JPH02101101A - Method for removing binder from powder injection molding body - Google Patents
Method for removing binder from powder injection molding bodyInfo
- Publication number
- JPH02101101A JPH02101101A JP63252672A JP25267288A JPH02101101A JP H02101101 A JPH02101101 A JP H02101101A JP 63252672 A JP63252672 A JP 63252672A JP 25267288 A JP25267288 A JP 25267288A JP H02101101 A JPH02101101 A JP H02101101A
- Authority
- JP
- Japan
- Prior art keywords
- water
- binder
- injection molded
- organic polymer
- molded article
- 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
- 239000011230 binding agent Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000843 powder Substances 0.000 title claims abstract description 25
- 238000001746 injection moulding Methods 0.000 title claims description 14
- 238000002347 injection Methods 0.000 claims abstract description 38
- 239000007924 injection Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229920000620 organic polymer Polymers 0.000 claims abstract description 31
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 30
- 238000005238 degreasing Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000004416 thermosoftening plastic Substances 0.000 claims abstract description 23
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 10
- 238000011282 treatment Methods 0.000 claims description 14
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229920000609 methyl cellulose Polymers 0.000 claims description 4
- 239000001923 methylcellulose Substances 0.000 claims description 4
- 235000010981 methylcellulose Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920001289 polyvinyl ether Polymers 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 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 claims 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims 2
- 238000007654 immersion Methods 0.000 abstract description 9
- -1 polyethylene Polymers 0.000 abstract description 7
- 239000004698 Polyethylene Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 229920000573 polyethylene Polymers 0.000 abstract description 6
- 238000000465 moulding Methods 0.000 abstract description 5
- 230000008961 swelling Effects 0.000 abstract description 3
- 238000010828 elution Methods 0.000 description 13
- 239000004793 Polystyrene Substances 0.000 description 5
- 229920002223 polystyrene Polymers 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000004898 kneading Methods 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
- 239000003960 organic solvent Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920000193 polymethacrylate Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920001490 poly(butyl methacrylate) polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Abstract
Description
【発明の詳細な説明】
「産業上の利用分野」
本発明は、金属やセラミックス等の粉末を射出成形法に
よって成形し、これより焼結品を得るための方法に係わ
り、特に射出成形体の組成および脱脂方法に関する。Detailed Description of the Invention "Field of Industrial Application" The present invention relates to a method for molding powder of metals, ceramics, etc. by an injection molding method and obtaining a sintered product from the powder, and particularly relates to a method for obtaining a sintered product from the powder by injection molding. Regarding composition and degreasing method.
「従来技術とその課題」
従来、金属粉末やセラミックス粉末から焼結品を製造す
る方法として、上記粉末に有機バインダーを配合して混
練し、粉末に流動性を付与してこれを射出成形し、得ら
れた成形体を脱脂・焼結することによって焼結品を製造
する方法が知られている。この場合、脱脂の方法として
は、
（イ）射出形成体を加熱にするごとによって有機バイン
ダーを分解・蒸発させる方法、
（ロ）溶媒を用いて射出成形体から有機バインダーを溶
出する方法がある。"Prior Art and its Problems" Conventionally, as a method for manufacturing sintered products from metal powder or ceramic powder, the above powder is mixed with an organic binder, kneaded, imparted fluidity to the powder, and then injection molded. A method of manufacturing a sintered product by degreasing and sintering the obtained molded body is known. In this case, degreasing methods include (a) a method in which the organic binder is decomposed and evaporated by heating the injection molded product, and (b) a method in which the organic binder is eluted from the injection molded product using a solvent.
（イ）の方法においては、成形体を変形ざＵることなく
脱脂するには非常に長い時間を要するという問題がある
。すなわち射出成形法では、混練物が加熱されることに
よって軟化し、流動性を呈するという現象を利用するも
のであるため、成形体が加熱時に軟化して変形すること
が当然予想される。したがってこれを防ぐためには、変
形温度に達する前に混練物中に含まれる有機バインダー
の部を除去すれば良いと考えられるが、変形温度以下で
有機バインダーを分解しあるいは蒸発して除去するので
は長時間が必要となる。逆に、変形温度以下で有機バイ
ンダーが簡単に分解・蒸発するようであると、混練物の
射出成形時にお（）る射出成形時の流動性が不安定とな
り、加えて、射出成形後に生ずるランナ一部やスプル一
部などの再生が困難となる。The problem with method (a) is that it takes a very long time to degrease the molded product without deforming it. That is, since the injection molding method utilizes the phenomenon that the kneaded material softens and exhibits fluidity when heated, it is naturally expected that the molded product will soften and deform during heating. Therefore, in order to prevent this, it is considered that the organic binder contained in the kneaded material should be removed before the deformation temperature is reached, but it is not possible to remove the organic binder by decomposing or evaporating below the deformation temperature. It takes a long time. On the other hand, if the organic binder easily decomposes and evaporates below the deformation temperature, the fluidity during injection molding of the kneaded product will become unstable, and in addition, the runners formed after injection molding will become unstable. It becomes difficult to play some parts or parts of the sprue.
