SE535684C2 - Method of producing a gradient component of metal / cemented carbide - Google Patents
Method of producing a gradient component of metal / cemented carbide Download PDFInfo
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- SE535684C2 SE535684C2 SE1150254A SE1150254A SE535684C2 SE 535684 C2 SE535684 C2 SE 535684C2 SE 1150254 A SE1150254 A SE 1150254A SE 1150254 A SE1150254 A SE 1150254A SE 535684 C2 SE535684 C2 SE 535684C2
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- sintering
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- preterably
- temperature
- fgm
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Links
- 238000000034 method Methods 0.000 title claims abstract description 58
- 229910052751 metal Inorganic materials 0.000 title claims description 12
- 239000002184 metal Substances 0.000 title claims description 12
- 238000005245 sintering Methods 0.000 claims abstract description 70
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 43
- 239000010959 steel Substances 0.000 claims description 43
- 229910000831 Steel Inorganic materials 0.000 claims description 42
- 238000002490 spark plasma sintering Methods 0.000 claims description 23
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000010941 cobalt Substances 0.000 claims description 10
- 229910017052 cobalt Inorganic materials 0.000 claims description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 10
- 238000007731 hot pressing Methods 0.000 claims description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- 150000004767 nitrides Chemical class 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 101000635799 Homo sapiens Run domain Beclin-1-interacting and cysteine-rich domain-containing protein Proteins 0.000 claims 1
- 102100030852 Run domain Beclin-1-interacting and cysteine-rich domain-containing protein Human genes 0.000 claims 1
- 239000010410 layer Substances 0.000 description 33
- 239000000843 powder Substances 0.000 description 22
- 238000002844 melting Methods 0.000 description 11
- 230000008018 melting Effects 0.000 description 11
- ZVNPWFOVUDMGRP-UHFFFAOYSA-N 4-methylaminophenol sulfate Chemical compound OS(O)(=O)=O.CNC1=CC=C(O)C=C1.CNC1=CC=C(O)C=C1 ZVNPWFOVUDMGRP-UHFFFAOYSA-N 0.000 description 7
- 229910052582 BN Inorganic materials 0.000 description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 5
- 229910009043 WC-Co Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910000851 Alloy steel Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 241000606333 Phos Species 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008094 contradictory effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000013021 overheating Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- BWHLPLXXIDYSNW-UHFFFAOYSA-N ketorolac tromethamine Chemical compound OCC(N)(CO)CO.OC(=O)C1CCN2C1=CC=C2C(=O)C1=CC=CC=C1 BWHLPLXXIDYSNW-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/008—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression characterised by the composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0292—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with more than 5% preformed carbides, nitrides or borides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
63883 17 ABSTRACT The invention reiotes to o method of preporotion of o FGM shope with o first surfocecomprising up to 100% of o first moteriol ond o second surfoce comprising up to100% of o second moterioi using sintering, preferobiy spork plosmo sintering (SPS).The method comprises the steps of: selecting the first moterioi with o first sinteringtemperoture ond o first meiting temperoture ond the second moteriol with o secondsintering temperoture ond o second meiting temperoture , wherein the first meitingtemperature is higher thon the second meiting temperoture, looding o first ioyer ofthe first moteriol in o die, odding ot ieost one intermediote ioyer on the first loyer,the intermediote ioyer comprising o mix of the first ond second moterioi creoting onintermediote groded composite region ond iooding o second loyer of the secondmoteriol on the ot ieost one intermediote ioyer. The invention is chorocterized in thoton eiectricoiiy insuioting ioyer is odded on the second ioyer of the second moterioiwhich enforces the current from the sintering process to fiow only through the die ond not through the second loyer of the FGM-shope. (Fig. i)
Description
63883 METHOD OF PREPARATION OF A METAL / CEMENTED CARBIDE FUNCTiONAíLYGRADED MATERIAL Technical field [000l] The present invention relates generally to a method of preparation of ametal / cemented carbide, such as a steel / cemented tungsten carbide, functionally graded material shape by sintering, preferably by spark plasma sintering (SPS).
