JPS63264303A - Cast-molding of powder - Google Patents
Cast-molding of powderInfo
- Publication number
- JPS63264303A JPS63264303A JP9753387A JP9753387A JPS63264303A JP S63264303 A JPS63264303 A JP S63264303A JP 9753387 A JP9753387 A JP 9753387A JP 9753387 A JP9753387 A JP 9753387A JP S63264303 A JPS63264303 A JP S63264303A
- Authority
- JP
- Japan
- Prior art keywords
- slurry
- tank
- monochlorotrifluoromethane
- powder
- compact
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 238000000465 moulding Methods 0.000 title description 7
- 239000002002 slurry Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 12
- AFYPFACVUDMOHA-UHFFFAOYSA-N chlorotrifluoromethane Chemical compound FC(F)(F)Cl AFYPFACVUDMOHA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002612 dispersion medium Substances 0.000 claims description 16
- 238000005266 casting Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 5
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- -1 Alternatively Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- SLGOCMATMKJJCE-UHFFFAOYSA-N 1,1,1,2-tetrachloro-2,2-difluoroethane Chemical compound FC(F)(Cl)C(Cl)(Cl)Cl SLGOCMATMKJJCE-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 2
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 2
- 239000011225 non-oxide ceramic Substances 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011505 plaster Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 description 1
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 1
- BTXXTMOWISPQSJ-UHFFFAOYSA-N 4,4,4-trifluorobutan-2-one Chemical compound CC(=O)CC(F)(F)F BTXXTMOWISPQSJ-UHFFFAOYSA-N 0.000 description 1
- BQACOLQNOUYJCE-FYZZASKESA-N Abietic acid Natural products CC(C)C1=CC2=CC[C@]3(C)[C@](C)(CCC[C@@]3(C)C(=O)O)[C@H]2CC1 BQACOLQNOUYJCE-FYZZASKESA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- 229920001875 Ebonite Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229910039444 MoC Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001347 Stellite Inorganic materials 0.000 description 1
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 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
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 125000006487 butyl benzyl group Chemical group 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- AHICWQREWHDHHF-UHFFFAOYSA-N chromium;cobalt;iron;manganese;methane;molybdenum;nickel;silicon;tungsten Chemical compound C.[Si].[Cr].[Mn].[Fe].[Co].[Ni].[Mo].[W] AHICWQREWHDHHF-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007582 slurry-cast process Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Producing Shaped Articles From Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、金属粉またはセラミック粉を液状分散媒に
分散させてスラリーとし、このスラリーを鋳込み成形し
たのち、残留する分散媒を超臨界のモノクロロトリフル
オロメタンで抽出除去する方法に関するものである。[Detailed Description of the Invention] [Field of Industrial Application] This invention involves dispersing metal powder or ceramic powder in a liquid dispersion medium to form a slurry, casting the slurry, and then converting the remaining dispersion medium into a supercritical solution. This relates to a method of extracting and removing with monochlorotrifluoromethane.
例えば２％Ｎ ｉ −９８％Ｆｅ粉、５ＵＳ３１６粉、
あるいは、ステライト粉などの金属粉、例えばアルミナ
、炭化ケイ素、窒化ケイ素、ジルコニア、炭化モリブデ
ン、炭・化チタンなどのセラミック粉、例えば炭化クン
ゲステン−コバルト、炭化チクンーニッケルなどのセラ
ミックと金属の混合粉などから成形体を得る方法として
鋳込み形成法がある。For example, 2% Ni-98% Fe powder, 5US316 powder,
Alternatively, metal powder such as stellite powder, ceramic powder such as alumina, silicon carbide, silicon nitride, zirconia, molybdenum carbide, titanium carbide, etc., mixed powder of ceramic and metal such as Kungesten-cobalt carbide, chikune-nickel carbide, etc. There is a casting method as a method of obtaining a molded body from such methods.
この方法は、原料粉体を液状分散媒に分散させてスラリ
ーを形成し、このスラリーをあらかじめ、離型剤塗布な
どの型処理を施した石膏型を型組みして形成した吸液性
の鋳型に流し込み、分散媒の一部を鋳型に吸収させるこ
とによって型面ζζ沿って着内層を形成させ、時間の経
過と共にこれ、を成長させて成形強度を確保し、脱型後
に分散媒を加熱除去して成形体を得るものである。In this method, raw material powder is dispersed in a liquid dispersion medium to form a slurry, and this slurry is molded into a liquid-absorbing mold that is formed by molding a plaster mold that has been treated with a mold release agent and other mold treatments. A part of the dispersion medium is absorbed into the mold to form an inner layer along the mold surface ζζ, which grows over time to ensure molding strength, and after demolding, the dispersion medium is removed by heating. A molded body is obtained by doing this.
