JPH06122903A - Method for degreasing metal powder compact - Google Patents
Method for degreasing metal powder compactInfo
- Publication number
- JPH06122903A JPH06122903A JP4312595A JP31259592A JPH06122903A JP H06122903 A JPH06122903 A JP H06122903A JP 4312595 A JP4312595 A JP 4312595A JP 31259592 A JP31259592 A JP 31259592A JP H06122903 A JPH06122903 A JP H06122903A
- Authority
- JP
- Japan
- Prior art keywords
- furnace
- metal powder
- degreasing
- binder
- pressure
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、金属の粉末とバインダ
との成形体からバインダの混合物を除去しながら焼結す
る際の脱脂技術に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a degreasing technique for sintering a mixture of a metal powder and a binder while removing a mixture of the binder.
【０００２】[0002]
【従来の技術】近年、粉末射出成形法が開発され、業界
において注目されている。しかし成形体中に含まれる多
量のバインダの混合物の除去（脱脂）に２日〜７日とい
う長時間を要するのが欠点である。この欠点を解消する
ための工夫として、バインダを有機溶剤で抽出する方
法、反応性ガスを流してバインダを分解する方法、高真
空下で脱脂する方法・・・等が提案されているが、これ
らの中で例えば特開平３−１９７６０２号公報記載の如
き高真空で脱脂する方法が、特別な装置を必要としない
点において比較的簡便である。この技術は図３に示すよ
うな温度（Ａ）と圧力（Ｂ）で実施されている。2. Description of the Related Art In recent years, a powder injection molding method has been developed and attracted attention in the industry. However, the disadvantage is that it takes a long time of 2 to 7 days to remove (defatt) the mixture of a large amount of binder contained in the molded body. As a device for solving this drawback, a method of extracting a binder with an organic solvent, a method of decomposing the binder by flowing a reactive gas, a method of degreasing under high vacuum, etc. have been proposed, Among them, the method of degreasing under high vacuum as described in, for example, Japanese Patent Laid-Open No. 3-197602 is relatively simple in that no special device is required. This technique is carried out at temperature (A) and pressure (B) as shown in FIG.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、この従
来技術には次のような欠点がある。However, this conventional technique has the following drawbacks.
【０００４】成形体中に含まれているバインダは、炉内
が高真空であるためにガス化して発生する。そしてこの
ガス化したバインダが、炉内に充満し断熱材及び炉壁の
近傍で凝縮しながら液化あるいは固化してこれに付着す
る。そうすると断熱材は損傷するし、炉の真空度は劣化
する。したがって、炉壁に付いたバインダを除去するた
めに、炉壁を加熱する装置を設けなければならない。断
熱材の損傷については防ぎようがない。The binder contained in the compact is gasified and generated due to the high vacuum in the furnace. The gasified binder fills the inside of the furnace and liquefies or solidifies while condensing in the vicinity of the heat insulating material and the furnace wall and adheres thereto. This will damage the insulation and degrade the furnace vacuum. Therefore, in order to remove the binder attached to the furnace wall, a device for heating the furnace wall must be provided. There is no protection against damage to the insulation.
【０００５】さらに、成形体及びこれを納めたボックス
内の加熱は、輻射のみで行われているので温度の上昇が
おそく、また成形体の温度バラツキが大きい。このた
め、脱脂率が成形体毎で異なり、脱脂不充分な成形体に
は変化やふくれといった欠陥が発生してしまう。Further, since the heating of the molded body and the box containing the molded body is performed only by radiation, the temperature rises slowly, and the temperature variation of the molded body is large. For this reason, the degreasing rate differs depending on the molded product, and defects such as change and swelling occur in the molded product with insufficient degreasing.
【０００６】また、成形体の焼結が終わったあとのボッ
クス内温度を常温近くまで下げてから次のサイクルを開
始しなければならないので、このサイクルの時間が長く
なってしまう。もし、この時間を短縮するために不十分
な降温のままで次のサイクルを開始したならば、炉内が
高温であることから脱脂の進行が急激に進み焼結体のふ
くれや変形の発生原因となる。Further, since the temperature in the box after the completion of the sintering of the compact must be lowered to near room temperature and the next cycle must be started, the cycle time becomes long. If the next cycle is started with insufficient cooling to reduce this time, the progress of degreasing will proceed rapidly due to the high temperature inside the furnace, causing the swelling and deformation of the sintered body. Becomes
【０００７】[0007]
【課題を解決するための手段】本発明は、叙上の欠点を
解決するものであって、その特徴とするところは、以下
のとおりである。The present invention solves the above drawbacks, and the features thereof are as follows.
