EP1587772B1 - Procede de fabrication de pieces frittees poreuses - Google Patents
Procede de fabrication de pieces frittees poreuses Download PDFInfo
- Publication number
- EP1587772B1 EP1587772B1 EP04705030A EP04705030A EP1587772B1 EP 1587772 B1 EP1587772 B1 EP 1587772B1 EP 04705030 A EP04705030 A EP 04705030A EP 04705030 A EP04705030 A EP 04705030A EP 1587772 B1 EP1587772 B1 EP 1587772B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- molding composition
- foaming
- sintered
- blowing agent
- molding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 68
- 239000011148 porous material Substances 0.000 claims abstract description 45
- 239000011230 binding agent Substances 0.000 claims abstract description 38
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000000919 ceramic Substances 0.000 claims abstract description 14
- 230000001413 cellular effect Effects 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 229920006248 expandable polystyrene Polymers 0.000 claims abstract description 4
- 229920006327 polystyrene foam Polymers 0.000 claims abstract description 3
- 238000000465 moulding Methods 0.000 claims description 68
- 239000000203 mixture Substances 0.000 claims description 37
- 238000005187 foaming Methods 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 35
- 239000004604 Blowing Agent Substances 0.000 claims description 31
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 15
- 239000004793 Polystyrene Substances 0.000 claims description 13
- 229920002223 polystyrene Polymers 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 238000007493 shaping process Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 5
- 239000004952 Polyamide Substances 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000000197 pyrolysis Methods 0.000 claims description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 230000009969 flowable effect Effects 0.000 claims description 2
- 150000004678 hydrides Chemical class 0.000 claims description 2
- 238000010348 incorporation Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 150000004767 nitrides Chemical class 0.000 claims 1
- 229910000510 noble metal Inorganic materials 0.000 claims 1
- 239000008188 pellet Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 238000009757 thermoplastic moulding Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 22
- 239000011159 matrix material Substances 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- 239000011324 bead Substances 0.000 description 12
- 210000004027 cell Anatomy 0.000 description 7
- 239000012778 molding material Substances 0.000 description 7
- 229920001169 thermoplastic Polymers 0.000 description 7
- 239000004416 thermosoftening plastic Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000005755 formation reaction Methods 0.000 description 6
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- -1 polyoxyethylene Polymers 0.000 description 5
- 239000003380 propellant Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 239000004088 foaming agent Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 210000002421 cell wall Anatomy 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 229920006328 Styrofoam Polymers 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 239000008261 styrofoam Substances 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- IKOKHHBZFDFMJW-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-(2-morpholin-4-ylethoxy)pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)OCCN1CCOCC1 IKOKHHBZFDFMJW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical class OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000006262 metallic foam Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910000048 titanium hydride Inorganic materials 0.000 description 1
- 150000003613 toluenes Chemical class 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1125—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers involving a foaming process
-
- 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
Definitions
- the invention relates to a method for producing a cellular porous shaped sintered body with the manufacturing steps of preparing a thermoplastic flowable molding compound by mixing ceramic u / o metal powder with binder components and incorporation of organic blowing agents, converting the molding material into a molten state and introduction into a molding device, foaming the molding material by means of the blowing agent, solidification of the foamed molding composition, spreading of blowing agents and organic components and sintering of the thus treated molding.
- a ductile binder has to be added to the matrix powder, for example a ductile metal powder in hard metal production, in order to obtain products which can be pressed and sintered.
- a relatively recent technology for producing ceramic metallic sintered shaped bodies is the MIM (metal injection molding) process, in which the ceramic metallic matrix powder particles are mixed with organic binder components, and the mixture is usually brought into the desired shape in the thermoplastic state which solidifies molded part and then freed by pyrolysis u / o by dissolving and extracting its organic and / or inorganic binder components and finally sintered to form an approximately pore-free dense molded body.
- the shaping takes place alternatively for injection molding, for example by means of extrusion.
- Targeted pore structures in sintered bodies are created, for example, by mixing the matrix starting powders with a pulverulent placeholder, wherein the placeholder particles usually chemically before or during the sintering process from the molded composite material removed u / o removed by thermal decomposition and take their place free spaces, or pores. It is also known to produce pore structures in moldings by blowing in gases, for example argon or nitrogen gas, into a molten metal.