前述の型の吸水現象は、継続的に行われるので、着肉層
中の水分は徐々に減少し、それに伴って鋳込み体は硬さ
を増すと共に収縮して型から離れろようになる。Since the above-mentioned water absorption phenomenon of the mold occurs continuously, the water content in the ink layer gradually decreases, and accordingly, the cast body increases in hardness, contracts, and becomes detached from the mold.
乙のような階段に到達したら、幼込み体を脱型し、必要
に応じて生加工ののち乾燥させるのであるが、同時に、
吸水した石膏も屹煙して繰返１７（史用に供するように
している。Once the stage like Otsu is reached, the immature body is demolded, and if necessary, it is processed raw and then dried, but at the same time,
The gypsum that absorbed water also smoked and was used repeatedly (17) for historical purposes.
とこて（重用する原料粉体け、例えば、水と少量の分散
剤などからなる分散媒とＯｔせてボールミルなどで粉砕
混合することによってスラリーとしているが、安定した
スラリーとするためにはこの混合操作に数日間にわたる
攪拌を行い、水分量、粘性を調節したのち真空脱泡して
７４ている。Slurry is made by grinding and mixing important raw material powders with a dispersion medium such as water and a small amount of dispersant in a ball mill, etc. In order to make a stable slurry, it is necessary to After stirring for several days and adjusting the water content and viscosity, the mixture was degassed under vacuum.
このような製造方法において、使用する分散媒としては
、各種のアルコールを使用！、 １’Ｊることが知られ
ている。In this manufacturing method, various alcohols are used as the dispersion medium! , 1'J is known.
また、型材としては、石膏の代わりに機械的強度や耐ｇ
耗性に擾れているプラスチック、金属−ヒラミック、繊
維複合材料、炭化ケイ素などのセラミックなどからなろ
吸液性鋳型を使用することも知られている。Also, as a mold material, it can be used instead of plaster for mechanical strength and g-resistance.
It is also known to use absorbent molds made of abrasive plastics, metal ceramics, fiber composites, ceramics such as silicon carbide, and the like.
ところが、このように従来使用されている金属粉あるい
はセラミック粉を使用した鋳込成形法には次に示す如き
問題点があった。However, the conventional casting method using metal powder or ceramic powder has the following problems.
（１）鋳込みから脱型までの工程に長時間を要する。(1) The process from casting to demolding takes a long time.
その所要時間は、目的とする成形体の形状、寸法などに
より異なり鋼環には言えないが、例えば、１２ＩＩＶＩ
Ｉφ×２０Ｍの円筒形状の物体をアルミナの水系スラリ
ーの鋳込み形成により１ｑる場合、およそ８時間を要す
る。The time required varies depending on the shape and dimensions of the target molded product, and cannot be said for steel rings, but for example, 12IIVI
It takes about 8 hours to form a cylindrical object of Iφ×20M by casting 1q of alumina aqueous slurry.
（２）成形体の乾燥工程に長時間を要する。(2) It takes a long time to dry the molded body.
例えば、上述の成形体を成形したのち、これを大気乾燥
に処すると、およそ２４時間を要する。For example, if the above-mentioned molded article is molded and then subjected to air drying, it will take approximately 24 hours.
（３）鋳型の乾燥工程が必要である。(3) A mold drying process is required.
この工程には、長時間を要することから、生産性が低下
し、可能であるならば省略できるようなタイプのものと
したい。Since this process requires a long time, it reduces productivity, and if possible, it is desirable to use a type that can be omitted.
（４）乾燥工程において、成形体に歪みゃ亀裂が発生し
やすい。(4) In the drying process, distortion and cracks are likely to occur in the molded body.
これは、分散媒が成形体表面から蒸発する際に、成形体
内に空孔を形成するが、この中の気液表面、気固液接触
点などｔζおいて、毛細管現１による力が働き、隣りあ
う粒子同志を引き寄せる作用を行い、乙の現家により表
層部から収縮が進行して、成形体に歪や亀裂を発生させ
るか、発生させやすくなる。This is because when the dispersion medium evaporates from the surface of the molded object, pores are formed inside the molded object, and at points tζ such as the gas-liquid surface and the gas-solid-liquid contact point, the force due to the capillary current 1 acts. It has the effect of attracting adjacent particles to each other, and shrinkage progresses from the surface layer due to the presence of particles, causing distortion and cracks to occur in the molded product, or making them more likely to occur.