また、加熱時の軟化の程度を抑えることにより、脱脂時
の変形を抑える方法では、射出成形時の流動性が悪くな
り精密な成形が困難になる。一方、変形を防ぐために熱
硬化性樹脂を用いたり、昇華物質を加えたりする方法も
考えられるが、その場合には混練物の流動性が劣化した
り、ランナ一部やスプル一部の再生が不可能になるとい
った問題がある。またこの場合、脱脂初期の急激な有機
バインダーの分解・蒸発に起因して射出成形体にふくれ
や亀裂を生じるといった問題もある。Furthermore, in the method of suppressing deformation during degreasing by suppressing the degree of softening during heating, fluidity during injection molding deteriorates, making precise molding difficult. On the other hand, methods of using a thermosetting resin or adding a sublimation substance to prevent deformation may be considered, but in that case, the fluidity of the kneaded product may deteriorate, or part of the runner or sprue may be regenerated. The problem is that it becomes impossible. Further, in this case, there is a problem that blisters and cracks occur in the injection molded product due to rapid decomposition and evaporation of the organic binder at the initial stage of degreasing.
そこで、（ロ）の方法により、変形温度以下の低温にお
いて溶媒で、有機バインダーの一部を溶出除去すれば、
後の加熱によっても変形が起きず、除去された有機バイ
ンダーの部分が道となって、残りの有機バインダーの分
解・蒸発ガスが抜けやすくなり、ふくれや亀裂が生じに
くくなる。また、熱的に不安定な成分を入れる必要がｔ
ｌいことからランナ一部やスプル一部の再生も可能とな
る。Therefore, if a part of the organic binder is eluted and removed using a solvent at a low temperature below the deformation temperature using the method (b),
Deformation does not occur even when heated afterwards, and the removed organic binder becomes a channel, making it easier for the decomposition and evaporation of the remaining organic binder to escape, making it difficult for blisters and cracks to occur. Also, there is no need to add thermally unstable components.
Since it is small, it is also possible to regenerate part of the runner and part of the sprue.
しかしながら、（ロ）の方法では、従来の粉末の射出成
形法に用いられている一般の有機バインダーを溶出する
には有機溶剤を用いる必要があるが、有機溶剤は高価で
あり、また有機溶剤の取り扱いによっては危険を伴うこ
とがある。However, in method (b), it is necessary to use an organic solvent to elute the general organic binder used in the conventional powder injection molding method, but organic solvents are expensive and May be dangerous depending on handling.
また、可塑剤、潤滑剤のみを溶出した後、加熱脱脂する
といった方法も考えられるが、その場合にも可塑剤や潤
滑剤の量を増やすと成形体の強度劣化や、射出成形時に
滲みだしなとがおこるため、添加量を増やせず、加熱脱
脂時の変形やふくれを防止するには未だ不十分である。Another option is to elute only the plasticizer and lubricant and then heat and degrease, but in that case too, increasing the amount of plasticizer or lubricant may cause deterioration in the strength of the molded product or bleed during injection molding. Because of this, the amount added cannot be increased, and it is still insufficient to prevent deformation and blistering during heat degreasing.
この発明はｊ二記事情に鑑みてなされたもので、その目
的とするところは、粉末の射出成形法の脱脂工程におい
て、変形やふくれ、亀裂を生じさせることなく短時間で
の脱脂を可能にすることにある。This invention was made in view of the above two circumstances, and its purpose is to enable degreasing in a short time without causing deformation, blistering, or cracking in the degreasing process of powder injection molding. It's about doing.
「課題を解決するための手段」
この発明の方５法では、粉末と有機バインダーを混合し
、これを射出成形して射出成形体としりこ後、脱脂・焼
結の各処理を行って焼結体を製造するための方法におい
て、−］二二記機バインダーとして、少なくとも１種の
水溶性の熱可塑性有機ポリマーと、少なくとも１種の水
に不溶の熱可塑性有機ポリマーとを含む有機バインダー
を用い、」１記脱脂処理として、射出成形体と水とを接
触せしめて上記水溶性の熱可塑性有機ポリマーを溶出し
た後、加熱炉において残りの何機バインダーを加熱除去
することを上記課題の解決手段とした。``Means for Solving the Problems'' In method 5 of the present invention, powder and organic binder are mixed, this is injection molded to form an injection molded body, and then subjected to degreasing and sintering treatments, and then sintered. In the method for producing a body, an organic binder comprising at least one water-soluble thermoplastic organic polymer and at least one water-insoluble thermoplastic organic polymer is used as the binder. 1. As the degreasing treatment, the injection molded body is brought into contact with water to elute the water-soluble thermoplastic organic polymer, and then the remaining binder is removed by heating in a heating furnace. And so.
以下、この発明の詳細な説明する。The present invention will be described in detail below.
