JP2000290703A - Manufacture of lubricant for warm die lubrication, iron- base powder mixture for warm die lubricating compaction, high density green compact of iron-base powder, and high density iron-base sintered compact - Google Patents

Manufacture of lubricant for warm die lubrication, iron- base powder mixture for warm die lubricating compaction, high density green compact of iron-base powder, and high density iron-base sintered compact

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Publication number
JP2000290703A
JP2000290703A JP11308590A JP30859099A JP2000290703A JP 2000290703 A JP2000290703 A JP 2000290703A JP 11308590 A JP11308590 A JP 11308590A JP 30859099 A JP30859099 A JP 30859099A JP 2000290703 A JP2000290703 A JP 2000290703A
Authority
JP
Japan
Prior art keywords
lubricant
iron
powder
melting point
temperature
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
Application number
JP11308590A
Other languages
Japanese (ja)
Other versions
JP3931503B2 (en
Inventor
Shigeru Unami
繁 宇波
Yukiko Ozaki
由紀子 尾崎
Satoshi Uenosono
聡 上ノ薗
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JFE Steel Corp
Original Assignee
Kawasaki Steel Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kawasaki Steel Corp filed Critical Kawasaki Steel Corp
Priority to JP30859099A priority Critical patent/JP3931503B2/en
Priority to CA2356253A priority patent/CA2356253C/en
Priority to EP00948302A priority patent/EP1145788B1/en
Priority to PCT/JP2000/005089 priority patent/WO2001032337A1/en
Priority to US09/631,033 priority patent/US6355208B1/en
Priority to TW089115743A priority patent/TW486396B/en
Publication of JP2000290703A publication Critical patent/JP2000290703A/en
Application granted granted Critical
Publication of JP3931503B2 publication Critical patent/JP3931503B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To provide a method of manufacturing a high density green compact of iron-base powder, capable of giving a high density green compact by a single compaction, and a method of manufacturing a sintered compact using the green compact. SOLUTION: A lubricant, which consists of 0.5-80 wt.% lubricant having a melting point higher than the compaction temperature and the balance lubricant having a melting point lower than the compaction temperature, is allowed to adhere to the surface of a die by electrification. After the die is filled with a heated iron-base powder mixture, the powder mixture is compacted at prescribed temperature into a green compact or the green compact is further sintered. The iron-base powder mixture contains an iron-base powder and a compaction lubricant in which a lubricant having a low melting point not higher than the prescribed compaction temperature comprises 10-75 mass % of the total amount of lubricant and the balance is composed of a lubricant having a melting point higher than a prescribed compaction temperature.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、粉末冶金用鉄基粉
末成形体および鉄基焼結体の製造方法に係り、とくに、
温間成形により高密度の鉄基粉末成形体を製造する際に
使用する潤滑剤の改善に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an iron-based powder compact for powder metallurgy and a method for producing an iron-based sintered body.
The present invention relates to improvement of a lubricant used when manufacturing a high-density iron-based powder compact by warm compaction.

【0002】[0002]

【従来の技術】粉末冶金用鉄基粉末成形体は、鉄基粉末
に、銅粉、黒鉛粉などの合金粉末と、さらにステアリン
酸亜鉛、ステアリン酸鉛等の潤滑剤を混合した鉄基粉末
混合物を金型に充填したのち、加圧成形し製造されるの
が一般的である。成形体の密度としては、6.6 〜7.1Mg/
m3が一般的である。
2. Description of the Related Art An iron-based powder compact for powder metallurgy is a mixture of iron-based powder, alloy powder such as copper powder and graphite powder, and a lubricant such as zinc stearate and lead stearate. After filling in a mold, it is generally manufactured by pressure molding. The density of the compact is 6.6 to 7.1 Mg /
m 3 is common.