【０００８】成形体及びこれを入れる箱内をあらかじめ
摂氏５０度から摂氏２００度に予熱する。この予熱は焼
結炉中あるいは脱脂炉中で実施するが、サイクルを短く
するためには別に設けたオーブン等で且つ大気圧下で実
施しても良い。予熱温度はバインダの種類で選定される
が，ポリプロピレンやアクリルを多く含むバインダでは
摂氏８０度から１３０度の範囲が望ましい。The molded body and the inside of the box in which it is placed are preheated from 50 ° C to 200 ° C in advance. This preheating is carried out in a sintering furnace or a degreasing furnace, but in order to shorten the cycle, it may be carried out in a separately provided oven or the like and under atmospheric pressure. The preheating temperature is selected depending on the type of binder, but a binder containing a large amount of polypropylene or acrylic is preferably in the range of 80 to 130 degrees Celsius.
【０００９】また、炉内に成形体の納められた箱を挿入
し、温度は予熱温度と同じに保つか、漸時上昇させるも
のとする。この漸昇速度は、望ましくは時間当り摂氏１
０度以内の速さで昇温させる。昇温させる理由は、予熱
した成形体を予熱炉から脱脂炉あるいは焼結炉へ移す際
の温度低下を補うためであり、また最終到達圧力が１０
−１〜１０−２トールと高い場合であっても脱脂の促進
を可能にさせるためである。Further, the box in which the molded body is housed is inserted into the furnace, and the temperature is maintained at the same as the preheating temperature or gradually increased. This rate of ascent is preferably 1 degree Celsius per hour.
The temperature is raised at a speed of 0 degree or less. The reason for raising the temperature is to compensate for the temperature decrease when the preheated compact is transferred from the preheating furnace to the degreasing furnace or the sintering furnace, and the final ultimate pressure is 10
This is because even if it is as high as −1 to 10 −2 Torr, it is possible to promote degreasing.
【００１０】炉内圧力は、大気圧から１０−１トール以
下の最終到達圧力まで１〜１０時間かけて漸次低下させ
る。所要時間および圧力のサイクルは成形体に欠陥が発
生しない範囲内で決定されるが、圧力対時間の関係は例
えば図２の如くである。最終到達圧力は１０−１トール
より高ければ効果は少なく、１０−６トールより低いの
はコストの面で実用的ではない。図２は、時間の経過に
伴う圧力の低下を示すものであり、実線は傾斜が一定な
低下，破線は階段状の低下，一点鎖線は不規則な低下を
示すものである。圧力のコントロールは、使用する真空
ポンプの稼働と合せ、炉内圧力を検知しながら雰囲気ガ
スの流量を増減させることによって行う。この時、ガス
化したバインダが炉壁の方向へ向けて流れないよう図１
に示す如く零囲気ガスを炉壁側から成形体の方向へに向
けて流すことが肝要である。The pressure in the furnace is gradually decreased from atmospheric pressure to the final ultimate pressure of 10 -1 Torr or less over 1 to 10 hours. The required time and the pressure cycle are determined within a range in which no defects occur in the molded body, and the pressure-time relationship is as shown in FIG. 2, for example. If the final ultimate pressure is higher than 10 -1 Torr, the effect is small, and if it is lower than 10 -6 Torr, it is not practical in terms of cost. FIG. 2 shows a decrease in pressure with the passage of time. A solid line shows a constant decrease, a broken line shows a stepwise decrease, and a chain line shows an irregular decrease. The pressure is controlled by increasing or decreasing the flow rate of the atmospheric gas while detecting the pressure inside the furnace in conjunction with the operation of the vacuum pump used. At this time, make sure that the gasified binder does not flow toward the furnace wall.
It is important to flow the zero atmosphere gas from the furnace wall side toward the molded body as shown in FIG.
【００１１】成形体へ向けて流す雰囲気ガスは、成形体
から気化して排出されるバインダと共に炉外へ放出され
る。The atmospheric gas flowing toward the compact is discharged outside the furnace together with the binder vaporized and discharged from the compact.