まず、粉末と有機バインダーを混合し、これを射出成形
して射出成形体とする、ここで粉末としては、金属粉末
、セラミックス粉末などが用いられる。また、有機バイ
ンダーとしては、少なくとも１種の水溶性の熱可塑性有
機ポリマーと、少なくとも１種の水に不溶の熱可塑性有
機ポリマーとを含む有機バインダーが用いられる。」１
記水溶性の熱可塑性有機ポリマーとしては、ポリエチレ
ンオキサイド、ポリエチレングリコール、メチルセルロ
ース、カルポギシルメチルセルロース、ポリアクリルア
ミド、ポリビニルエーテル、ポリアクリル酸、ポリメタ
クリル酸などが用いられ、中でもポリエチレンオキサイ
ドが好適に用いられる。First, a powder and an organic binder are mixed and the mixture is injection molded to form an injection molded body. Here, the powder used is a metal powder, a ceramic powder, or the like. Further, as the organic binder, an organic binder containing at least one type of water-soluble thermoplastic organic polymer and at least one type of water-insoluble thermoplastic organic polymer is used. ”1
As the water-soluble thermoplastic organic polymer, polyethylene oxide, polyethylene glycol, methyl cellulose, carpogyl methyl cellulose, polyacrylamide, polyvinyl ether, polyacrylic acid, polymethacrylic acid, etc. are used, and among them, polyethylene oxide is preferably used. .
すなわちポリエチレンオキサイドは、射出成形性に優れ
、他の水溶性ポリマーとの相溶性か良好であるばかりで
なく、水に不溶の熱可塑性ポリマー例えばポリスチレン
、ポリエチレン、ポリメタクリル酸エステル、エチレン
酢酸ビニル共重合体などとの相溶性も良好であり、さら
には熱分解性ら良好であるからである。上記水に不溶の
熱可塑性有機ポリマーとしては、」二連したポリスチレ
ン、ポリエチレン、ポリメタクリル酸エステル、エチレ
ン酢酸ビニル共重合体なとの、通常の金属粉末やセラミ
ックス粉末の射出成形に使用される熱可塑性ポリマーが
用いられる。In other words, polyethylene oxide not only has excellent injection moldability and good compatibility with other water-soluble polymers, but also has excellent compatibility with water-insoluble thermoplastic polymers such as polystyrene, polyethylene, polymethacrylate, and ethylene-vinyl acetate copolymers. This is because it has good compatibility with coalescence, etc., and also has good thermal decomposition properties. The above-mentioned water-insoluble thermoplastic organic polymers include ``dyadic polystyrene, polyethylene, polymethacrylate, ethylene-vinyl acetate copolymer, etc.'' A plastic polymer is used.
次に、この射出成形体に脱脂処理を行って脱脂体とする
。脱脂処理としては、まず射出成形体を水（常温水およ
び加熱水を含む。以下同様）に接触せしめ、これにより
上記水溶性の熱可塑性有機ポリマーを溶出する。ここで
、射出成形体と水との接触方法としては、射出成形体を
水中に浸漬ことによって処理するのが、作業性等の点か
らもまた溶出時間の短縮といった点からも好適とされる
。Next, this injection molded body is subjected to a degreasing treatment to obtain a degreased body. In the degreasing treatment, the injection molded article is first brought into contact with water (including room temperature water and heated water; the same applies hereinafter), thereby eluting the water-soluble thermoplastic organic polymer. Here, as a method of contacting the injection molded article with water, treatment by immersing the injection molded article in water is preferred from the viewpoint of workability and shortening of elution time.
その後、加熱炉において加熱脱脂を施し、水に不溶の熱
可塑性有機ポリマーなどの残りの有機バインダーを除去
ケる。ここで、加熱脱脂を行うにあたっては、常圧で加
熱脱脂しても良いが、減圧下にて行うのがより有機バイ
ンダーの除去時間を短縮し得ることから好適とされ、特
に真空脱脂を行うのが望ましい。Thereafter, it is heated and degreased in a heating furnace to remove remaining organic binders such as thermoplastic organic polymers that are insoluble in water. Here, when performing heat degreasing, heat degreasing may be carried out at normal pressure, but it is preferable to perform it under reduced pressure because it can further shorten the time required to remove the organic binder. is desirable.
その後、この脱脂体に加熱焼結処理を行い、金属、セラ
ミックスなどからなる焼結体を得る。Thereafter, this degreased body is heated and sintered to obtain a sintered body made of metal, ceramics, or the like.
［作用−１
この発明の方法によれば、有機バインダーとして少なく
とも１種の水溶性の熱可塑性有機ポリマーと、少なくと
も１種の水に不溶の熱可塑性有機ポリマーとを含む有機
バインダーを用い、脱脂処理として射出成形体と水とを
接触せしめて上記水溶性の熱可塑性有機ポリマーを溶出
するので、溶出時の該熱可塑性有機ポリマーの膨潤など
に起因する成形体の割れなどの発生が防止される。また
、水溶性熱可塑性ポリマーを溶出・除去することによっ
て射出成形体中に含まれる有機バインダーが十分に減少
しているため、残りの有機バインダーの加熱除去時にお
ける成形体の軟化および変形が防止され、また溶出され
た有機ポリマーの道付けの効果に起因するふくれ、亀裂
の発生が防止される。[Function-1] According to the method of the present invention, an organic binder containing at least one water-soluble thermoplastic organic polymer and at least one water-insoluble thermoplastic organic polymer is used, and the degreasing treatment is performed. Since the water-soluble thermoplastic organic polymer is eluted by bringing the injection molded body into contact with water, the molded body is prevented from cracking due to swelling of the thermoplastic organic polymer during elution. In addition, by eluting and removing the water-soluble thermoplastic polymer, the amount of organic binder contained in the injection molded product is sufficiently reduced, which prevents the molded product from softening and deforming when the remaining organic binder is removed by heating. In addition, the occurrence of blisters and cracks caused by the spreading effect of the eluted organic polymer is prevented.