【0003】これら鉄基粉末成形体は、さらに焼結処理
を施され焼結体とされ、さらに必要に応じてサイジング
や切削加工が施され、粉末冶金製品とされる。また、さ
らに高強度が必要な場合は焼結後に浸炭熱処理や光輝熱
処理を施されることもある。この粉末冶金技術により、
高寸法精度の複雑な形状の部品をニアネット形状に生産
することが可能となり、従来の製造方法に比べ大幅に切
削コストの低減が可能である。
[0003] These iron-based powder compacts are further subjected to a sintering process to form sintered compacts, and further subjected to sizing and cutting as required, to be powder metallurgy products. If higher strength is required, carburizing heat treatment or bright heat treatment may be performed after sintering. With this powder metallurgy technology,
It is possible to produce a component having a complicated shape with high dimensional accuracy in a near net shape, and it is possible to greatly reduce the cutting cost as compared with the conventional manufacturing method.

【0004】さらに、最近では、切削加工の省略による
コスト削減のための一層の高寸法精度化や、部品の小型
軽量化のための高強度化が鉄系の粉末冶金製品へ強く要
求されている。粉末冶金製品(焼結部品)の高強度化に
対しては、成形体の高密度化による焼結部品の高密度化
が有効である。焼結部品の密度が高いほど、部品中の空
孔が減少し、引張強さ、衝撃値や疲労強度などの機械的
特性が向上する。
Further, recently, there has been a strong demand for iron-based powder metallurgy products to have higher dimensional accuracy for cost reduction by omitting cutting work and higher strength for smaller and lighter parts. . To increase the strength of powder metallurgy products (sintered parts), it is effective to increase the density of sintered parts by increasing the density of a compact. The higher the density of the sintered part, the less porosity in the part and the better the mechanical properties such as tensile strength, impact value and fatigue strength.

【0005】鉄基粉末成形体の高密度化を可能とする成
形方法として、鉄基粉末混合物を通常の成形と焼結を施
したのち、さらに成形・焼結を繰り返して行う2回成形
2回焼結法や、1回成形1回焼結後熱間で鍛造する焼結
鍛造法などが提案されている。また、例えば、特開平2-
156002号公報、特公平7-103404号公報、USP 第5,256,18
5 号公報、USP 第5,368,630 号公報には、金属粉末を加
熱しつつ成形する温間成形技術が開示されている。この
温間成形技術は、温間成形時に潤滑剤の一部または全部
を溶融させて粉末粒子間に潤滑剤を均一に分散させ、粒
子間および成形体と金型の間の摩擦抵抗を下げ成形性を
向上させようとするものであり、上記した高密度成形体
の製造方法のなかではコスト的には最も有利であると考
えられている。この温間成形技術によれば、Fe-4Ni-0.5
Mo-1.5Cu系の部分合金化鉄粉に0.5 質量%の黒鉛、0.6
質量%の潤滑剤を配合した鉄基粉末混合物を150 ℃で7t
/cm2(686 MPa )の圧力で成形した場合、7.30Mg/m3
度の成形体が得られる。
[0005] As a molding method capable of increasing the density of an iron-based powder compact, a conventional molding and sintering of an iron-based powder mixture is performed, and then molding and sintering are repeated twice. A sintering method and a sintering forging method in which hot forging is performed after one molding and one sintering have been proposed. Also, for example, Japanese Patent Application Laid-Open
No. 156002, Japanese Patent Publication No. Hei 7-103404, USP 5,256,18
No. 5, US Pat. No. 5,368,630 discloses a warm forming technique for forming a metal powder while heating it. This warm forming technology melts part or all of the lubricant during warm forming to evenly disperse the lubricant between the powder particles, thereby lowering the frictional resistance between the particles and between the compact and the mold. It is intended to improve the properties, and is considered to be the most advantageous in terms of cost among the above-described methods for producing a high-density molded article. According to this warm forming technology, Fe-4Ni-0.5
Mo-1.5Cu partially alloyed iron powder with 0.5 mass% graphite, 0.6 mass%
7 tons of iron-based powder mixture containing 150% by mass of lubricant
When molded at a pressure of / cm 2 (686 MPa), a molded body of about 7.30 Mg / m 3 is obtained.