Background art
[0002] Previous attempts have been made to consolidate a steel / cementedtungsten carbide gradient component (as a complete tool without brazing) whichcan be used as a carbide tool in areas where components are exposed to excessivewear and shocks, such as cutting picks used in the mining industry, and weargraders in the road maintenance applications eg. snow plows and road cleaning,etc. Preferred materials to combine are for example steel and cemented tungsten carbide to offer a tough steel base with a hard and wear resistant carbide surface.
[0003] The common cemented carbide graded tools are usually fabricated bymaking tungsten carbide (WC, often referred to as hard metal) bi-Iayers withdifferent content of binder phase, such as cobalt (Co), and/or various tungstencarbide grain sizes and sinter-bonding them with steel. This process is metastableand the graded microstructure is very sensitive to the sintering conditions such assintering temperature, holding time and other factors. lt is usually difficult to make afinal material with a cobalt gradient because of the flow of liquid phase cobalt and its homogenization during sintering at high temperature.
[0004] An alternative is to make a gradient composition which changes from the steel base to the cemented carbide surface, i.e. a functionally graded material (FGM). 63883
[0005] A functionolly groded moteriol (FGM) is o moteriol design conceptwhich provides o (oining solution to relieve the residuol thermol stresses ond toincorporote incompotible properties of two dissimilor moteriols, such os the heot, theweor, ond the oxidotion resistance of o refroctory ceromic, such os for exomplecemented corbide, with the high toughness, the high strength, ond the mochinobilityof o metol, such os steel, by plocing groded composite interloyers of the two moteriols between the pure end loyers.
[0006] Generolly, in o metol / ceromic FGM system with o groded regionconsisting of severol composite loyers, there is o groduol voriotion of themicrostructure with the composition chonge. The motrix is reploced groduolly frommetol to ceromic, ond the microstructure profile vories concurrently from o puremetol, (ii) o metol-rich region (the ceromic porticles ore dispersed in metol motrices),(iii) intertwined composites (networks of metol ond ceromic phoses with comporoblevolume froctions), (iv) o ceromic-rich region (the metol motrix diminishes ond turns into discrete phoses or porticles in ceromic motrices), to finolly (v) o pure ceromic.
[0007] FGMs con be prepored through different techniques such os conventionolpowder metollurgy processing, vopour deposition ond sintering techniques. Thespork plosmo sintering method (SPS), olso referred to os for exomple field ossistedsintering technique (FAST), is o powerful sintering technique which ollows very ropidheoting under high mechonicol pressures. This process, hereofter referred to os SPS,hos proved to be very well suited for the production of functionolly grodedmoteriols. Other sintering techniques could possibly olso be used for preporing FGMs, such os for exomple direct hot-pressing, hot-pressing or hot isostotic pressing.
[0008] For moteriols such os steel / tungsten corbide, there is o difference in themoteriols' sintering temperotures. in this cose tungsten corbide hos the highersintering temperoture, opproximotely 200°C higher thon steel. lt is necessory to sinter the FGM component ot o proper temperoture ot which the whole component 63883 can be fully sintered. When sintering, especially when using spark plasma sintering,it is critical not to sinter steel or stainless steel alloys above around l000°Cotherwise melting occurs due to local overheating spots, which can reach atemperature close to the melting point of steel, i.e. =i 500°C. On the other hand, theappropriate sintering temperature of tungsten carbide by SPS is generally l00-200°C higher than this limit. The sintering temperature is influenced by the tungsten carbide grain size and the content of binder material.