「実施例」 以下、実施例によりこの発明を具体的に説明する。"Example" EXAMPLES The present invention will be specifically explained below with reference to Examples.
（実施例１ ）
Ｆｅ−８％Ｎｉ合金粉末（平均粒径８μｍ）１００重量
部に、水溶性熱可塑性樹脂としてポリエチレンオキサイ
ド５重量部、水に不溶性の熱可塑性樹脂としてポリエチ
レン３重量部、ステアリン酸１重量部を配合し、これを
混練機によって１５０℃で６０分間混練した。次に、得
られた混練物を粉砕し、スクリュウ式射出成形機でリン
グ状複雑形状部品（最大肉厚部約５Ｘ６ｍｍ）に成形し
た。この場合に射出温度は１７０℃、射出圧力は＋００
ＯＫｇ／ａｍ’とした。(Example 1) 100 parts by weight of Fe-8% Ni alloy powder (average particle size 8 μm), 5 parts by weight of polyethylene oxide as a water-soluble thermoplastic resin, 3 parts by weight of polyethylene as a water-insoluble thermoplastic resin, and stearic acid. 1 part by weight was blended and kneaded for 60 minutes at 150°C using a kneader. Next, the obtained kneaded material was pulverized and molded into a ring-shaped complex-shaped part (maximum thickness about 5 x 6 mm) using a screw injection molding machine. In this case, the injection temperature is 170℃ and the injection pressure is +00℃.
It was set as OKg/am'.
次いで、得られた成形体を常温および５０℃の水中にそ
れぞれ１〜５時間浸漬し、取り出した後３０分間真空乾
燥した。このときのバインダーの溶出率と水中に浸漬し
ている時間との関係を調べ、その結果を第１図および第
１表に示した。ただし、第１図および第１表中の溶出率
は以下の式により算出した。Next, the obtained molded body was immersed in water at room temperature and 50° C. for 1 to 5 hours, and after being taken out, it was vacuum dried for 30 minutes. The relationship between the binder elution rate and the immersion time in water was investigated, and the results are shown in FIG. 1 and Table 1. However, the elution rates in FIG. 1 and Table 1 were calculated using the following formula.
溶出率−
（溶出したバインダー重量）÷（総バインダー重量）さ
らに、乾燥後の成形体を窒素雰囲気炉内に入れ、１００
°Ｃ／ｈｏｕｒの昇温速度で４５０℃まで昇温して１時
間保持し、脱脂体を得た。得られた脱脂体の状態を観察
してその結果を第１表に併記した。Elution rate - (weight of eluted binder) ÷ (total weight of binder) Furthermore, the dried molded body was placed in a nitrogen atmosphere furnace and heated to 100
The temperature was raised to 450°C at a heating rate of °C/hour and held for 1 hour to obtain a defatted body. The state of the obtained defatted body was observed and the results are also listed in Table 1.
また、比較例として、エヂレン酢酸ビニル共重合体−ワ
ックス−ポリメタクリル酸ブチル系バインダーを用い、
上記と同条件で処理を行なって脱脂体を得、これの状態
も観察してその結果を第１表に示した。In addition, as a comparative example, using an ethylene vinyl acetate copolymer-wax-polybutyl methacrylate binder,
A degreased product was obtained by processing under the same conditions as above, and the condition of the product was also observed, and the results are shown in Table 1.
第１表
第１表に示したように、本発明の実施例のものでは、常
温（２５℃）水中で３時間以上保持したもの、あるいは
５０℃水中で２時間以上保持したものについてはふくれ
や亀裂・変形が全く見られず良好な脱脂体であることが
確認された。また、比較例のものでは内部に亀裂の発生
が認められた。As shown in Table 1, examples of the present invention did not blister when kept in water at room temperature (25°C) for more than 3 hours or in water at 50°C for more than 2 hours. It was confirmed that the degreased body was well-degreased with no cracks or deformation observed. In addition, cracks were observed inside the comparative example.
その後、上記脱脂体を水素雰囲気にて加熱炉で１３５０
℃で２時間焼結し、その焼結密度を測定したところ、７
．６２ｇ／ｃｍ３となり、高い焼結密度を有するもので
あることが確認された。Thereafter, the degreased body was heated to 1350°C in a heating furnace in a hydrogen atmosphere.
When sintered at ℃ for 2 hours and measured the sintered density, it was 7
．． It was confirmed that it had a high sintered density of 62 g/cm3.
（実施例２ ）
ＳＵＳ−３１６Ｌ粉末（平均粒径的８μｍ）１００重量
部に、ポリエチレンオキサイド６重量部、ポリスチレン
３重量部、さらに可塑剤、潤滑剤２重量部を配合し、上
記実施例１と同様に混練・射出を行なって同形の成形体
を得た。(Example 2) 100 parts by weight of SUS-316L powder (average particle size 8 μm) was blended with 6 parts by weight of polyethylene oxide, 3 parts by weight of polystyrene, and further 2 parts by weight of a plasticizer and a lubricant. Kneading and injection were carried out in the same manner to obtain a molded article of the same shape.