このような問題点を解決するために、本出願人は、金属
粉あるいはセラミック粉を、液体または超臨界の二酸化
炭素によって抽出可能であってかつ融点が０〜１００℃
の物質を主要成分とする分散媒に分散させてスラリーと
し、このスラリーを非吸液性の鋳型に鋳込むと共に冷却
して凍結固化させて成形体としてから脱型し、ついで、
液体または超臨界の二酸化炭素により成形体中の分散媒
の主要部分を抽出除去する、方法を出願したく特願昭６
１−２３８６３号）。In order to solve these problems, the applicant has developed a metal powder or ceramic powder that can be extracted with liquid or supercritical carbon dioxide and has a melting point of 0 to 100°C.
This substance is dispersed in a dispersion medium as a main component to form a slurry, and this slurry is cast into a non-liquid-absorbing mold and cooled to freeze and solidify to form a molded body, which is then demolded.
A patent application was filed in 1983 for a method for extracting and removing the main part of the dispersion medium in a molded body using liquid or supercritical carbon dioxide.
1-23863).
この方法によれば、成形時間を従来の８時間から１分間
に短縮し、かつ２４時間かかる鋳型の乾燥工程を省くこ
とができ、また、成形体に歪、亀裂などの発生を防止し
得るという極めて優れた方法であった。According to this method, the molding time can be shortened from the conventional 8 hours to 1 minute, the mold drying process that takes 24 hours can be omitted, and it is possible to prevent the occurrence of distortions, cracks, etc. in the molded product. It was an extremely excellent method.
ところが、このように改善が図られた成形方法ではあっ
たが、次に示すような問題点については、未だ改善の余
地が残されているものであった。However, although the molding method has been improved in this way, there is still room for improvement regarding the following problems.
すなわち、窒化物、炭化化物、ホウ化物等の非酸化物セ
ラミック粉、あるいは金属粉を使用したｊＡ合には、高
圧の二酸化炭素との接触によりその表面の酸化が進行す
る可能性があり、表面に酸化膜の被膜が形成すると、非
酸化化物セラミック粉の場合には焼結体の高温時の機械
的強度の低下を招き、また、金属粉の場合には焼結性を
阻害するようになることが認められた。In other words, when non-oxide ceramic powder such as nitride, carbide, or boride, or metal powder is used, oxidation of the surface may proceed due to contact with high-pressure carbon dioxide. When an oxide film is formed on a non-oxide ceramic powder, it causes a decrease in the mechanical strength of the sintered body at high temperatures, and in the case of a metal powder, it impedes sinterability. This was recognized.
従って、二酸化炭素に変わる粉体の表面酸化の恐れのな
い物質を抽出剤として選択することが望まれていた。Therefore, it has been desired to select a substance as an extractant that has no fear of oxidizing the surface of the powder in exchange for carbon dioxide.
ＣＩ？ｆｆ題点を照点するための手段〕本発明は、前述
のような従来のスラリー鋳込み成形技術をさらに改善す
ることについて種々検討を加えた結果到達したものであ
って、金属粉あるいはセラミック粉のスラリーを鋳込み
形成した後、分子ｌｌ＆ 媒を超臨界のモノクロロトリ
フルオロメタンで抽出除去することを特徴とする金属粉
あるいはセラミック粉の成形方法、に関するものである
。CI? ff Means for addressing the problem] The present invention was arrived at as a result of various studies to further improve the conventional slurry casting technology as described above. The present invention relates to a method for molding metal powder or ceramic powder, which comprises casting a slurry and then extracting and removing the molecules and the medium with supercritical monochlorotrifluoromethane.
本発明方法では、３９気圧の臨界圧以上のモノクロロ１
゛リフルオロメタンによって抽出可能であって、かつ融
点がＯ℃〜１００℃の物質を分散剤として用いる。In the method of the present invention, monochloro 1
A substance which is extractable by difluoromethane and has a melting point of 0° C. to 100° C. is used as a dispersant.
このような物質としては、例えば、炭酸メチル（融点０
．５℃）、ｔ−ブチルアルコール（同、２５．６℃）、
テトラクロロジフルオロエタン（同、２６℃）、ステア
リルアルコール（同１５９℃）、ステアリン酸（同、７
０．１℃）など数多くの物質がある。Examples of such substances include methyl carbonate (melting point 0
．． 5°C), t-butyl alcohol (25.6°C),
Tetrachlorodifluoroethane (26℃), stearyl alcohol (159℃), stearic acid (7℃)
There are many substances such as 0.1℃).
