to the metallographic preparation has been added; d) in Clause 6 “Procedure”, specifications relating to etching have b
8、een extended; e) photomicrographs (Figures 1 to 3) have been included; f) normative references have been updated; g) the standard has been editorially revised. Previous editions DIN ISO 4499: 1991-07 DIN EN ISO 4499-1:2010-10 3 National Annex NA (informative) Bibliography DIN ISO 3878:1991-07, Hardm
9、etals Vickers hardness test DIN EN ISO 4499-2, Hardmetals Metallographic determination of microstructure Part 2: Measurement of WC grain size DIN EN ISO 4499-1:2010-10 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4499-1 May 2010 ICS 77.040.99; 77.160 Su
10、persedes 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 4499-1:2008
11、) Hartmetalle - Metallographische Bestimmung der 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 giving this European Standard the status of a national standard without any alter
12、ation. 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 versions (English, French, German). A version in any other language made by tran
13、slation 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, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Fran
14、ce, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, 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
15、 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: E(ISO 4499-1:2008) Mikrostruktur - Teil 1: Gefgebilder und Beschreibung 2 DIN EN ISO 4499-1:2010-10
16、 EN ISO 4499-1:2010 (E) Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Apparatus .4 5 Preparation of testpiece section 4 6 Procedure .5 7 Test report . 11 Bibliography. 12 3 Foreword The text of ISO 4499-1:2008 has been prepared by Technical Committee ISO/TC
17、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 national standard, either by publication of an identical text or by endorsement, at the latest by November 2010, an
18、d 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 patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. Th
19、is 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 for the quantitative measurement of the WC grain size of hardmetals. ISO 4499-3 and ISO 4499-4 are additiona
20、l 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-stoichiometric phases (e.g. carbon and eta-phase). ISO 4499-3 and ISO 4499-4 are currently in development. In st
21、andard 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 is stoichiometric. If the composition is either high or low in total carbon content then it is possible to see
22、 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 determination of these phases will be outlined in ISO 4499-3. ISO 4499 consists of the following parts, under the genera
23、l title Hardmetals Metallographic determination of microstructure: Part 1: Photomicrographs and description Part 2: Measurement of WC grain size According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Sta
24、ndard: Austria, Belgium, 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 the Unite
25、d 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. DIN EN ISO 4499-1:2010-10 EN ISO 4499-1:2010 (E) 1 Scope This part of ISO 4499 specifies the methods of metallographic determination of the microstructure of hardmetal
26、s using photomicrographs. 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.
27、ISO 3878:1983, Hardmetals 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 bind
28、er phase (for example, 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 m
29、icroscope for magnification over 1 500 . 4.3 Equipment for preparation of testpiece sections. DIN EN ISO 4499-1:2010-10 EN ISO 4499-1:2010 (E) 45 Preparation of testpiece section The testpiece section shall be prepared as for metallographic examination, and the surface to be examined shall be free f
30、rom 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 rem
31、ove 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 p
32、aper. 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 B66
33、5)2. 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 mic
34、rostructure 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
35、observed. 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
36、 on 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, bu
37、t sufficiently 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 in
38、scribed 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 t
39、hese 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
40、 poured 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 rel
41、atively 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 an
42、d they shall be stored in cool conditions. DIN EN ISO 4499-1:2010-10 EN ISO 4499-1:2010 (E) 5A 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-setting resins c
43、an 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 all the main supp
44、liers 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
45、 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 of preparation is removed, and then continued for the same amount of time to remove su
46、bsurface damage. Typically, for homogenous microstructures, at least 200 m of material (see ISO 3878:1983) should be removed during the grinding process to obtain a section representative of the bulk microstructure. For materials with gradient structures, more care may be needed in controlling the a
47、mount removed. The diamond grinding discs are available in several forms; metal bonded, resin bonded, wire mesh and plastic encapsulated. These vary considerably in cost and longevity of use, the resin bonded being the most durable and expensive. 6.1.5 Lapping Occasionally, a lapping stage may be in
48、corporated into the preparation procedure immediately after grinding. Lapping is normally carried out on a glass, metal, plastic or composite platen to which diamond abrasive is applied. The key features of lapping are the following: the production of a plane surface; an intermediate step between gr
49、inding and polishing; the removal of surface damage without imparting substantial further subsurface damage; relatively high rates of surface removal compared to the same size of diamond abrasive used on a polishing cloth. Several suppliers provide laps of different compositions depending on the hardness of the material to be prepared. However, this stage of preparation may not be necessary if a coarser size of diamond abrasive is used on a polishing cloth as an additional stage. As with the grinding stages, the time of l