[0009] One method of preparing a cemented carbide / steel PGM is described inpaperl lpn Soc Powder Powder Metall. Vol 47, No 5, pp. 564-568, 2000,wherein a Japanese group reported the preparation of cemented carbide / steelFGM using SPS by sinter bonding WC-Co bi-layers with a steel substrate. The FGMhad a gradient in WC grain size and cobalt composition. lt consisted of 3 layers:steel/WC-40Co/WC-25Co. The particle size of WC in the surface layer is coarserthan that in the middle layer and the end product was not fully dense. They have used the material in oil well drilling tools. [00l 0] At the 2002 international Conference on Functionally Graded Materials,NJ, D. K. Agrawal et al. presented a method of producing compositionally gradientsteel / tungsten carbide-cobalt-diamond FGM systems (steel / WC-25Codia FGM)by microwave heating. ln-situ hot pressing was needed to prevent mushrooming ofsintered samples. The outcome of the production process was fairly dense productdepending on the steel composition, the sintering temperature and the diamondcoating type. When using microwave heating, a special and expensive equipment has to be used. [00l l] ln US2007/02l49l 3 Al, the formation of various bi-layers WC-Co FGMby liquid phase sintering (iPS) is described. Because the liquid phase cobaltnormally homogenizes during sintering, a complex process of enriching/deficienting each layer with an element of for example carbon is used. The exact gradient 63883 composition will be a tunction ot the sintering time and temperature and the dimension ot the part to be made.
[OOl 2] Another way ot preparing a tungsten carbide / stainless steel FGM(Stainless steel / WC-25Co) by SPS is presented by Y. Kawakami et al. in SolidState Phenomena Voi l27, pp. l79-l 84, 2007. Here they tried to prepare thecompositionally gradient material by using a special shape graphite mold set (withupper thinner part and lower thicker part) to overcome the ditterence between thetwo sintering temperatures ot stainless steel and tungsten carbide. Even so, it washard to obtain a properly sintered body and the process is sensitive to the sintering temperature and the number ot graded layers.
[OOT 3] Theretore, there is a need tor a simple yet ettective production method torthe tabrication ot a metal / cemented carbide tunctionally graded material (preterably a steel/tungsten carbide FGM) that is highly dense and has no cracking.
Summary ot invention [OOT 4] An object ot the present invention is to prepare a metal / cementedcarbide tunctionally graded material by sintering, preterably by spark plasmasintering (SPS), in order to combine a tough metal base with a hard carbide surtacein an economical way. The tunctionally graded material can be a steel/cementedtungsten carbide (steel / WC-Co FGM). The end product is a tully densecompositionally gradient shape with pure metal and pure cemented carbide atloy astwo end surtaces (pure metal layer / x number ot composite layers / pure cemented carbide layer).
[OOiS] The term "cemented" means that the carbide alloy powder includes anamount ot metaltic binder, such as tor example cobalt, nickel, iron, or their alloys.During the sintering process, the tungsten carbide particles are captured in the metallic binder and cemented together by torming a metatlurgical bond. 63883 [OOi ó] The base layer can be o steel alloy, a stainless steel alloy or other metallic material.
[OOl 7] Thus, the invention relotes to a method of preporation of a FGM shapewith a first surface comprising up to lOO% of a first material and o second surfacecomprising up to 100% of o second material. The method is characterized in that it comprises the steps of: selecting the first moteriol with o first sintering temperature and o first meltingtemperature ond the second material with o second sintering temperature ond osecond melting temperature , wherein the first melting temperature is higher than the second melting temperature,loading o first layer of the first material in o sintering rnold referred to os die, adding at leost one intermediote layer on the first layer, the intermediote layercomprising o mix of the first ond second material creating on intermediote groded composite region, loading o second loyer of the second moteriol on the ot least one intermediote layer, adding on electricolly insulating layer on the second layer of the second material,adding o pressure on the loyers creating o FGM shope, ond sintering the whole shape under o predetermined time, pressure ond temperature.
[OOt 8] The loyers are preferably added os powders, but solid blocks of the pure moteriols ond composites con also be used.
