EP1587772B1 - Verfahren zur herstellung poröser sinterformkörper - Google Patents

Verfahren zur herstellung poröser sinterformkörper Download PDF

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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
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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
Application number
EP04705030A
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German (de)
English (en)
French (fr)
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EP1587772A1 (de
Inventor
Jörg FÄRBER
Manfred Jaeckel
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Plansee SE
Original Assignee
Plansee SE
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Publication date
Application filed by Plansee SE filed Critical Plansee SE
Publication of EP1587772A1 publication Critical patent/EP1587772A1/de
Application granted granted Critical
Publication of EP1587772B1 publication Critical patent/EP1587772B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)
EP04705030A 2003-01-30 2004-01-26 Verfahren zur herstellung poröser sinterformkörper Expired - Lifetime EP1587772B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT422003U 2003-01-30
AT0004203U AT6727U1 (de) 2003-01-30 2003-01-30 Verfahren zur herstellung poröser sinterformkörper
PCT/AT2004/000025 WO2004067476A1 (de) 2003-01-30 2004-01-26 Verfahren zur herstellung poröser sinterformkörper

Publications (2)

Publication Number Publication Date
EP1587772A1 EP1587772A1 (de) 2005-10-26
EP1587772B1 true EP1587772B1 (de) 2008-08-13

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EP04705030A Expired - Lifetime EP1587772B1 (de) 2003-01-30 2004-01-26 Verfahren zur herstellung poröser sinterformkörper

Country Status (6)

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US (1) US20060118984A1 (ja)
EP (1) EP1587772B1 (ja)
JP (1) JP2006516678A (ja)
AT (2) AT6727U1 (ja)
DE (1) DE502004007830D1 (ja)
WO (1) WO2004067476A1 (ja)

Cited By (1)

* Cited by examiner, † Cited by third party
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
CN102438778B (zh) * 2009-03-30 2014-10-29 三菱综合材料株式会社 铝多孔烧结体的制造方法和铝多孔烧结体
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
JP5763055B2 (ja) * 2009-06-02 2015-08-12 ビーエーエスエフ ソシエタス・ヨーロピアＢａｓｆ Ｓｅ 多孔性の金属焼結成形体の製造方法
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
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Cited By (2)

* Cited by examiner, † Cited by third party
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 (de) 2009-09-04 2014-01-01 Manfred Jaeckel Verfahren zur Herstellung eines zellularen Sinterformkörpers

Also Published As

Publication number Publication date
DE502004007830D1 (de) 2008-09-25
ATE404506T1 (de) 2008-08-15
EP1587772A1 (de) 2005-10-26
US20060118984A1 (en) 2006-06-08
WO2004067476A1 (de) 2004-08-12
AT6727U1 (de) 2004-03-25
JP2006516678A (ja) 2006-07-06

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