- gases for example argon or nitrogen gas
- sintered bodies having a pore structure are produced by introducing blowing agents as additives as homogeneously as possible into a matrix material mixed with thermoplastic binder and heating this composite or molding compound to the evaporation or foaming temperature of the blowing agent.
- blowing agents as additives as homogeneously as possible into a matrix material mixed with thermoplastic binder
- this composite or molding compound to the evaporation or foaming temperature of the blowing agent.
- bubble-shaped gas spaces are formed in the, or foam formations of the thermoplastic or molten molding material, which stabilize upon cooling and transfer of the molding compound into a solid state and then allow extraction of the gas inclusions or the remaining propellant leaving pores.
- the binder additives are extracted. The ready mechanical stabilization of the shaped body takes place by means of an additional sintering step.
- a useful foaming agent is an isocyanate-capped polyoxyethylene polyol, which eliminates the need for an additional binder. According to one embodiment, under 50% volume expansion is foamed.
- a disadvantage of this method is the use of water in conjunction with polyurethane or polyethylene binders, which allows the mass thus formed little thermoplastic properties and thus foaming in only a very limited volume. He comes to shrinkage after foaming.
- the practically controllable pore content in the sintered body is 10-20% by volume, which generally precludes the formation of cellular pore structures.
- the DE 177 15 20 A1 describes a method for producing ceramic masses by casting, with honeycomb structure in the mass inside and with a smooth surface, are stirred in the plastics with pearl structure in the tempered casting slurry and the molded body solidifies under cooling.
- Preferred plastic is blowing agent-containing polystyrene which has been prefoamed depending on the desired bead size.
- a disadvantage of this method is only unsatisfactory controllability of the bead distribution and arrangement in the casting slip, which is the use of the method with only moderate requirements for the mechanical minimum capacity of the cooled ceramic mass on the production of Shaped bodies with only low pore volume. The method does not provide for dispensing the polystyrene beads from the mass.
- the essential features of the process lie in the separate preparation of two different components of a molding composition, on the one hand as an aqueous solution containing the foaming or blowing agent in a resinous binder and on the other hand, as a metal powder and a water-soluble, resinous binder solution , which are both brought together just before the planned foaming process.
- the foaming step takes place in an atmosphere with at least 65% humidity.
- the water-soluble resin binder stabilizes the pores formed in the bulk during foaming during the foaming and subsequent drying.
- the water-soluble resin binder with temperature-dependent viscosity allows a suitable adjustment of the viscosity of the molding compound in adaptation to the individual production steps.
- methyl cellulose hydroxypropylmethyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, ammonium, ethyl celluslose and polyvinyl alcohol.
- volatilizable hydrocarbons having 5 to 8 carbon atoms in the hydrocarbon radical are cited as means for forming gas bubbles or pores in the molding compound, specifically pentanes, hexanes, octanes, benzene and toluenes.
- the foamable suspension may additionally contain organic plasticizers. A variety of oils, esters, glycerines and other organics are listed explicitly. The possible addition of specific means for stabilizing the foam state and the shaped microcells is provided.
- the EP 0 460 392 A1 describes a method of producing foamable metal bodies by the steps of manufacturing, mixing metal powder and gas releasing propellant powder into a molding composition, heat compacting the molding composition under conditions permitting bonding and mechanical strengthening of the metal powders by diffusion, thereby gas tightly enclosing the propellant and simultaneously decomposing the propellant prevent. Furthermore, the compacted molding compound is brought to such a high temperature in an open container or in a mold that the matrix metal melts and the blowing agent decomposes to foam the melt. Depending on the heating and cooling rate, as well as the foaming time at maximum temperature, foam bodies of different pore size and structure are achieved. Titanium hydride, aluminum hydroxide and sodium bicarbonate are mentioned as blowing agents.
- the object of the present invention is thus to provide an improved process for producing a highly porous metallic U / o ceramic sintered body by means of foaming a molding composition with the aid of a blowing agent.
- the method thus serves to produce highly porous sintered shaped bodies with a cellular pore structure, ie the shaped body has comparatively thin cell walls, measured on the volume of the pores formed by them.
- the finished sintered bodies have a solid sintered skeleton of the matrix materials metal u / o ceramic, free of additives, or only with insignificantly small residual amounts of such, the molding compound originally added additives. They have high mechanical strength.
- the sintered cell walls are largely free of microporosity, but can also be manufactured on request in microporous execution.