【００１２】[0012]
【作用】成形体の温度が、予熱温度に保たれた状態、あ
るいは漸次上昇しつつある状態で圧力が下がって行く
と、バインダのうちの、最も気化しやすい成分が気化し
始める。さらに圧力が下がると順次気化しやすい順に気
化する。この時、雰囲気ガスは、炉壁側から成形体の方
向へ向けて流す。When the pressure decreases while the temperature of the molded body is maintained at the preheating temperature or is gradually increasing, the most volatile component of the binder begins to vaporize. When the pressure is further reduced, it is vaporized in order of easy vaporization. At this time, the atmospheric gas flows from the furnace wall side toward the molded body.
【００１３】[0013]
【実施例１】平均粒径９．７μｍのＳＵＳ３１６Ｌ組成
の原料粉末１００重量部に対し、バインダ９．５重量部
を加えたコンパウンドを射出成形して１２×１１×７．
５ｍｍの直方体形状の成形体６Ａを形成した。ここでバ
インダは、ポリプロピレン５５重量％，パラフィンワッ
クス３０重量％，カルナウバワックス１４重量％，ジオ
クチルフタレート１重量％より成る。Example 1 A compound in which 9.5 parts by weight of a binder was added to 100 parts by weight of a raw material powder of SUS316L composition having an average particle size of 9.7 μm was injection-molded to obtain 12 × 11 × 7.
A 5 mm rectangular parallelepiped shaped molded body 6A was formed. Here, the binder comprises 55% by weight of polypropylene, 30% by weight of paraffin wax, 14% by weight of carnauba wax, and 1% by weight of dioctyl phthalate.
【００１４】この成形体６Ａを黒鉛製の箱５に納め、箱
ごと大気雰囲気中で図示しないオーブン内で摂氏１１０
度に加熱した。この箱をオーブンから取り出し、焼結炉
２０に挿入し、摂氏１１０度に加熱すると同時に、少量
の窒素ガスを炉壁側から成形体６Ａの方向へ向けて流し
ながら減圧した。はじめの１時間は１トールで、次の１
時間は０．１トールで、次の３時間は０．００１トール
で脱脂したあと、摂氏４５０度まで５時間かけて昇温し
て脱脂を終了した後、引き続き同一の炉で焼結を行っ
た。出来上った焼結体６Ａには、変形やクラックの発生
がなかった。焼結体６Ａのカーボン量は０．００５％で
あった。This molded body 6A was placed in a box 5 made of graphite, and the whole box was heated to 110 ° C. in an oven (not shown) in the atmosphere.
Heated every time. This box was taken out of the oven, inserted into the sintering furnace 20 and heated to 110 degrees Celsius, and at the same time, a small amount of nitrogen gas was flown from the furnace wall side toward the compact 6A to reduce the pressure. 1 hour for the first hour and 1 for the next
The time was 0.1 torr, the next 3 hours was degreased at 0.001 torr, the temperature was raised to 450 degrees Celsius over 5 hours to complete the degreasing, and then sintering was performed in the same furnace. . The finished sintered body 6A had no deformation or cracks. The carbon content of the sintered body 6A was 0.005%.
【００１５】[0015]
【実施例２】平均粒径５μｍのカーボニルニッケル粉４
％とカーボニル鉄粉９６％を混合し、さらに混合粉１０
０重量部に対しポリアミド樹脂８．５量部を加えたコン
パウンドを射出成形して１２×１１×７．５ｍｍの直方
体形状の成形体６Ｂを作成した。Example 2 Carbonyl nickel powder 4 having an average particle size of 5 μm
% And carbonyl iron powder 96% are mixed, and further mixed powder 10
A compound in which 8.5 parts by weight of polyamide resin was added to 0 part by weight was injection-molded to prepare a cuboid-shaped molded body 6B having a size of 12 × 11 × 7.5 mm.