[OOl 9] When using this method for creating a FGM-shape, the electricolly insulating layer added on the second material enforces the current from the sintering 63883 process to flow only through the die and not through the second layer of the hGM-shape. Thus, the temperature increase in the second layer becomes limited. Thetemperature in the first layer is high enough to sinter the first material but it does notexceed the melting temperature of the second material. The resulting end product from the process is a near fully dense FGM without any melted material.
[0020] in embodiments of the invention said first material is a cementedcarbide and said second material is a metal, preferably said first material is cemented tungsten carbide and said second material is steel. [002i] When using a cemented carbide, such as for example cementedtungsten carbide, and combining it with a metal, preferably steel, it is possible tocombine the high wear resistance of the carbide with the high toughness, the highstrength, and the machinability of the metal. Due to the different sintering andmelting temperatures of the respective materials, these materials are especially suitable to sinter using the above described inventive method.
[0022] ln another embodiment, the first material includes a metallic binder. The metallic binder may be cobalt and the amount of cobalt can be between 5 and 25wt%.
[0023] During the sintering process, the carbide particles are captured in themetallic binder and cemented together by forming a metallurgical bond. The result is a more dense FGM.
[0024] ln another embodiment, said electrically insulating layer is chosen fromany of the materials boron nitride, alumina, zirconia, silicon nitride, aluminum nitride, silica, magnesia.
[0025] All above mentioned materials are electrically insulating. When steel/cemented tungsten carbide FGM is sintered, the most preferred irisulating 63883 material is boron nitride. The insulating layer can either be a powder or a solid disc.
[0026] ln one embodiment ot the method, the sintering takes place under asintering temperature ot between 1000 °C and 1200 °C, preterably between1050°C and 1 150°C, more preterably between 1070 °C and 1 120°C and mostpreterably 1 100 °C, a pressure ot between 20 and 120 MPa, preterably between50 and 90 MPa, more preterably between 65 and 80 MPa and most preterably75 MPa, and a sintering time ot between 5 and 30 min, preterably between 10 and 20 min, more preterably 15 min.
[0027] ln one embodiment the shape is sintered using one ot the tollowingsintering techniques; spark plasma sintering [SPS] or direct hot pressing [DHP]Possible sintering techniques are also hot pressing (HP) or hot isostatic pressing (HIP). But preterably, spark plasma sintering [SPS] is used.
[0028] ln another embodiment, the sintering pressure is applied through two punches arranged on opposite sides ot the loaded material in the die.
[0029] ln one embodiment, the dies are lined with a graphite toil and this isalso inserted between the tirst and second surtace ot the FGM shape and the twopunches. ln another embodiment, the dies are graphite dies surrounded by graphite telt.
[0030] The graphite toil ensures good electric and thermal contacts betweenthe die and the punches and also tacilitates removal ot the sintered compact without damaging the die or punch surtaces.[0031] ln one embodiment ot the method, the method turther comprises the step: removing the electrically insulating layer atter the sintering process has been performed. 63883
[0032] Removal of the remains of the insuloting layer ofter sintering can beperformed through sand blasting or similar. The end product is a pure FGM ready to be manufactured into o cemented carbide tool.
[0033] All individual features of the above methods may be combined or exchanged unless such combination or exchange is clearly contradictory.
[0034] The sintering conditions, such as holding time and pressure, depend on the size of the FGM shape and the die dimension.
Brief description of drawinqs
[0035] The invention is now described, by way of example, with reference to the accompanying drawings, in which:Fig. l shows a longitudinal cross-section of a FGM die setup Table i lists the relative densities and the sintering conditions during sintering of individual steel and cemented carbide powders by SPS Table 2 lists the relative densities ond the sintering conditions during sintering of steel / WC~Co FGM compacts by SPS at l l00°C/75MPo/l Smin/SOCJC/min.