- the cell-like pores have a largely homogeneously uniform mean pore diameter of preferably 0.1 to 10 mm in the finished sintered body, in contrast to a microporosity that is regularly smaller by at least one order of magnitude, as known from sintering technology ,
- the pore volume in the sintered body is preferably 60-85 vol.%.
- Such high pore volume fractions are achievable only with strictly geometrically similar, for example honeycomb-like arrangement of the pores in the sintered shaped body.
- EPS expandable poly-styrene
- polystyrene blowing agent ie non-foamed polystyrene beads having a particle diameter of preferably 0.1 to 5 mm and containing as the blowing agent the volatile hydrocarbons pentane or hexane in a proportion of 1 to 8 % By weight.
- copolymers of the monomeric styrene with fractions of acrylic esters or acrylonitrile instead of the pure EPS polystyrene beads.
- the suitable combination of inventive blowing agent and matched thermoplastic binder components allows foaming of the molding composition up to comparatively very high pore volumes, measured on the known prior art.
- sintered shaped bodies with greater than 30% by volume up to more than 85% by volume of cell-forming pores are produced in the sintered shaped body.
- the plasticity of the molding material which is sufficient for foaming, is still present at significantly more than 50% by volume of metallic u / o ceramic matrix powder and correspondingly lower binder content in the prepared, unfoamed molding composition.
- High proportions of matrix powder favor the subsequent sintering to mechanically strong sintered molded body substantially or make this possible.
- Known methods aimed at achieving high pore volumes did not allow comparably favorable volume fractions in practice.
- both the binder components and the inflated polystyrene beads are predominantly discharged from the molding composition via a solution process in organic solvents, such as acetone or ethyl acetate.
- organic solvents such as acetone or ethyl acetate.
- the process according to the invention uses, as a preponderantly predominant binder component, already known high-polymer plastics, such as, for example, polyamides, which are insoluble in the abovementioned solvents customary for extraction.
- binder components used are plasticizers, surfactants and release agents that are as soluble in acetone and ethyl acetate at temperatures above 30 ° C as the polystyrene. These solvent-soluble additional components can lead to microporosity of the (still unsintered) cell walls and facilitate the application of solvent and solutes therein.
- the proportion of binder in the molding compound must be matched to the materials used in the molding compound and the process parameters for their processing. If this proportion is too high, it impairs the sintering together of the matrix powder during the subsequent sintering process. If the proportion is too low, the foamed molding composition falls below a minimum mechanical strength, which is indispensable for manipulability and further processing.
- the prepared molding material in a suitable shaping device is to be brought to a temperature suitable for volatilizing the blowing agents in the blowing agent, at the same time as the melting point of the molding compound.
- Foaming is all the more controlled and uniform the more evenly the polystyrene particles or EPS beads are distributed in the molding compound and the more homogeneous the temperature distribution in the molding compound.
- the process steps forming the molding compound and foaming can be carried out according to a number of different, previously practiced process.
- the shaping and foaming of the molding composition has proven particularly useful by known injection molding.
- Simply dimensioned shaped bodies such as plates, rounds or spheres, can be obtained by pressing a pulverulent EPS-containing molding compound Producing compacts and subsequent foaming with steam in a form perforated by slots economically.
- the compacts can optionally be laminated with a non-foamable surface layer in a subsequent powder pressing process. This will give you plates or discs with pore-free outer layer.
- the EPS is incorporated homogeneously into the molding compound melt at temperatures below 80 ° C. on a granulating extruder and the mass strands emerging from the perforated plate of the extruder are knocked off by means of so-called underwater granulation.
- underwater granulation In order not to have to accept premature gas losses from the EPS beads, it is expedient to carry out the underwater granulation under increased media pressure.
- Such EPS-containing molding compositions can be easily processed with the usual in plastics processing units to foamed molding compositions on.
- EPS-containing granules are introduced directly into a vapor-permeable mold and foamed at the same time, as happens to a large extent with prefoamed EPS balls in the packaging industry.
- this preferred method the production of large-scale and large-volume moldings is feasible.
- the molding material is brought in a screw or piston press on melting and foaming simultaneously and pressed under high pressure of, for example 10 6 to 10 8 Pascal by a shaping tool.
- the melt emerging from the mold increases its volume under foaming and is brought to a so-called calibration with simultaneous cooling in its enlarged shape to solidification and thus deducted steadily.