【００１６】この成形体６Ｂを黒鉛製の箱に納め、箱ご
と大気雰囲気中で図示しないオーブンで摂氏１３０度に
加熱した。この箱をオーブンから取出し、焼結炉２０に
挿入するに当たり炉内の中央部位に置いて摂氏１３０度
に加熱し、さらに時間当り摂氏５度で昇温すると同時
に、少量の窒素ガスを炉壁側から成形体６Ｂの方向へ向
けて流しながら成形体近傍へ集め、この集めたガスを炉
壁の位置より一定距離離れた部位から炉外へ放出するよ
うになして、炉壁側と成形体近傍との間に圧力差をもた
らせながら減圧した。はじめの１時間は１トールで、次
の１時間は０．１トールで、次の２時間は０．０１トー
ルで脱脂したあと摂氏４５０度まで５時間かけて昇温し
て脱脂を終了した後、引き続き同一の炉で焼結を行っ
た。出来上った焼結体には、変形やクラックの発生がな
かった。This molded body 6B was placed in a box made of graphite, and the whole box was heated to 130 ° C. in an oven not shown in the atmosphere. When this box was taken out of the oven and inserted into the sintering furnace 20, it was placed in the central portion of the furnace and heated to 130 degrees Celsius, and the temperature was raised to 5 degrees Celsius per hour, and at the same time, a small amount of nitrogen gas was added to the furnace wall side. While flowing in the direction of the molded body 6B from near to the molded body, the collected gas is discharged to the outside of the furnace from a portion distant from the position of the furnace wall by a certain distance. The pressure was reduced while causing a pressure difference between After degreasing at 1 Torr for the first hour, 0.1 Torr for the next 1 hour, and 0.01 Torr for the next 2 hours, after heating to 450 degrees Celsius over 5 hours to complete the degreasing Then, sintering was performed in the same furnace. The resulting sintered body did not have any deformation or cracks.
【００１７】[0017]
【発明の効果】雰囲気ガスを炉壁側から成形体の方向へ
向けて流しているので、ガス化したバインダは、炉壁及
び断熱材に凝縮しながら付着することがない。また、成
形体を予熱するのでワンサイクルの時間が短縮できる。
さらに炉内の温度あるいは成形体が納められている箱の
温度を常温まで下げなくて良いので、サイクル時間が短
縮できる。さらにまた、低温での脱脂なので雰囲気ガス
による粉体の酸化のおそれがない。そのため、窒素，ア
ルゴンはもとより、空気も使用できる。Since the atmospheric gas is flowed from the furnace wall side toward the molded body, the gasified binder does not condense and adhere to the furnace wall and the heat insulating material. Moreover, since the molded body is preheated, the time for one cycle can be shortened.
Further, since it is not necessary to lower the temperature in the furnace or the temperature of the box in which the compact is housed to room temperature, the cycle time can be shortened. Furthermore, since the degreasing is performed at a low temperature, there is no fear of oxidizing the powder due to the atmospheric gas. Therefore, not only nitrogen and argon but also air can be used.
【図１】本発明における零囲気ガスの流れ方向を示す模
式図。FIG. 1 is a schematic view showing a flow direction of a zero atmosphere gas in the present invention.
【図２】本発明における圧力の時間依存性を示す模式
図。FIG. 2 is a schematic diagram showing the time dependence of pressure in the present invention.
【図３】従来の技術における温度と圧力のサイクル図。FIG. 3 is a cycle diagram of temperature and pressure in a conventional technique.
１・・・・・雰囲気ガスの入っているボンベ ２・・・・・炉体 ３・・・・・炉壁 ４・・・・・断熱材 ５・・・・・黒鉛製の箱 ６（６Ａ，６Ｂ）・・・・・成形体 ７・・・・・油拡散ポンプ ８・・・・・メカニカルブースターポンプ ９．・・・・油回転ポンプ １０・・・・・バインダのトラップ １１・・・・・雰囲気ガスの流れ 1 ... Cylinder containing atmosphere gas 2 ... Furnace body 3 ... Furnace wall 4 ... Insulation material 5 ... Graphite box 6 (6A , 6B) ... Molded body 7 ... Oil diffusion pump 8 ... Mechanical booster pump 9.・ ・ ・ ・ Oil rotary pump 10 ・ ・ ・ Binder trap 11 ・ ・ ・ Flow of atmospheric gas
Claims (7)
ウンドの成形体が、焼結によってつくられる焼結体とな
るに際し、あらかじめ摂氏５０度から摂氏２００度の範
囲に予熱した後、炉内温度をこの予熱温度に保ちなが
ら、雰囲気ガスを炉壁側から成形体の方向へ向け流しつ
つその流量を増減させ、同時に炉内圧力を大気圧から１
０−１トール以下の最終到達圧力まで、１〜１０時間か
けて漸減させる過程でバインダの除去を実施する金属粉
末成形体の脱脂方法。1. When a molded body of a compound composed of a metal powder and a binder is to be a sintered body produced by sintering, it is preheated in the range of 50 ° C. to 200 ° C. and then the temperature in the furnace is raised. While maintaining this preheating temperature, the atmospheric gas is made to flow from the furnace wall side toward the molded body and its flow rate is increased or decreased, and at the same time, the furnace pressure is changed from atmospheric pressure to 1
0 -1 until the following final ultimate pressure Torr, degreasing method of the metal powder compact to carry out removal of the binder in the process of gradually decreasing over 1 to 10 hours.