本発明方法において、融点の低すぎろ物質を使用すると
、スラリーの凍結固化のための低温冷媒の製造設備が大
川りとなり好ましくないし、逆に融点が高すぎると設備
を停止したときにスラリーが固着し清掃が容易でないな
どの不都合な現象を見せはじめるので好ましくなく、融
点の範囲をθ℃〜１００℃とすることが好ましい。In the method of the present invention, if a filter material with a melting point that is too low is used, the production equipment for the low-temperature refrigerant for freezing and solidifying the slurry will become overcrowded, which is undesirable.On the other hand, if the melting point is too high, the slurry will stick when the equipment is stopped. However, this is not preferable because it starts to exhibit inconvenient phenomena such as difficulty in cleaning, so it is preferable that the melting point range is θ°C to 100°C.
また、本発明では、特願昭６１−３２８６３号における
二酸化炭素の代わりに、モノクロロトリフルオロメタン
を分散媒抽出剤として（ｅｍするが、乙のものは、炭素
、塩素およびフッ素からなる安定な化合物であることか
ら、金属あるいはセラミックの表面を酸化させるおそれ
ば皆無となった。In addition, in the present invention, monochlorotrifluoromethane is used as a dispersion medium extractant (em) instead of carbon dioxide in Japanese Patent Application No. 61-32863. Because of this, there is no risk of oxidizing the metal or ceramic surface.
これを使用することにより従来技術の問題点を解決しう
るのである。By using this, the problems of the prior art can be solved.
非吸液性の鋳型に鋳込む直前のスラリーの粘度が所定の
値より低いと、Ｐｉ雑形状の鋳型への鋳込みは容易であ
るが、固液分離が生じ易く、かつ、分散媒除去後に成形
体が崩れ易くなるという自体を生じやす（、従って、粘
度は５０センチポイズ以上とすることが望ましい。If the viscosity of the slurry immediately before being poured into a non-liquid-absorbing mold is lower than a predetermined value, it will be easy to cast into a Pi miscellaneous-shaped mold, but solid-liquid separation will likely occur, and molding will be difficult after removing the dispersion medium. This tends to cause the body to collapse easily (therefore, it is desirable that the viscosity be 50 centipoise or higher).
一方高粘度であり過ぎろと、逆に固液分離は起きにくく
なるが、流動性が低下し複雑な形状の鋳型への幼込みが
困難となる。従って粘度は１０４センチボイズ以下であ
ることが望ましい。On the other hand, if the viscosity is too high, solid-liquid separation will be less likely to occur, but the fluidity will decrease and it will be difficult to fill molds with complex shapes. Therefore, it is desirable that the viscosity be 104 centivoise or less.
非吸液性の鋳型は外部雰囲気冷却であってもよいし、あ
るいは内部に冷却媒体の回路を有するものであってもよ
い。The non-liquid-absorbing mold may be externally cooled or may have an internal cooling medium circuit.
鋳型の材料として工具鋼のほか木、硬質ゴム、アルミニ
ウム、ステンレス清等の安価な材料が適用できる。In addition to tool steel, inexpensive materials such as wood, hard rubber, aluminum, and stainless steel can be used as the mold material.
スラリーの流動性の改善、および分散媒の主要部分を抽
出除去後の成形体にハンドリングに耐えろ強度を付与す
るために、前述のモノクロロトリフルオロメタンによっ
て抽出可能な物質に結合剤、可塑剤、分散剤、湿潤剤、
滑剤などを適宜添加してもよい。In order to improve the fluidity of the slurry and to impart handling strength to the molded product after the main portion of the dispersion medium has been extracted and removed, binders, plasticizers, and dispersants are added to the substances extractable by monochlorotrifluoromethane. , wetting agent,
A lubricant or the like may be added as appropriate.
結合剤としては、セルロースアセテ−１、ブチリレート
、二１・ロセルロース、石油レジン、ポリエチレン、ポ
リアクリル酸エステル、ポリメチルメククリレ−１・、
ポリビニルアルコール、ポリビニルブチラール、塩化ビ
ニル、ポリメタクリル酸エステル、エチルセルロース、
アビエチン酸レジン等が使用できる。As a binder, cellulose acetate-1, butyrate, 21-cellulose, petroleum resin, polyethylene, polyacrylic acid ester, polymethyl meccrylate-1,
Polyvinyl alcohol, polyvinyl butyral, vinyl chloride, polymethacrylate, ethyl cellulose,
Abietic acid resin etc. can be used.