- the molding composition is cooled to prevent foaming after exiting the extrusion die under high pressure.
- the shaped mass is reheated, foamed in a volume increase adapted shape, cooled and treated according to the features of the invention.
- This process variant is used primarily for the production of highly porous, large-area sintered moldings with either open or closed cell structure.
- metallic and ceramic matrix materials is only in so far as a limitation, as they must be in the form of sinterable powder, a requirement whose implementation belongs to the knowledge of Pulvermetallurgen.
- Preferred ceramic matrix materials are the oxides of aluminum, silicon and zirconium, as well as silicon nitride and mixtures thereof.
- metallic matrix materials metals and alloys from the group Fe, Co, Ni, Cu, Ti, Ta, Mo, W and the precious metals, as well as metallic oxides, hydrides and hard metals have proven particularly useful.
- Sintered bodies produced by the process according to the invention have a wide field of application. The focus is on the application in the field of lightweight components and parts with relatively low thermal conductivity, as well as in the case of open-pored sintered moldings in the field of mechanical filters and catalysts.
- Example 1 describes the preparation of a porous chromium nickel steel sintered body.
- Water-atomized chromium nickel powder grade 316 L (Pamco, Japan, 90% particle size less than 15 microns) is in a kneading aggregate with binder components, composed of polyamide, plasticizer, wetting and release agent (the binder), in a weight ratio, 93 , 5% by weight of 316 L powder, 6.5% by weight of binder are thoroughly mixed and kneaded at about 100 ° C. until a low-viscosity melt is present.
- This mass is discharged from the kneading unit, solidified by cooling and ground to powder of a particle size smaller than 0.3 mm.
- 140 g of this powder are mixed with 13 g of EPS beads (Styrofoam P 656 from BASF, particle size 0.3 to 0.4 mm) in a laboratory mixer and at room temperature under a pressure of 200 bar to a powder compact of dimensions 60 x 90 x 7.2 mm 3 pressed.
- This compact is placed in a 20 mm high Al frame of dimensions 70 x 100 mm 2 , its top and bottom surfaces are covered with filter paper and fine mesh and then each with 6 mm thick Al plates, so that a closed, pressure-resistant and yet vapor permeable form arises.
- the vapor permeability is ensured by holes in the plates of 4 mm diameter and 3 mm spacing.
- the mold filled with compact is exposed for 4 minutes in a steam autoclave with steam at 120 ° C. under steam pressure of less than 0.7 bar. After cooling the autoclave to less than 100 ° C, the mold is removed and cooled to about 30 ° C under cold water.
- the molded article of dimensions 70 ⁇ 100 ⁇ 20 mm 3 inflated compact is removed after removal from the mold from the filter paper and dried for 2 h at 60 ° C. He loses 2.5 wt.% Of moisture. Thereafter, the molding is treated for 24 hours, resting on a perforated plate, in 50 ° C warm ethyl acetate as a solvent.
- the solvent-soluble and dissolved in it substances, already porous shaped body is removed from the bath and freed from the solution by means of vacuum distillation.
- the not yet extracted portion of polystyrene and binder components, above all polyamide in volatile form is removed from the molding by means of pyrolysis at 500 ° C.
- a sintered compact of dimensions 61.5 x 88 x 17.3 mm 3 and 130 g of weight is produced. This corresponds to a density of about 1.4 g / cm 3 or a pore volume of 82%.
- the average diameter of the largely uniformly sized pores, or cells in the sintered shaped body is about 0.60 mm.
- Example 2 describes the preparation of a porous Al 2 O 3 sintered body.
- a sinterable Al 2 O 3 powder of 3 microns average particle size and 99.80% purity (grade CT 3000 SG, Fa. ALCOA) in a kneading unit with binder components (polyamide, plasticizer, wetting and release agent) at 100 ° C. mixed thoroughly and kneaded until a low-viscosity melt is present.
- the weight fractions are 86.0% by weight of CT 3000 SG and 14.0% by weight of binder components.
- the kneaded mass is discharged from the kneading unit, cooled and ground into powder of a particle size smaller than 0.3 mm.
- the compact is processed to a foamed compact of dimensions 70 x 100 x 20 mm 3 and then stored for the extraction of soluble substances in ethyl acetate as a solvent.