Description of embodiments
[0036] The invention will now be described in more detail in respect ofembodiments and in reference to the accompanying drawings. All examples hereinshould be seen as part of the general description and therefore possible to combinein any way in general terms. Again, individual features of the various embodimentsand methods may be combined or exchanged unless such combination or exchangeis clearly contradictory to the overall method of production of the functionally graded material shape. 63883
[0037] FIG. T shows o longitudinol cross-section of the die setup for producing oFGM-shope 4 occording to the invention. Powders of ot leost o first ond o secondmoteriol MT, M2 ore sintered under o pressure creoted by punches 3o, 3b in o dieT, preferobly o grophite die. The sintering process creotes sornples of the FGMshope 4, for exomple cylindricol-shoped discs. Other shopes including onypolygonol-shoped discs con olso be sintered. The sintering process is performed byspork plosmo sintering under o high temperoture ond pressure on the closed die tocreote o dense/neor fully dense FGM-shope. The powder loyers to be sintered conbe cold-pressed prior to the sintering. The sintering tokes preferobly ploce ot osintering temperoture of between T000 °C ond T200 °C, preferobly betweenT050°C ond T T50°C, more preferobly between T070 °C ond T T20°C ond mostpreferobly T T00 °C, o pressure of between 20 ond T20 MPo, preferobly between50 ond 90 MPo, more preferobly between 65 ond 80 MPo ond most preferobly 75MPo, ond o sintering time of between 5 ond 30 min, preferobly between T0 ond20 min, more preferobly TS min. Different sintering techniques con be used, suchos for exomple spork plosmo sintering (SPS) or direct hot pressing (DHP). Preferoblyspork plosmo sintering (SPS) is used. Other sintering techniques ore olso hot pressing (HP) or hot isostotic pressing (HIP).
[0038] The FGM shope hos o first Toyer lT with o first surfoce 4o comprisingup to T00% of the first moteriol MT ond o second loyer |2 with o second surfoce Abcomprising up to T00% of the second moteriol M2. Between the first Toyer TT of thefirst moteriol MT ond the second Toyer l2 of the second moteriol M2 ot leost onethird Toyer l3 comprising o mix of the first ond second moteriol MT, M2 is odded.The ot leost one third Toyer is creoting on intermediote groded composite region Tc.Preferobly the numbers of groded loyers ore between two ond ten, with o 50-T0vol% grodient chonge. However, other numbers of loyers ore of course olso possible, os is o non-lineor grodient chonge in composition. 63883
[0039] The first moteriol Ml hos o first sintering temperoture Tsl ond o firstmelting temperoture Tml ond the second moteriol M2 hos o second sinteringtemperoture Ts2 ond o second melting temperoture Tm2. The first meltingtemperoture Tml is higher thon the second rnelting temperature Tm2. Thus, in orderto ochieve o fully dense ?GM~shope, the sintering temperoture during the SPS-process needs to reoch the first sintering temperoture Tsl of the first moteriol but notexceed the second melting temperoture Tm2 of the second moteriol. Otherwise, this con leod to melting of the second moteriol M2.
[0040] in order to decreose the temperoture increose locolly in the secondmoteriol M2, on electricolly insuloting loyer 5 of on electricolly insuloting powder isploced on the second surfoce 4b of the FGM-shope 4, between the second loyer l2of the second moteriol M2 ond the grophite punch 3b. The function of theelectricolly insuloting powder is to enforce the current to flow only through the die ond not through the second loyer l2 of the tïGM-shope. [004l] The first moteriol Ml is preferobly o cemented corbide ond the secondmoteriol M2 o metol. More preferobly, the first moteriol Ml is cemented tungstencorbide ond the second moteriol M2 is steel. The first moteriol Ml includes o metollic binder such os for exomple cobolt Co or on iron-nickel olloy Fe-Ni.