【0006】[0006]

【発明が解決しようとする課題】しかしながら、特開平
2-156002号公報、特公平7-103404号公報、USP 第5,256,
185 号公報、USP 第5,368,630 号公報に記載された技術
では、粉末混合物の流動性が不十分で、生産性が低下す
るうえ、成形体の密度にばらつきが生じ、焼結体の特性
が変動するという問題があり、さらに、成形時の抜き出
し力が高く、成形体表面に疵が発生するとともに金型の
寿命が短いなどの問題があった。
SUMMARY OF THE INVENTION
2-156002, JP-B-7-103404, USP 5,256,
In the technology described in Japanese Patent No. 185, USP 5,368,630, the fluidity of the powder mixture is insufficient, the productivity is reduced, and the density of the compact is varied, and the characteristics of the sintered body fluctuate. In addition, there is a problem that the extraction force at the time of molding is high, flaws are generated on the surface of the molded body, and the life of the mold is short.

【0007】さらに、これらの温間成形技術では、粒子
間および成形体と金型の間の摩擦抵抗を下げ成形性を向
上させる目的で、鉄基粉末混合物中に潤滑剤を含有させ
るが、潤滑剤は、温間成形時にその一部又は全部が溶融
して成形体表面付近に押し出され、その後の焼結処理に
より、加熱分解あるいは蒸発して成形体から逸散し、焼
結体表面付近に粗大な空孔を形成する。そのため、焼結
体の機械的強度を低下させるという問題があった。
Furthermore, in these warm forming techniques, a lubricant is contained in the iron-based powder mixture for the purpose of reducing the frictional resistance between the particles and between the compact and the mold and improving the formability. During warm forming, part or all of the agent is melted and extruded near the surface of the molded body, and is heated and decomposed or evaporated by the subsequent sintering process and escapes from the molded body, and near the surface of the sintered body. Form coarse pores. Therefore, there is a problem that the mechanical strength of the sintered body is reduced.

【0008】この問題を解決するために、特開平8-1002
03号公報には常温または温間成形において、帯電させた
潤滑剤粉末を金型表面に塗布して、鉄基粉末混合物中の
潤滑剤量を低減し、高密度の成形体を成形する技術が開
示されている。しかしながら、この方法では、塗布する
潤滑剤の種類が単体であるため、その融点前後で潤滑剤
の形態が変わり、潤滑機能が著しく変化する。このた
め、成形温度範囲が潤滑剤の融点によって限定されると
いう問題があった。さらに金型潤滑剤を金型表面に塗布
し鉄基粉末混合物中の潤滑剤量を低減したとしても、混
合する潤滑剤の成分によっては量の低減によって潤滑効
果を失い、圧粉密度の増大が実現できないという問題も
生じている。
In order to solve this problem, Japanese Patent Application Laid-Open No. Hei 8-1002
No. 03 discloses a technique for forming a high-density compact by applying a charged lubricant powder to a mold surface at room temperature or warm molding to reduce the amount of lubricant in the iron-based powder mixture. It has been disclosed. However, in this method, since the type of the lubricant to be applied is a single substance, the form of the lubricant changes around its melting point, and the lubricating function changes significantly. For this reason, there is a problem that the molding temperature range is limited by the melting point of the lubricant. Furthermore, even if the mold lubricant is applied to the surface of the mold to reduce the amount of lubricant in the iron-based powder mixture, the lubrication effect is lost due to the decrease in the amount of lubricant depending on the components of the mixed lubricant, and the green compact density increases. There is also a problem that it cannot be realized.

【0009】また、自動車用部品の高強度化という観点
と、コストという観点からは、更なる高密度の成形体
を、しかも1回の成形で得ることのできる、高密度鉄基
粉末成形体の製造方法の開発が望まれていた。本発明
は、上記した従来技術の問題を有利に解決し、例えば、
Fe-4Ni-0.5Mo-1.5Cu組成の部分合金化鉄粉に0.5 重量%
の黒鉛粉を混合した鉄基粉末混合物を温間加圧成形した
場合には7.4 Mg/m3 以上の、高密度の成形体を1回の成
形で得ることができる、高密度鉄基粉末成形体の製造方
法を提案することを第1の目的とする。また、本発明
は、鉄基粉末成形体を焼結処理して高密度の鉄基焼結体
を得ることができる、高密度鉄基焼結体の製造方法を提
案することを第2の目的とする。
In addition, from the viewpoint of increasing the strength of automobile parts and the cost, a high-density iron-based powder compact that can be obtained by a single compacting process is obtained. Development of a manufacturing method was desired. The present invention advantageously solves the above-mentioned problems of the prior art, for example,
0.5% by weight in partially alloyed iron powder with Fe-4Ni-0.5Mo-1.5Cu composition
High-density iron-based powder molding, in which a high-density compact of 7.4 Mg / m 3 or more can be obtained by one molding when warm-press molding an iron-based powder mixture containing A first object is to propose a method for producing a body. A second object of the present invention is to propose a method for producing a high-density iron-based sintered body, which can obtain a high-density iron-based sintered body by sintering an iron-based powder compact. And