- the molded article present after vacuum distillation is 62 g and has the unaltered dimensions of 70 ⁇ 100 ⁇ 20 mm 3.
- the weight loss compared to the weighing-in amounts at this point to 28 g, which corresponds to 89% of the theoretically extractable amount of substance of 31.5 g equivalent.
- the sintered compact After pyrolysis of the remaining portions of the polystyrene and the binder components at 500 ° C in air and sintering at 1550 ° C for 60 minutes, the sintered compact has the dimensions 60 x 86 x17 mm 3 and a weight of 56 g. This corresponds to a density of about 0.64 g / cm 3 , or a pore volume of 84%. The mean diameter of the macropores is 0.60 mm.
- the sintered body is mechanically stable or insensitive to breakage so that it can be manipulated and used without restrictive precautions with only a slight risk of damage.
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Abstract
Claims (15)
- Procédé de fabrication d'un corps moulé fritté cellulaire qui présente les étapes de fabrication consistant:à préparer une pâte de moulage fluide thermoplastique en mélangeant une poudre de céramique et/ou une poudre métallique avec des composants de liant et en y incorporant des agents organiques et/ou des agents minéraux de gonflement,à transférer la pâte de moulage à l'état fondu liquide et à l'amener dans un dispositif de moulage,à faire mousser la pâte de moulage à l'aide de l'agent de gonflement,à solidifier la pâte de moulage moussée,à extraire les agents de gonflement et les composants organiques età fritter le corps moulé ainsi traité,caractérisé en ce que
comme agent de gonflement, on utilise des particules de polystyrène expansible et en ce que l'étape de moussage s'effectue à une température comprise entre 80° et 130°C dans un moule en caisson dont l'espace permet la dilatation de la pâte de moulage pour former différentes particules de polystyrène moussées qui occupent dans la pâte de moulage une forme spatiale fermée respective et qui présentent une étroite répartition des diamètres. - Procédé selon la revendication 1, caractérisé en ce que l'on utilise des particules de polystyrène en forme de perles d'un diamètre moyen de 0,1 à 5 mm et à étroite dispersion des diamètres.
- Procédé selon les revendications 1 à 2, caractérisé en ce que l'on utilise comme agent de gonflement un copolymère dont les monomères sont le styrène et un ester d'acide acrylique ou l'acrylonitrile.
- Procédé selon les revendications 1 à 3, caractérisé en ce que l'on utilise du polystyrène doté de pentane ou d'hexane comme agent d'expansion.
- Procédé selon les revendications 1 à 4, caractérisé en ce que l'agent de gonflement est incorporé sous la forme d'un granulé solide non pré-expansé dans le mélange prévu pour la pâte de moulage.
- Procédé selon l'une des revendications 1 à 5, caractérisé en ce qu'à la pâte de moulage, on ajoute de plus, de façon séparée spatialement des particules de polystyrène expansibles, une petite proportion d'autres substances thermiquement instables et se dissociant en gaz pour former des micropores dans le corps moulé.
- Procédé selon les revendications 1 à 5, caractérisé en ce qu'à la pâte de moulage, on ajoute, en plus des particules de polystyrène et de façon spatialement séparée de celles-ci, des particules d'écartement qui sont chimiquement solubles ou se volatilisent par pyrolyse, pour former des micropores dans le corps moulé.
- Procédé selon les revendications 1 à 5, caractérisé en ce que lors du moussage, on forme une proportion en volume de pores de formation de cellules supérieure à 30 % et inférieure à 85 % par rapport au volume du corps moulé fritté.
- Procédé selon les revendications 1 à 8, caractérisé en ce que des pores de formation de cellules d'un diamètre moyen de 0,1 à 10 mm et d'une proportion en pores de 60 à 85 % en volume par rapport à leur état dans le corps moulé fritté sont formés.
- Procédé selon les revendications 1 à 9, caractérisé en ce que l'extraction d'agents de gonflement et de composants organiques s'effectue en les dissolvant dans des solvants organiques.
- Procédé selon les revendications 1 à 10, caractérisé en ce que l'extraction de l'agent de gonflement s'effectue par pyrolyse.
- Procédé selon les revendications 1 à 11, caractérisé en ce que l'opération de moulage et de moussage s'effectue après une opération d'extrusion.