次に、得られた成形体を５０℃の水に４時間浸漬し、取
り出した後３０分間真空乾燥した。このときのバインダ
ーの溶出率を調べたところ、４７％であった。Next, the obtained molded body was immersed in water at 50° C. for 4 hours, taken out, and vacuum-dried for 30 minutes. When the elution rate of the binder at this time was examined, it was 47%.
次いで、この乾燥後の成形体を空気中にて１００℃／ｈ
ｏｕｒで３００℃まで昇温し、１時間保持して脱脂体を
得た。得られた脱脂体の状態を観察したところ、ふくれ
や亀裂の発生が見られず、９８％のバインダーの除去が
認められた。Next, this dried molded body was heated at 100°C/h in air.
The temperature was raised to 300° C. and maintained for 1 hour to obtain a defatted body. When the state of the obtained degreased body was observed, no blisters or cracks were observed, and 98% of the binder was removed.
その後、この脱脂体を真空中にて加熱炉で１３５０℃で
２時間焼結し、その焼結密度を測定したところ、７．８
７ｇ／ｃｍ”となり、高い焼結密度を有するものである
ことが確認された。Thereafter, this degreased body was sintered in a heating furnace in a vacuum at 1350°C for 2 hours, and the sintered density was measured and found to be 7.8.
7 g/cm'', and it was confirmed that it had a high sintered density.
（実施例３ ）
実施例２と同一の５ＵＳ−３１６Ｌ粉末１００重量部に
、ポリエチレンオキサイド５重量部、ポリエチレングリ
コール１重量部、ポリスチレン３゜５重量部、さらに可
塑剤、潤滑剤１．５重量部を配合し、上記実施例Ｉ、２
と同様に混練・射出を行い、寸法が７ｍｍＸ ７ｍｍＸ
７０ｍｍの棒状部品に成形した。(Example 3) To 100 parts by weight of the same 5US-316L powder as in Example 2, 5 parts by weight of polyethylene oxide, 1 part by weight of polyethylene glycol, 5 parts by weight of polystyrene 3.5 parts by weight, and further 1.5 parts by weight of a plasticizer and a lubricant. and the above Examples I and 2.
Knead and inject in the same manner as above, and the dimensions are 7mmX 7mmX
It was molded into a 70 mm rod-shaped part.
次に、得られた成形体を室温の水に２〜ｌＯ時間浸し、
取り出した後１時間真空乾燥した。この乾燥後の成形体
を第２図に示すように支持台１１１上に配置し、空気中
にて１００℃／ｈｏｕｒで３００℃まで昇温し、さらに
１時間保持した後溶出率、変形量、欠陥の有無を調べた
。得られた結果を第２表に示す。ここで、第２図におい
て符号２は成形体であり、またｄ、の寸法は５０ｊ＋ｘ
、ｄ、の寸法は５ｍＲである。Next, the obtained molded body is immersed in water at room temperature for 2 to 10 hours,
After taking it out, it was vacuum dried for 1 hour. The dried molded body was placed on a support stand 111 as shown in FIG. 2, and the temperature was raised to 300°C at a rate of 100°C/hour in air, and the temperature was maintained for another 1 hour. The presence or absence of defects was investigated. The results obtained are shown in Table 2. Here, in FIG. 2, numeral 2 is a molded body, and the dimension d is 50j+x
, d, has a dimension of 5 mR.
第２表
第２表に示したように水浸時間が２時間では、脱脂中に
成形体２の中央部が重力によって下方向に垂れ下がり、
変形（ふくれ）が大となるのに対し、水浸時間が５時間
以」二では、配置した状態のままで脱脂されており、ま
た水浸時間１０時間では、溶出率が３７％で変形も欠陥
も生じることなく脱脂されていることが確認された。Table 2 As shown in Table 2, when the water immersion time is 2 hours, the center part of the molded body 2 hangs downward due to gravity during degreasing.
In contrast, when the water immersion time was longer than 5 hours, the degreasing occurred as it was placed, and when the water immersion time was 10 hours, the dissolution rate was 37% and there was no deformation. It was confirmed that the degreasing was completed without any defects occurring.
（実施例４ ）
実施例２と同一組成のもの配合し、これを実施例１．２
．３と同様に混練射出成形して実施例１．２と同形の成
形体を得た。(Example 4) The same composition as in Example 2 was blended, and this was used in Example 1.2.
．． A molded article having the same shape as Example 1.2 was obtained by kneading and injection molding in the same manner as in Example 3.
次に、この成形体を５０℃の水に４時間浸漬し、４７％
のバインダーを除去した、
次いで、この乾燥後の成形体を５００ ｍｍＨｇの減圧
雰囲気にて１５０°Ｃ／ｈｏｕｒで４００℃まで昇温し
、１時間保持したところ、ふくれ・亀裂等の発生の無い
良好な脱脂体が得られた。Next, this molded body was immersed in water at 50°C for 4 hours, and 47%
After removing the binder, the dried molded product was heated to 400°C at 150°C/hour in a reduced pressure atmosphere of 500 mmHg and held for 1 hour. A defatted body was obtained.