【0010】[0010]

【課題を解決するための手段】本発明者らは、温間成形
技術および金型潤滑成形技術を利用して上記した課題を
達成するために、金型潤滑用潤滑剤および鉄基粉末混合
粉の潤滑剤配合について鋭意検討を行った。その結果、
抜き出し力を低減させるため、予熱した金型表面に帯電
付着により付着させることのできる金型潤滑用潤滑剤と
して、所定の加圧成形の温度以下の低い融点を有する潤
滑剤とその温度より高い融点を有する潤滑剤を適正な配
合で混合した潤滑剤がよいという知見を得た。
Means for Solving the Problems In order to achieve the above-mentioned object by using the warm forming technique and the mold lubricating molding technique, the present inventors have proposed a lubricant for mold lubrication and a mixed powder of iron-based powder. The intensive investigation was conducted on the lubricant compounding. as a result,
As a lubricant for mold lubrication that can be adhered to the preheated mold surface by electrostatic adhesion in order to reduce the ejection force, a lubricant with a low melting point below the temperature of the specified pressure molding and a melting point higher than that temperature It has been found that a lubricant obtained by mixing a lubricant having the following formula with an appropriate blend is preferable.

【0011】本発明は、上記した知見に基づき、さらに
検討して完成されたものである。すなわち、第1の本発
明は、粉末を予熱された金型で加圧成形する際に金型表
面に帯電付着させて使用する温間金型潤滑用潤滑剤であ
って、所定の加圧成形の温度より高い融点を有する潤滑
剤と、前記所定の加圧成形の温度以下の低い融点を有す
る潤滑剤との混合物であることを特徴とする温間金型潤
滑用潤滑剤である。また、第1の本発明では、粉末を予
熱された金型で加圧成形する際に金型表面に帯電付着さ
せて使用する温間金型潤滑用潤滑剤であって、所定の加
圧成形の温度より高い融点を有する潤滑剤を 0.5〜80質
量%含有し、残部が前記所定の加圧成形の温度以下の低
い融点を有する潤滑剤であることを特徴とする温間金型
潤滑用潤滑剤としてもよく、また、本発明では、前記所
定の加圧成形の温度より高い融点を有する潤滑剤は、金
属石鹸、熱可塑性樹脂、熱可塑性エラストマー、層状の
結晶構造を有する無機または有機潤滑剤のうちから選ば
れた1種または2種以上であるのが好ましく、また、本
発明では、前記所定の加圧成形の温度以下の低い融点を
有する潤滑剤は、金属石鹸、アミド系ワックス、ポリエ
チレンおよびこれらのうちの2種以上の共溶融物のうち
から選ばれた1種または2種以上とするのが好ましい。
The present invention has been completed by further study based on the above findings. That is, a first aspect of the present invention relates to a lubricant for warm mold lubrication, which is used by charging and adhering a powder to the surface of a mold when the powder is compacted by a preheated mold, wherein And a lubricant having a melting point lower than the temperature of the predetermined pressure molding and a lubricant having a melting point lower than the predetermined pressure forming temperature. In the first aspect of the present invention, there is provided a lubricant for warm mold lubrication, which is used by charging and adhering the powder to the surface of the mold when the powder is compacted by a preheated mold. A lubricant having a melting point higher than the temperature of 0.5 to 80% by mass, and the remainder being a lubricant having a melting point lower than the predetermined pressure forming temperature. In the present invention, the lubricant having a melting point higher than the predetermined pressure molding temperature may be a metal soap, a thermoplastic resin, a thermoplastic elastomer, an inorganic or organic lubricant having a layered crystal structure. Preferably, the lubricant having a low melting point not higher than the predetermined pressure molding temperature is metal soap, amide wax, polyethylene or the like. And two or more of these Preferably with one or more members selected from among the melt.