- Procédé selon les revendications 1 à 12, caractérisé en ce que l'on introduit dans le mélange prévu pour former la pâte de moulage la poudre métallique sélectionnée dans l'ensemble constitué de Fe, Co, Ni, Cu, Ti, Ta, Mo, W et/ou les métaux précieux, sous la forme du métal pur, d'oxyde, de nitrure et/ou d'hydrure.
- Procédé selon les revendications 1 à 13, caractérisé en ce que la poudre métallique est introduite sous la forme d'un type de métal dur dans le mélange pour la pâte de moulage.
- Procédé selon les revendications 1 à 14, caractérisé en ce qu'on utilise un mélange de différents composants de liant dont la proportion pondérale prédominante est constituée de polyamide.
Applications Claiming Priority (3)
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AT422003U | 2003-01-30 | ||
AT0004203U AT6727U1 (de) | 2003-01-30 | 2003-01-30 | Verfahren zur herstellung poröser sinterformkörper |
PCT/AT2004/000025 WO2004067476A1 (fr) | 2003-01-30 | 2004-01-26 | Procede de fabrication de pieces frittees poreuses |
Publications (2)
Publication Number | Publication Date |
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EP1587772A1 EP1587772A1 (fr) | 2005-10-26 |
EP1587772B1 true EP1587772B1 (fr) | 2008-08-13 |
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EP04705030A Expired - Lifetime EP1587772B1 (fr) | 2003-01-30 | 2004-01-26 | Procede de fabrication de pieces frittees poreuses |
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US (1) | US20060118984A1 (fr) |
EP (1) | EP1587772B1 (fr) |
JP (1) | JP2006516678A (fr) |
AT (2) | AT6727U1 (fr) |
DE (1) | DE502004007830D1 (fr) |
WO (1) | WO2004067476A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102009040258A1 (de) | 2009-09-04 | 2011-03-24 | Jaeckel, Manfred, Dipl.-Ing. | Verfahren zur Herstellung eines zellularen Sinterformkörpers |
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AT6556U1 (de) * | 2003-02-20 | 2003-12-29 | Plansee Ag | Verfahren zum schäumen von sinterformkörpern mit zellstruktur |
AT9339U1 (de) * | 2006-07-06 | 2007-08-15 | Plansee Se | Verfahren zur herstellung eines extrudierten formkörpers |
US9447503B2 (en) * | 2007-05-30 | 2016-09-20 | United Technologies Corporation | Closed pore ceramic composite article |
EP2415543B1 (fr) * | 2009-03-30 | 2021-07-28 | Mitsubishi Materials Corporation | Procédé de production d'aluminium fritté poreux, et aluminium fritté poreux |
JP5402380B2 (ja) | 2009-03-30 | 2014-01-29 | 三菱マテリアル株式会社 | アルミニウム多孔質焼結体の製造方法 |
US20120087823A1 (en) * | 2009-06-02 | 2012-04-12 | Basf Se | Method for producing porous metal sintered molded bodies |
US9992917B2 (en) | 2014-03-10 | 2018-06-05 | Vulcan GMS | 3-D printing method for producing tungsten-based shielding parts |
US10590529B2 (en) * | 2015-11-20 | 2020-03-17 | Fourté International, Sdn. Bhd | Metal foams and methods of manufacture |
KR20180041343A (ko) * | 2016-10-14 | 2018-04-24 | 주식회사 엘지화학 | 금속합금폼의 제조 방법 |
US10822280B2 (en) * | 2017-12-15 | 2020-11-03 | Rolls-Royce High Temperature Composites Inc. | Method of making a fiber preform for ceramic matrix composite (CMC) fabrication utilizing a fugitive binder |
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CH494197A (de) * | 1965-05-26 | 1970-07-31 | Ohno Atsumi | Verfahren zur Herstellung eines porösen Sintermaterials und nach diesem Verfahren hergestelltes Sintermaterial |
US4517069A (en) * | 1982-07-09 | 1985-05-14 | Eltech Systems Corporation | Titanium and titanium hydride reticulates and method for making |