（実施例５ ）
平均粒子径０．６４μｍ、比表面積６．８０ｍ２／ｇの
Ｙ２０３３ｍｏ１％の部分安定化Ｚｒ０２１００重量部
に、水溶性熱可塑性樹脂のポリエチレンオキサ１１１０
重量部、ポリエチレン７重量部、ステアリン酸３重量部
を配合し、これを混練機によって１５０°Ｃで６０分間
混練した、次に、得られた混練物を粉砕し、スクリュー
式射出成形機により射出温度１６５℃、射出圧力１００
０ Ｋｇ／ ｃｍ’の成形条件下で７ｍｍＸ ７ｍｍＸ
７０ｍｍの棒状部品を射出成形した。(Example 5) Polyethylene oxa 1110, a water-soluble thermoplastic resin, was added to 100 parts by weight of partially stabilized Zr02 of 1% Y2033 mo with an average particle diameter of 0.64 μm and a specific surface area of 6.80 m2/g.
parts by weight, 7 parts by weight of polyethylene, and 3 parts by weight of stearic acid were mixed together using a kneader at 150°C for 60 minutes.The resulting kneaded product was then pulverized and injected using a screw injection molding machine. Temperature 165℃, injection pressure 100
7mmX 7mmX under molding condition of 0 Kg/cm'
A 70 mm rod-shaped part was injection molded.
次いで、得られた成形体を２５°Ｃおよび５０℃の水中
に１〜５時間浸漬し、取り出した後真空乾燥した。この
ときのバインダーの溶出率と水中に浸している時間との
関係を調べ、その結果を第３図に示した。Next, the obtained molded body was immersed in water at 25°C and 50°C for 1 to 5 hours, taken out, and then vacuum dried. The relationship between the elution rate of the binder and the time of immersion in water was investigated, and the results are shown in FIG.
次いで、この乾燥後の成形体のうち溶出率が２０％ 〔
溶出時間５時間〕のものを、大気雰囲気下にて常温から
１００℃まで１時間、１００８Ｃ〜４００℃まで６時間
で昇温し、４００℃で１時間保持した。得られた脱脂体
を調べたところ、脱脂率が９８％であり、無欠陥の脱脂
体が得られ、従来より短時間で脱脂することが判明した
。Next, the elution rate of the molded body after drying is 20% [
elution time of 5 hours] was heated in air from room temperature to 100°C in 1 hour, from 1008C to 400°C in 6 hours, and held at 400°C for 1 hour. When the obtained degreased body was examined, it was found that the degreasing rate was 98%, that a defect-free degreased body was obtained, and that it was degreased in a shorter time than conventionally.
さらに、得られた脱脂体を大気雰囲気下にて１４５０℃
で４時間焼結し、その焼結体密度を測定したところ、６
．０２ｇ／ａｍ３となり、ふくれ・亀裂等の無い無欠陥
の焼結体が得られた。Furthermore, the obtained degreased body was heated to 1450°C under an air atmosphere.
When sintered for 4 hours and measured the density of the sintered body, it was 6
．． 02 g/am3, and a defect-free sintered body with no blisters, cracks, etc. was obtained.
なお、比較例として」１記Ｚｒ０ｚにポリスチレン、ア
タクティックポリプロピレンを主成分とするバインダー
を添加して射出成形体を成形し、上記と同様の脱脂を行
ったところ、ふくれ・亀裂等の欠陥の発生が見られた。As a comparative example, when a binder containing polystyrene or atactic polypropylene as a main component was added to Zr0z in 1., an injection molded product was molded, and degreased in the same manner as above, defects such as blisters and cracks occurred. It was observed.
「発明の効果」
以」二説明したように、本発明における請求項１に記載
した発明は、有機バインダーとして少なくとも１種の水
溶性の熱可塑性有機ポリマーと、少なくとも１種の水に
不溶の熱可塑性有機ポリマーとを含む有機バインダーを
用い、上記脱脂処理として射出成形体と水とを接触せし
めて上記水溶性の熱可塑性有機ポリマーを溶出した後、
加熱炉において残りの有機バインダーを加熱除去するも
のであるから、溶出時における熱可塑性ポリマーの膨潤
などに起因する成形体の割れなどの発生を防止すること
ができ、また水溶性熱可塑性ポリマーを溶出・除去する
ことによって射出成形体中に含まれる有機バインダーが
十分に減少しているため、残りの有機バインダーの常圧
下または減圧下での加熱除去時における成形体の軟化お
よび変形を防止することができる。さらに、溶出された
有機ポリマーの道付けの効果に起因するふくれ、亀裂の
発生が防止されているため、例えば急速加熱や減圧雰囲
気中での加熱等の方法を用いることによって短時間で脱
脂を行うことができる。"Effects of the Invention" As explained hereinafter, the invention described in claim 1 of the present invention comprises at least one water-soluble thermoplastic organic polymer as an organic binder and at least one water-insoluble thermoplastic polymer. Using an organic binder containing a plastic organic polymer, the injection molded article is brought into contact with water as the degreasing treatment to elute the water-soluble thermoplastic organic polymer,
Since the remaining organic binder is removed by heating in a heating furnace, it is possible to prevent cracking of the molded product due to swelling of the thermoplastic polymer during elution, and also to elute the water-soluble thermoplastic polymer.・Because the organic binder contained in the injection molded product is sufficiently reduced by removing it, it is possible to prevent the molded product from softening and deforming when the remaining organic binder is removed by heating under normal pressure or reduced pressure. can. Furthermore, since the formation of blisters and cracks due to the effect of leaching organic polymers is prevented, degreasing can be done in a short time by using methods such as rapid heating or heating in a reduced pressure atmosphere. be able to.