[0042] The electricolly insuloting loyer con be chosen from ony of theelectricolly insuloting moteriols of boron nitride, olumino, zirconio, silicon nitride,oluminum nitride, silico, mognesio, but preferobly boron nitride BN is used. This moteriol con either be o powder or o solid disc.
[0043] The inner wolls of the dies l con be lined with thin grophite foil 2inserted between the shope 4 ond the two punches 3o, 3b. A grophite foil con olsobe inserted between the first ond second surfoce lo, lb of the FGM shope l ond the two punches (3o, 3b). The grophite foil 2 ensures good electric ond thermol 6388311 contacts between the die 1 and the punches 3a, 3b, and also facilitates removal of the sintered compact without damaging the die 1 or punch surfaces 3a, 3b.
[0044] The graphite dies 1 can be surrounded by graphite felt ó to reduce theheat loss by radiation from the outer die surface. The temperature can for example be measured at a hole 7 in the graphite die ó.
Examples
[0045] The present invention is further illustrated by the following experimentalresults, which should not limit the claims in any way. For example, other metals andcemented carbide powders than steel/cemented tungsten carbide can be used.
Other sintering techniques than SPS can also be used.
[0046] At the beginning, basic SPS experiments for single steel and tungstencarbide powders were carried out to find an optimum sintering condition at whichboth materials become highly dense. Fabrication of steel / cemented tungsten carbide FGM compacts was thereafter performed. Steel powders with low carboncontent and cemented tungsten powders of about 10wt% cobalt composition were used in the experiment.
[0047] For the tïGM gradient layers, the steel and tungsten carbide compositepowder mixtures were dry mixed at room temperature for one hour in plastic containers with tungsten carbide milling rods on a jar rolling mill.
[0048] The steel / WC-Co FGMs were designed to comprise four compositeinterlayers between the pure steel and tungsten carbide layers at the two ends. Thecomposites consisted of steel - cemented carbide mixtures with a 20vol% gradientchange (i.e. 80/20, 60/40, 40/60, 20/80 vol%). The total six layers were loadedin order, layer by layer, in a graphite die and a BN insulating layer was interposed between the punch and the steel layer. 6388312
[0049] A steel / cemented tungsten carbide FGM disc (ø20xó mm) wassuccessfully sintered according to the above conditions. lt was fully dense and no cracl discs of the sizes ø20x8.25 mm and øl 2x7.25 mm.[0050] The sintering was done in ordinary cylindrical graphite molds. [005l] During the sintering of single steel powders, the samples 4 weresintered with and without an electricolly insulating layer 5 of boron nitride powder BN placed between the steel powder to be sintered and the graphite punches 3a,3b.
[0052] The powders inside the closed dies were first cold-pressed. Then, thesamples were sintered in vacuum in a spark plasma sintering unit (SPS-5A0 MK-Vlsystem from SPS Syntex inc, Japan). Once the pre~determined SPS-pressure wasapplied, the dies were heated to 600 °C in 3 minutes and then heated further at arate of 50-] 00 °C/min to the desired holding temperature. The holding time wasbetween 5 and l5 minutes. The temperature was measured with an optical pyrometer focused on a hole 7 at the half height of the outer surface of the die.
[0053] After sintering, the resulting sintered discs were blasted to remove theresidues of graphite foil and BN layer, and then polished with #l 20 silicon carbidegrinding paper. The relative densities were measured by Archimedes method(European Standard EN 993-l) using deionized water as the immersion medium.The possible existence of surface cracks in the sintered pellets was examinedvisually and through optical microscopy (Olympus SZxl2 model, Olympus OpticalCo. Ltd, Japan).
[0054] The relative densities and the sintering conditions are listed in Tables l and 2, wherein Table l lists sintering of individual steel and cemented carbide 6388313 powders loy SPS ond Talole 2 lists sinteríng of steel / WC-Co FGM compacts loy SPSai l lOO°C/75Ml°a/l Smln/SOCJC/mln.