【0012】また、第2の本発明は、鉄基粉末と、粉末
成形用潤滑剤とを含む鉄基粉末混合物であって、前記粉
末成形用潤滑剤が、粉末成形用潤滑剤全量の10〜75質量
%の、加圧成形の温度以下の低い融点を有する潤滑剤を
含み、残部が、加圧成形の温度より高い融点を有する潤
滑剤であることを特徴とする温間金型潤滑成形用鉄基粉
末混合物であり、また、本発明では、前記粉末成形用潤
滑剤の含有量を、0.05〜0.40質量%とするのが好まし
い。
[0012] A second aspect of the present invention is an iron-based powder mixture comprising an iron-based powder and a powder-forming lubricant, wherein the powder-forming lubricant is 10 to 10% of the total amount of the powder-forming lubricant. 75% by mass of a lubricant having a melting point lower than the pressing temperature, the balance being a lubricant having a melting point higher than the pressing temperature, for lubricating in warm molds. It is an iron-based powder mixture, and in the present invention, the content of the powder-forming lubricant is preferably 0.05 to 0.40% by mass.

【0013】また、第3の本発明は、金型に、加熱した
鉄基粉末混合物を充填したのち、所定の温度で加圧成形
する鉄基粉末成形体の製造方法において、前記金型を、
予熱され、表面に、温間金型潤滑用潤滑剤を帯電付着さ
せた金型とし、前記温間金型潤滑用潤滑剤を、 0.5〜80
質量%の、所定の加圧成形の温度より高い融点をもつ潤
滑剤を含み、残部が、所定の加圧成形の温度以下の低い
融点をもつ潤滑剤である潤滑剤とし、さらに前記鉄基粉
末混合物が鉄基粉末と粉末成形用潤滑剤とを含み、前記
粉末成形用潤滑剤が粉末成形用潤滑剤全量の10〜75質量
%の、所定の加圧成形の温度以下の低い融点をもつ潤滑
剤を含み、25〜90質量%の、所定の加圧成形の温度より
高い融点をもつ潤滑剤である混合潤滑剤とすることを特
徴とする高密度鉄基粉末成形体の製造方法であり、ま
た、本発明では、前記温間金型潤滑用潤滑剤における前
記所定の加圧成形の温度より高い融点を有する潤滑剤
を、金属石鹸、熱可塑性樹脂、熱可塑性エラストマー、
層状の結晶構造を有する無機または有機潤滑剤のうちか
ら選ばれた1種または2種以上とするのが好ましく、ま
た、本発明では、前記温間金型潤滑用潤滑剤における前
記所定の加圧成形の温度以下の低い融点を有する潤滑剤
を、金属石鹸、アミド系ワックス、ポリエチレンおよび
これらのうちの2種以上の共溶融物のうちから選ばれた
1種または2種以上とするのが好ましく、また、本発明
では、前記粉末成形用潤滑剤の含有量を、0.05〜0.40質
量%とするのが好ましい。
[0013] Further, a third aspect of the present invention provides a method for producing an iron-based powder compact, which comprises filling a mold with a heated iron-based powder mixture and then press-forming at a predetermined temperature.
The mold is preheated and the surface is lubricated with a lubricant for warm mold lubrication, and the lubricant for warm mold lubrication is 0.5 to 80
% By mass of a lubricant having a melting point higher than a predetermined pressing temperature, the balance being a lubricant having a lower melting point lower than or equal to a predetermined pressing temperature; The mixture contains an iron-based powder and a powder-forming lubricant, wherein the powder-forming lubricant has a low melting point of 10 to 75% by mass of the total amount of the powder-forming lubricant, which is not higher than a predetermined pressing temperature. A high-density iron-based powder molded body, characterized in that the mixed lubricant is a lubricant having a melting point higher than a predetermined pressing temperature of 25 to 90% by mass, including Further, in the present invention, the lubricant having a melting point higher than the predetermined pressure molding temperature in the lubricant for warm mold lubrication, metal soap, thermoplastic resin, thermoplastic elastomer,
It is preferable to use one or more selected from inorganic or organic lubricants having a layered crystal structure, and in the present invention, the predetermined pressurization in the warm mold lubricant is performed. The lubricant having a low melting point not higher than the molding temperature is preferably one or more selected from metal soaps, amide waxes, polyethylene and co-melts of two or more thereof. In the present invention, the content of the powder molding lubricant is preferably 0.05 to 0.40% by mass.