工程を炉内温度をさらに漸昇温させながらの工程に代え
て実施する請求項１の金属粉末成形体の脱脂方法。2. The degreasing method for a metal powder compact according to claim 1, wherein the step of maintaining the temperature in the furnace at a preheating temperature is replaced with the step of gradually increasing the temperature in the furnace.
バインダの除去を実施する炉とが夫々独立したものであ
る請求項１及び２記載の金属粉末成形体の脱脂方法。3. A furnace for preheating the compact,
The method for degreasing a metal powder compact according to claim 1 or 2, wherein the furnace for removing the binder is independent from each other.
１０−６トールの範囲であることを特徴とする請求項１
及び２記載の金属粉末成形体の脱脂方法。4. The final pressure achieved is in the range of 10 −1 Torr to 10 −6 Torr.
And the method for degreasing a metal powder compact according to 2.
の範囲であることを特徴とする請求項１及び２記載の金
属粉末成形体の脱脂方法。5. The method for degreasing a metal powder compact according to claim 1, wherein the preheating temperature is in the range of 80 to 130 degrees Celsius.
成形体近傍のガスを炉壁の位置より一定距離離れた部位
から炉外へ放出するようになして炉壁側と成形体近傍と
の間に圧力差をもたせながら実施する請求項１及び２記
載の金属粉末成形体の脱脂方法。6. The molded body is placed at a central portion in the furnace, and the gas in the vicinity of the molded body is discharged outside the furnace from a portion distant from the position of the furnace wall by a certain distance. The degreasing method for a metal powder compact according to claim 1 or 2, which is carried out while giving a pressure difference to the vicinity.
氏１０度以内であることを特徴とする請求項２記載の金
属粉末成形体の脱脂方法。7. The method for degreasing a metal powder compact according to claim 2, wherein the rate of increase in temperature in the furnace is within 10 degrees Celsius per hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4312595A JPH06122903A (en) | 1992-10-09 | 1992-10-09 | Method for degreasing metal powder compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4312595A JPH06122903A (en) | 1992-10-09 | 1992-10-09 | Method for degreasing metal powder compact |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06122903A true JPH06122903A (en) | 1994-05-06 |
Family
ID=18031095
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4312595A Pending JPH06122903A (en) | 1992-10-09 | 1992-10-09 | Method for degreasing metal powder compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06122903A (en) |
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| US8235710B2 (en) | 2005-06-13 | 2012-08-07 | Basf Se | Device and method for continuously and catalytically removing binder, with improved flow conditions |
| CN103706790A (en) * | 2013-12-19 | 2014-04-09 | 宁波恒普真空技术有限公司 | Automatic temperature control method for vacuum degreasing sintering furnace trap |
| CN108220895A (en) * | 2018-01-15 | 2018-06-29 | 福建阿石创新材料股份有限公司 | Plasma heating formula high temperature oxygen supply |
| CN112355304A (en) * | 2020-10-14 | 2021-02-12 | 陕西斯瑞新材料股份有限公司 | Processing technology for preparing CuW60-CuW90 metal profile part through injection molding |
-
1992
- 1992-10-09 JP JP4312595A patent/JPH06122903A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8235710B2 (en) | 2005-06-13 | 2012-08-07 | Basf Se | Device and method for continuously and catalytically removing binder, with improved flow conditions |
| CN103706790A (en) * | 2013-12-19 | 2014-04-09 | 宁波恒普真空技术有限公司 | Automatic temperature control method for vacuum degreasing sintering furnace trap |
| CN108220895A (en) * | 2018-01-15 | 2018-06-29 | 福建阿石创新材料股份有限公司 | Plasma heating formula high temperature oxygen supply |
| CN108220895B (en) * | 2018-01-15 | 2019-10-08 | 福建阿石创新材料股份有限公司 | Plasma heating formula high temperature oxygen supply |
| CN112355304A (en) * | 2020-10-14 | 2021-02-12 | 陕西斯瑞新材料股份有限公司 | Processing technology for preparing CuW60-CuW90 metal profile part through injection molding |
| CN112355304B (en) * | 2020-10-14 | 2022-10-25 | 陕西斯瑞新材料股份有限公司 | Processing technology for preparing CuW60-CuW90 metal section part through injection molding |
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