[0055] lïrom the results, it con be seen that when no BN insulation wos usedthe melting of steel occurred when the SPS temperature was l lOO°C which impliesthot the temperature was locally at the powder particle surfaces much higher thanthat measured on the die surface and very close to the melting point of the steelalloy (l 5ló°C). When BN was used, the current flow through the steel powder wasinhíbited, which prevented the local overheating and thus no meltíng wos observed.The tungsten carbide alloy was well denslfied at this sintering temperature of l lOO °C when a holding time of l5 minutes was applied under a pressure of 75 MPa.
[0056] The steel / WC~Co FGM compacts were properly sintered with high densities by the sintering process described above and no crocks were observed.
Claims (13)
1. i . A method of preporation of a FGM shape (4) with o first surface (4a)comprising up to iOO% of a first materiai (Mi) and a second surface (4ia) comprising up to iOO% of a second moterioi (M2), comprising the steps: (i) seiecting the first materiai (Mi) with o first sintering temperature (Tsi) anda first meiting temperature (Tmi) ond the second materiai (M2) with osecond sintering temperature (Ts2) ond a second meiting temperature(Tm2), wherein the first meiting temperature (Tmi) is higher than the second meiting temperature (Tm2), (ii) loading a first iayer (ii) of the first moterioi (Mi) in o sintering moid referred to as die (i), (iii) adding ot ieast one intermediate iayer (i3) on the first iayer (ii), theintermediate iayer (i3) comprising a mix of the first and second materia) (Mi, M2) creating an intermediate graded composite region (ic), (iv) loading o second iayer (i2) of the second moterioi (M2) on the ot ieast one intermediate iayer (i3) (v) adding an eiectricaiiy insuioting iayer (S) on the second iayer (i2) of the second material (M2),(vi) adding o pressure on the ioyers (ii-iS) creating a FGM shape (i), and (vii) sintering the whoie shape (i) under a predetermined time, pressure and temperature.
2. A method according to ciaim i, wherein said first material (Mi) is a cemented carbide and said second material (M2) is a metal. 63883
3. A method according to claim 2, wherein said tirst material (Mi) is cemented tungsten carbide and said second material (M2) is steel.
4. A method according to claim 2 or 3, wherein the tirst material (Mi) includes a metallic binder.
5. A method according to claim 4, wherein the metallic binder is cobalt (Co). ó.
6. A method according to claim 4, wherein the amount ot cobalt (Co) is between 5 and 25wt%.
7. A method according to any ot the above claims, wherein said electricallyinsulating layer is chosen trom any ot the materials baron nitride, alumina, zirconia, silicon nitride, aluminum nitride, silica, magnesia.
8. A method according to any ot the above claims, wherein the shape (l) issintered using one ot the following sintering techniques; spark plasma sintering (SPS) or direct hot pressing (DHP).
9. A method according to any ot the above claims, wherein the sinteringtakes place under a sintering temperature ot between lOOO °C and lZOO °C,preterably between lO50°C and l l50°C, more preterably between lO7O °C andl l20°C and most preterably l lOO °C, a pressure ot between 20 and l2O MPa,preterably between 50 and 90 MPa, more preterably between 65 and 80 MPaand most preterably 75 MPa, and a sintering time ot between 5 and 30 min, preterably between lO and 20 min, more preterably l5 min.
10. lO. A method according to any ot the above claims, wherein the sinteringpressure is applied by two punches (Sa, 3b) arranged on opposite sides ot the loaded material in the die. 6388316
11. 1 1. A method according to claim 9, wherein the dies (1) are lined with agraphite toil (2) also inserted between the first and second surface (1 a, 1b) ot the FGM shape (1) and the two punches (3a, 3b).