また、本発明の請求項２に記載した発明にあっては、水
溶性の熱可塑性有機ポリマーとしてポリエヂレンオキサ
イド等を用いるので、上記効果を十分に発揮するととも
に、射出成形性にも優れたものとなる。In addition, in the invention described in claim 2 of the present invention, since polyethylene oxide or the like is used as the water-soluble thermoplastic organic polymer, the above-mentioned effects are fully exhibited and the injection moldability is also excellent. Become something.
本発明の請求項３に記載した発明にあっては、射出成形
体を水中に浸漬するようにしたので、処理に際しての作
業性を十分に向−ヒし得るとともに、水溶性熱可塑性何
機ポリマーの溶出を短時間にて確実に行うことができる
。In the invention described in claim 3 of the present invention, since the injection molded product is immersed in water, workability during processing can be sufficiently improved, and water-soluble thermoplastic polymer can be reliably eluted in a short time.
本発明の請求項４に記載した発明にあっては、脱脂処理
における打機バインダーの加熱除去を常圧下または減圧
下にて行うようにしたので、有機バインダーの除去時間
をより短縮することができる。In the invention described in claim 4 of the present invention, since the beating machine binder is removed by heating during the degreasing treatment under normal pressure or reduced pressure, the time required to remove the organic binder can be further shortened. .
さらに、本発明の請求項５および６に記載した発明にあ
っては、いずれも請求項４に記載した発明の効果をより
一層高めることができる。Furthermore, in the inventions described in claims 5 and 6 of the present invention, the effect of the invention described in claim 4 can be further enhanced.
第１図ないし第３図はこの発明の方法に係わる図であっ
て、第１図は実施例１における水浸時間とバインダーの
溶出率との関係を示すグラフ、第２図は水浸溶出処理後
の成形体の配置状態を示す側面図、第３図は実施例５に
おける水浸時間とバインダーの溶出率との関係を示すグ
ラフである。
・支持台、
成形体。Figures 1 to 3 are diagrams relating to the method of the present invention, in which Figure 1 is a graph showing the relationship between water immersion time and binder elution rate in Example 1, and Figure 2 is a graph showing the water immersion elution treatment. FIG. 3 is a side view showing the subsequent arrangement of the molded body, and is a graph showing the relationship between water immersion time and binder elution rate in Example 5.・Support stand, molded object.
Claims (6)
して射出成形体とした後、脱脂・焼結の各処理を行って
焼結体を製造する方法であって、上記有機バインダーと
して、少なくとも１種の水溶性の熱可塑性有機ポリマー
と、少なくとも１種の水に不溶の熱可塑性有機ポリマー
とを含む有機バインダーを用い、 上記脱脂処理として、射出成形体と水とを接触せしめて
上記水溶性の熱可塑性有機ポリマーを溶出した後、加熱
炉において残りの有機バインダーを加熱除去することを
特徴とする粉末の射出成形体からバインダーを除去する
方法。(1) A method for manufacturing a sintered body by mixing powder and an organic binder, injection molding the mixture to form an injection molded body, and then performing degreasing and sintering treatments, the organic binder comprising: Using an organic binder containing at least one water-soluble thermoplastic organic polymer and at least one water-insoluble thermoplastic organic polymer, the degreasing treatment is performed by bringing the injection molded article into contact with water to remove the water-soluble 1. A method for removing a binder from a powder injection molded article, the method comprising: eluating a thermoplastic organic polymer, and then heating and removing the remaining organic binder in a heating furnace.
塑性有機ポリマーとしてポリエチレンオキサイド、ポリ
エチレングリコール、メチルセルロース、カルボキシル
メチルセルロース、ポリアクリルアミド、ポリビニルエ
ーテル、ポリアクリル酸、ポリメタクリル酸の少なくと
も１種を用いることを特徴とする粉末の射出成形体から
バインダーを除去する方法。(2) In the method according to claim 1, at least one of polyethylene oxide, polyethylene glycol, methyl cellulose, carboxyl methyl cellulose, polyacrylamide, polyvinyl ether, polyacrylic acid, and polymethacrylic acid is used as the water-soluble thermoplastic organic polymer. A method for removing a binder from an injection molded powder body, characterized in that:
ける射出成形体と水との接触を、射出成形体を水中に浸
漬することによって処理することを特徴とする粉末の射
出成形体からバインダーを除去する方法。(3) In the method according to claim 1, the binder is removed from the powder injection molded article, characterized in that the contact between the injection molded article and water during the degreasing treatment is carried out by immersing the injection molded article in water. How to remove.
ける加熱炉での残りの有機バインダーの加熱除去を常圧
下または減圧下にて行うことを特徴とする粉末の射出成
形体からバインダーを除去する方法。(4) The method according to claim 1, wherein the remaining organic binder is removed by heating in a heating furnace during the degreasing treatment under normal pressure or reduced pressure. Method.