JPS61132572A (ja) * | 1984-11-29 | 1986-06-20 | 東京窯業株式会社 | 断熱レンガの製造方法 |
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JPS62158175A (ja) * | 1986-01-07 | 1987-07-14 | 住友大阪セメント株式会社 | 代替骨用多孔質セラミツク成形体およびその製造方法 |
JPH0784538B2 (ja) * | 1987-05-11 | 1995-09-13 | エヌオーケー株式会社 | 多孔質体の製造方法 |
DE3724156A1 (de) * | 1987-07-22 | 1989-02-02 | Norddeutsche Affinerie | Verfahren zum herstellen von metallischen oder keramischen hohlkugeln |
JPH01133989A (ja) * | 1987-11-19 | 1989-05-26 | Toshiba Ceramics Co Ltd | 多孔質セラミックスの製造法 |
DE4101630A1 (de) * | 1990-06-08 | 1991-12-12 | Fraunhofer Ges Forschung | Verfahren zur herstellung aufschaeumbarer metallkoerper und verwendung derselben |
JP2903738B2 (ja) * | 1991-02-22 | 1999-06-14 | ティーディーケイ株式会社 | 電波吸収体 |
US5213612A (en) * | 1991-10-17 | 1993-05-25 | General Electric Company | Method of forming porous bodies of molybdenum or tungsten |
US5830305A (en) * | 1992-08-11 | 1998-11-03 | E. Khashoggi Industries, Llc | Methods of molding articles having an inorganically filled organic polymer matrix |
US5506046A (en) * | 1992-08-11 | 1996-04-09 | E. Khashoggi Industries | Articles of manufacture fashioned from sheets having a highly inorganically filled organic polymer matrix |
JPH07130528A (ja) * | 1993-10-29 | 1995-05-19 | Tokin Corp | 多孔質軟磁性フェライト焼結体の製造方法 |
JPH07291759A (ja) * | 1994-04-27 | 1995-11-07 | Ngk Spark Plug Co Ltd | 多孔質セラミックスの製造方法 |
DE19648926C1 (de) * | 1996-11-26 | 1998-01-15 | Manfred Dipl Ing Jaeckel | Offenporige Polyamid gebundene Formkörper aus keramischen oder metallischen Pulvern |
US6210612B1 (en) * | 1997-03-31 | 2001-04-03 | Pouvair Corporation | Method for the manufacture of porous ceramic articles |
FR2780406B1 (fr) * | 1998-06-29 | 2000-08-25 | Bp Chem Int Ltd | Composition de polystyrene expansible, procede de preparation de la composition et materiaux expanses resultant de la composition |
US6759004B1 (en) * | 1999-07-20 | 2004-07-06 | Southco, Inc. | Process for forming microporous metal parts |
RU2185350C2 (ru) * | 2000-06-15 | 2002-07-20 | Российский химико-технологический университет им. Д.И. Менделеева | Способ получения керамических изделий |
JP4572287B2 (ja) * | 2001-03-23 | 2010-11-04 | 独立行政法人産業技術総合研究所 | 高強度多孔質体の製造方法及び高強度多孔質体 |
-
2003
- 2003-01-30 AT AT0004203U patent/AT6727U1/de not_active IP Right Cessation
-
2004
- 2004-01-26 DE DE502004007830T patent/DE502004007830D1/de not_active Expired - Lifetime
- 2004-01-26 AT AT04705030T patent/ATE404506T1/de not_active IP Right Cessation
- 2004-01-26 JP JP2006501335A patent/JP2006516678A/ja active Pending
- 2004-01-26 EP EP04705030A patent/EP1587772B1/fr not_active Expired - Lifetime
- 2004-01-26 US US10/543,933 patent/US20060118984A1/en not_active Abandoned
- 2004-01-26 WO PCT/AT2004/000025 patent/WO2004067476A1/fr active IP Right Grant
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102009040258A1 (de) | 2009-09-04 | 2011-03-24 | Jaeckel, Manfred, Dipl.-Ing. | Verfahren zur Herstellung eines zellularen Sinterformkörpers |
EP2679564A1 (fr) | 2009-09-04 | 2014-01-01 | Manfred Jaeckel | Procédé pour la fabrication d'un élément à structure alvéolaire en céramique |
Also Published As
Publication number | Publication date |
---|---|
ATE404506T1 (de) | 2008-08-15 |
US20060118984A1 (en) | 2006-06-08 |
JP2006516678A (ja) | 2006-07-06 |
DE502004007830D1 (de) | 2008-09-25 |
AT6727U1 (de) | 2004-03-25 |
WO2004067476A1 (fr) | 2004-08-12 |
EP1587772A1 (fr) | 2005-10-26 |
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