12. A method according to ctaim 9 or 10, wheretn the dies (1) are graphite dies surrounded by graphite telt
13. A method according to any ot the above ctaims, wherein the method further comprises the step: (viii) removing the ot etectrically insutating tayer (5) after the sintering process has been performed.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE1150254A SE535684C2 (en) | 2011-03-22 | 2011-03-22 | Method of producing a gradient component of metal / cemented carbide |
| PCT/SE2012/050303 WO2012128708A1 (en) | 2011-03-22 | 2012-03-20 | Method of preparation of a metal/cemented carbide functionally graded material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE1150254A SE535684C2 (en) | 2011-03-22 | 2011-03-22 | Method of producing a gradient component of metal / cemented carbide |
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| SE1150254A1 SE1150254A1 (en) | 2012-09-23 |
| SE535684C2 true SE535684C2 (en) | 2012-11-06 |
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| WO (1) | WO2012128708A1 (en) |
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| CN103182506B (en) * | 2013-03-29 | 2014-11-12 | 华南理工大学 | TiCp/M2 high-speed steel composite material and SPS (spark plasma sintering) preparation method thereof |
| ES2551980B1 (en) * | 2014-04-24 | 2016-11-03 | Universidad De Sevilla | Manufacturing procedure of advanced materials by concentration of electric current. |
| FR3030324B1 (en) * | 2014-12-17 | 2017-07-07 | Commissariat Energie Atomique | METHOD FOR MANUFACTURING A CONDUCTIVE LAYER ON A FACE OF A METAL PIECE BY SINTING BY UNIAXIAL COMPRESSION OF A POWDER |
| CN105081323A (en) * | 2015-09-16 | 2015-11-25 | 哈尔滨工业大学 | Method for preparing TiAl/Ti alloy laminated composite board through spark plasma sintering and pack hot rolling |
| CN106216674B (en) * | 2016-06-08 | 2018-04-24 | 四川大学 | W-V alloys functionally graded material and its discharge plasma sintering method |
| FR3060427A1 (en) * | 2016-12-21 | 2018-06-22 | Centre National De La Recherche Scientifique | PROCESS FOR PROCESSING SUPERDUR COMPOSITE MATERIAL FOR USE IN PRODUCING CUTTING TOOLS |
| US10926480B2 (en) * | 2017-09-05 | 2021-02-23 | The Boeing Company | Methods for manufacturing components having spatially graded properties |
| WO2019069701A1 (en) * | 2017-10-02 | 2019-04-11 | 日立金属株式会社 | Cemented carbide composite material, method for producing same, and cemented carbide tool |
| CN109755143A (en) * | 2017-11-01 | 2019-05-14 | 天津环鑫科技发展有限公司 | A kind of silicon slice alloy technique |
| CN110465670B (en) * | 2019-09-12 | 2022-03-04 | 哈尔滨工业大学 | Method for preparing layered composite material by spark plasma sintering |
| KR102376291B1 (en) * | 2020-03-19 | 2022-03-21 | 서울대학교산학협력단 | Methods of forming tungsten sintered body |
| FR3108919B1 (en) * | 2020-04-01 | 2022-04-08 | Commissariat Energie Atomique | Part made of a multilayer material with a composition gradient and its method of manufacture |
| EP4212266A1 (en) | 2022-01-14 | 2023-07-19 | Drill Holding ApS | Drill bit tip and drill with drill bit tip, mold and method for manufacturing drill bit tip |
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| US6124635A (en) * | 1997-03-21 | 2000-09-26 | Honda Giken Kogyo Kabushiki Kaisha | Functionally gradient integrated metal-ceramic member and semiconductor circuit substrate application thereof |
| US7763356B2 (en) * | 2006-03-13 | 2010-07-27 | United Technologies Corporation | Bond coating and thermal barrier compositions, processes for applying both, and their coated articles |
| JP2009129636A (en) * | 2007-11-21 | 2009-06-11 | Harison Toshiba Lighting Corp | Functionally gradient material, method for the same, and bulb |
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| SE1150254A1 (en) | 2012-09-23 |
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