塑性ポリマーとしてポリエチレンオキサイド、ポリエチ
レングリコール、メチルセルロース、カルボキシルメチ
ルセルロース、ポリアクリルアミド、ポリビニルエーテ
ル、ポリアクリル酸、ポリメタクリル酸の少なくとも１
種を用いることを特徴とする粉末の射出成形体からバイ
ンダーを除去する方法。(5) In the method according to claim 4, the water-soluble thermoplastic polymer is at least one of polyethylene oxide, polyethylene glycol, methyl cellulose, carboxyl methyl cellulose, polyacrylamide, polyvinyl ether, polyacrylic acid, and polymethacrylic acid.
A method for removing a binder from a powder injection molded article, the method comprising using seeds.
ける射出成形体と水との接触を、射出成形体を水中に浸
漬することによって処理することを特徴とする粉末の射
出成形体からバインダーを除去する方法。(6) In the method according to claim 4, the binder is removed from the powder injection molded article, wherein the contact between the injection molded article and water during the degreasing treatment is carried out by immersing the injection molded article in water. How to remove.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63252672A JPH0653884B2 (en) | 1988-10-06 | 1988-10-06 | Method for removing binder from powder injection molded body |
| US07/417,198 US5059388A (en) | 1988-10-06 | 1989-10-04 | Process for manufacturing sintered bodies |
| KR1019890014358A KR930006005B1 (en) | 1988-10-06 | 1989-10-06 | Process for manufacturing sintered bodies |
| EP89118587A EP0362866B1 (en) | 1988-10-06 | 1989-10-06 | Process for manufacturing sintered bodies |
| DE68914379T DE68914379T2 (en) | 1988-10-06 | 1989-10-06 | Process for the production of sintered bodies. |
| HK102095A HK102095A (en) | 1988-10-06 | 1995-06-22 | Process for manufacturing sintered bodies |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63252672A JPH0653884B2 (en) | 1988-10-06 | 1988-10-06 | Method for removing binder from powder injection molded body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02101101A true JPH02101101A (en) | 1990-04-12 |
| JPH0653884B2 JPH0653884B2 (en) | 1994-07-20 |
Family
ID=17240630
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63252672A Expired - Fee Related JPH0653884B2 (en) | 1988-10-06 | 1988-10-06 | Method for removing binder from powder injection molded body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0653884B2 (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02182803A (en) * | 1989-01-05 | 1990-07-17 | Sumitomo Cement Co Ltd | Method for degreasing powder molding body |
| JPH02182804A (en) * | 1989-01-05 | 1990-07-17 | Sumitomo Cement Co Ltd | Method for degreasing powder molding body |
| US5194203A (en) * | 1991-02-28 | 1993-03-16 | Mitsui Mining & Smelting Co., Ltd. | Methods of removing binder from powder moldings |
| WO1998014293A1 (en) * | 1996-10-03 | 1998-04-09 | Komatsu Ltd. | Dewaxing method, dewaxed product obtained therefrom and sintered product |
| US5744532A (en) * | 1994-03-23 | 1998-04-28 | Nippon Shokubai Co. Ltd. | Powder injection molding binder, powder injection molding composition and method for production of sintered member |
| US5877270A (en) * | 1994-03-14 | 1999-03-02 | Kabushiki Kaisha Komatsu Seisakusho | Water solvent extraction degreasing method and molded products produced therewith |
| JP2014514183A (en) * | 2011-03-16 | 2014-06-19 | ビーエーエスエフ ソシエタス・ヨーロピア | Method for producing metal or ceramic molded body |
| CN109653896A (en) * | 2017-10-10 | 2019-04-19 | 隆巴第尼有限责任公司 | Piston and its manufacturing method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101454797B1 (en) * | 2012-10-30 | 2014-10-28 | (주)엠티아이지 | method of manufacturing powder injection structure |
-
1988
- 1988-10-06 JP JP63252672A patent/JPH0653884B2/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02182803A (en) * | 1989-01-05 | 1990-07-17 | Sumitomo Cement Co Ltd | Method for degreasing powder molding body |
| JPH02182804A (en) * | 1989-01-05 | 1990-07-17 | Sumitomo Cement Co Ltd | Method for degreasing powder molding body |
| US5194203A (en) * | 1991-02-28 | 1993-03-16 | Mitsui Mining & Smelting Co., Ltd. | Methods of removing binder from powder moldings |
| US5877270A (en) * | 1994-03-14 | 1999-03-02 | Kabushiki Kaisha Komatsu Seisakusho | Water solvent extraction degreasing method and molded products produced therewith |
| US5744532A (en) * | 1994-03-23 | 1998-04-28 | Nippon Shokubai Co. Ltd. | Powder injection molding binder, powder injection molding composition and method for production of sintered member |
| WO1998014293A1 (en) * | 1996-10-03 | 1998-04-09 | Komatsu Ltd. | Dewaxing method, dewaxed product obtained therefrom and sintered product |
| KR100506681B1 (en) * | 1996-10-03 | 2005-11-25 | 가부시키가이샤 고마쓰 세이사쿠쇼 | Degreasing method and degreasing body and sintered body obtained by it |
| JP2014514183A (en) * | 2011-03-16 | 2014-06-19 | ビーエーエスエフ ソシエタス・ヨーロピア | Method for producing metal or ceramic molded body |
| CN109653896A (en) * | 2017-10-10 | 2019-04-19 | 隆巴第尼有限责任公司 | Piston and its manufacturing method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0653884B2 (en) | 1994-07-20 |
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