可塑剤としては、プチルベンジルフクレート、ジブチル
フタレ−１・、プチルフタレ−１・、ジメチルツクし一
−１−１．メチルアジテート、フタル酸エステルの混合
物、ポリエチレングリコールの誘導体、トリクレゾール
フォスフニー１・などを使用ずろことができる。Examples of the plasticizer include butylbenzyl fucrate, dibutyl phthalate-1., butyl phthalate-1., dimethyl phthalate-1-1. Methyl agitate, mixtures of phthalate esters, derivatives of polyethylene glycol, tricresol phosphamide 1, etc. can be used.
分散剤としては、グリセリントリオレエ−１・、天然魚
油、合成界面活性剤、ベンゼンスルフォン酸、オレイン
酸、メチルオフクジエン等が使用できる。As the dispersant, glycerol trioleate-1., natural fish oil, synthetic surfactant, benzenesulfonic acid, oleic acid, methylofcudiene, etc. can be used.
さらに、瀾潤剤としては、アルキルアリルポリエーテル
アルコール、ポリエチレングリコールの工千ルエーテル
、エチルフェニルグリコール、ポリオキシエチレンエス
テル、グリセリンのモノオレエート、アルコール類等が
使用できろ。Further, as a moistening agent, alkylaryl polyether alcohol, polyethylene glycol ether, ethyl phenyl glycol, polyoxyethylene ester, glycerin monooleate, alcohols, etc. can be used.
滑剤としては、ステアリン酸、ステアリルアルコール等
が１史用できる。As the lubricant, stearic acid, stearyl alcohol, etc. can be used.
マｈ 、抽出操作時のモノクロロトリフルオロメタンの
圧力は、該油剤に溶解能力を持たせろためには少なくと
も臨界圧３９気圧以上とする必要があり、この抽出操作
においては過大な圧力下は抽出効率を増すことなくいた
ずらにエネルギーの浪費となることから、その上限はお
よそ５００気圧、通常は３００気圧程度とすることによ
り好ましい結果が得られやすい。Mah, the pressure of monochlorotrifluoromethane during the extraction operation must be at least 39 atmospheres or higher, which is the critical pressure, in order to give the oil a dissolving ability. Since energy is wasted unnecessarily without increasing the pressure, preferable results are likely to be obtained by setting the upper limit to about 500 atm, usually about 300 atm.
固液が分離しない範囲でスラリーを加圧し鋳型に注入す
ることは、高粘度で粉体濃度の高い、従って除去の必要
な分散媒量の低いスラリーには極めて効果的であること
を示１７なが、通常達成しうろ４０〜７５容積％の範囲
では１０ ｋｇ ／ ｃＪ以下の加圧が、固液分離防止
の観点から望ましい。It has been shown that pressurizing the slurry and injecting it into the mold without solid-liquid separation is extremely effective for slurries with high viscosity and high powder concentration, and therefore with a low amount of dispersion medium that needs to be removed17. However, in the range of 40 to 75% by volume, which is normally achieved, pressurization of 10 kg/cJ or less is desirable from the viewpoint of preventing solid-liquid separation.
〔発明の実施例］
下記の手順で窒化ケイ素粉（Ｓｉ３Ｎ４）のスラリーを
調製した。[Example of the Invention] A slurry of silicon nitride powder (Si3N4) was prepared according to the following procedure.
二りず、５ｉｓＮ４９２．０重及部と焼結助剤としての
Ｙ２Ｏ，６，０重量部およ’ｒｆ’ Ａ ｌ ２０ ｓ
２ 。Nirisu, 5isN492.0 parts by weight, Y2O as a sintering aid, 6.0 parts by weight and 'rf' Al 20 s
2.
０重量部を、分散剤としてのオレイン酸０．５重量部を
含有するテトラクロロジフルオロエタン５１．１重量部
に少しずつ徐々に加えてボールミルで２４時間混合した
。0 parts by weight were gradually added little by little to 51.1 parts by weight of tetrachlorodifluoroethane containing 0.5 parts by weight of oleic acid as a dispersant, and mixed in a ball mill for 24 hours.
このようにして調製して得たスラリーを密閉攪拌タンク
に移し、３０℃に温度調節して２時間攪拌混合し、つい
で、タンク内のスラリー上部空間より真空ポンプで吸引
脱泡した。The slurry thus prepared was transferred to a sealed stirring tank, the temperature was adjusted to 30° C., and the mixture was stirred and mixed for 2 hours. Then, the slurry was suctioned and degassed from the upper space of the slurry in the tank using a vacuum pump.
一方、７０ ｍｒｍ Ｘ １００ ｍｍ Ｘ １０ ａ
ｍの平板状のキャピテイを持つステンレス鋼製でかつ冷
却水配管内蔵の鋳型を５℃の冷却水により冷却しつつ、
前記スラリータンク−Ｌ部室間に７ｋｇ ／ ｃｒ！
Ｇの圧力を窒素でかけ、３０℃に温度調節したフ１−ド
パイブを通してスラリーを鋳型に注入し、１分間７ ｋ
ｇ／ ｃｕｔ Ｇに保持しながら、窒素を排気してスラ
リーにかかる圧力を大気に戻し、平板形状の成形体を取
り出した。On the other hand, 70 mrm x 100 mm x 10 a
A mold made of stainless steel with a flat plate-like capacity of m and a built-in cooling water pipe is cooled with cooling water at 5°C.
7kg/cr between the slurry tank and L section!
The slurry was injected into the mold through a pipe with a temperature controlled at 30°C under a pressure of 7 k for 1 minute with nitrogen.
While maintaining the pressure at g/cut G, the pressure on the slurry was returned to the atmosphere by exhausting nitrogen, and the plate-shaped molded body was taken out.
このようにして得た平板形状成形体を抽出槽内に保持し
、３５℃のモノクロロトリフルオロメタンをポンプで２
００気圧に調節しつつ抽出槽に供給し、２時間保持して
成形体中のテ！・シクロ０ジフルオロエタンを抽出除去
を行い、次いでモノクロロトリフルオロメタンの供給を
止め、排気しながら１時間かけて大気圧に戻し、さらに
真空ポンプで１０−”Ｔｏｒｒまで真空排気し、ついで
窒素を供給し大気圧としてから成形体を取出した。The plate-shaped molded product thus obtained was held in an extraction tank, and monochlorotrifluoromethane at 35°C was pumped into the tank for 2 hours.
It is supplied to the extraction tank while adjusting the pressure to 0.00 atm, and kept for 2 hours until the temperature inside the molded body is removed.・Extract and remove cyclo0difluoroethane, then stop the supply of monochlorotrifluoromethane, return to atmospheric pressure for 1 hour while evacuation, further evacuate to 10-” Torr with a vacuum pump, and then supply nitrogen to increase the pressure. The molded body was taken out after being brought to atmospheric pressure.
以上のような脱分散媒操作を経たのちの成形体には、割
れ、亀裂、変形などの変化は認められず、また分散媒除
去前後の成形体の１「量差は使用したテトラクロロジフ
ルオロエタンの量にほぼ対応するものであることが認め
られた。No cracks, cracks, deformation or other changes were observed in the molded product after the dispersion medium removal operation as described above. It was recognized that the amount corresponds almost to the amount.
本発明で使用するトリフルオロメタンは、そのｈｓＴ造
として分子中に酸素を含まず、かつ化学的に安定であり
、原料粉体を酸化させろ可能性が全くないことから原材
粉体酸化による不都合を完全に回避することができると
いう効果を有している。The trifluoromethane used in the present invention does not contain oxygen in its molecules due to its hsT structure, and is chemically stable.Therefore, there is no possibility of oxidizing the raw material powder, so there are no disadvantages caused by oxidation of the raw material powder. This has the effect of being completely avoidable.
Claims (1)
た後、分散媒を超臨界のモノクロロトリフルオロメタン
で抽出除去することを特徴とする金属粉あるいはセラミ
ック粉の成形方法。A method for forming metal powder or ceramic powder, which comprises casting a slurry of metal powder or ceramic powder, and then extracting and removing the dispersion medium with supercritical monochlorotrifluoromethane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9753387A JPS63264303A (en) | 1987-04-22 | 1987-04-22 | Cast-molding of powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9753387A JPS63264303A (en) | 1987-04-22 | 1987-04-22 | Cast-molding of powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63264303A true JPS63264303A (en) | 1988-11-01 |
| JPH0420361B2 JPH0420361B2 (en) | 1992-04-02 |
Family
ID=14194892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9753387A Granted JPS63264303A (en) | 1987-04-22 | 1987-04-22 | Cast-molding of powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63264303A (en) |
-
1987
- 1987-04-22 JP JP9753387A patent/JPS63264303A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0420361B2 (en) | 1992-04-02 |
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