【0014】本発明によれば、一回の加圧成形で高密度
の成形体を容易に得ることができる。また、第4の本発
明は、上記した高密度鉄基粉末成形体の製造方法のいず
れかで製造された鉄基粉末成形体に、さらに焼結処理を
施し鉄基焼結体とすることを特徴とする高密度鉄基焼結
体の製造方法である。
According to the present invention, a high-density molded body can be easily obtained by one press molding. Further, a fourth aspect of the present invention is to provide an iron-based powder compact produced by any of the above-described methods for producing a high-density iron-based powder compact, which is further subjected to a sintering process to obtain an iron-based sintered compact. This is a method for producing a high-density iron-based sintered body, which is a feature.

【0015】[0015]

【発明の実施の形態】本発明では、金型に、加熱した鉄
基粉末混合物を充填したのち、所定の温度で加圧成形
し、鉄基粉末成形体とする。本発明では、成形に用いる
金型は、予め所定の温度に予熱される。金型の予熱温度
は、鉄基粉末混合物が所定の加圧成形の温度に保持でき
る温度であればよく、とくに限定する必要はないが、所
定の加圧成形の温度より20〜60℃高い温度とするのが望
ましい。
BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, a mold is filled with a heated iron-based powder mixture and then molded under pressure at a predetermined temperature to obtain a molded iron-based powder. In the present invention, the mold used for molding is preheated to a predetermined temperature. The preheating temperature of the mold is not particularly limited as long as the iron-based powder mixture can be maintained at a predetermined pressure molding temperature, and is not particularly limited, but is a temperature 20 to 60 ° C. higher than the predetermined pressure molding temperature. It is desirable that

【0016】予熱された金型に、帯電された金型潤滑用
潤滑剤を導入し、金型表面に帯電付着させる。金型潤滑
用潤滑剤(固体粉末)は金型潤滑装置(例えば、Gasbar
re社製Die Wall Lubricant System )に装入し、潤滑剤
(固体)粉末と装置内壁の接触帯電により帯電されるの
が好ましい。帯電された金型潤滑用潤滑剤は、噴射によ
り金型内に導入され、金型表面に帯電付着される。金型
表面に帯電付着させる金型潤滑用潤滑剤の付着量は、5
〜100g/m2 とするのが好ましい。付着量が5g/m2未満で
は潤滑効果が不足し、成形後の抜き出し力が高くなり、
100g/m2 を超えると、成形体表面に潤滑剤が残存し,成
形体の外観不良となる。
The charged mold lubricating lubricant is introduced into the preheated mold, and is charged and adhered to the mold surface. Lubricating lubricant (solid powder) for mold lubrication is used for mold lubrication equipment (eg, Gasbar
It is preferably charged into a Die Wall Lubricant System (manufactured by re) and charged by contact charging between the lubricant (solid) powder and the inner wall of the device. The charged lubricant for mold lubrication is introduced into the mold by injection, and is charged and adhered to the mold surface. The amount of the lubricant for mold lubrication to be charged and adhered to the mold surface is 5
It is preferably set to 100100 g / m 2 . When the adhesion amount is less than 5 g / m 2 , the lubricating effect is insufficient, and the withdrawal force after molding is increased,
If it exceeds 100 g / m 2 , the lubricant remains on the surface of the molded body, resulting in poor appearance of the molded body.

【0017】粉末を予熱した金型で加圧成形する際に金
型表面に帯電付着させて使用する温間金型潤滑用潤滑剤
は、所定の加圧成形の温度より高い融点を有する潤滑剤
を 0.5〜80質量%含有し、残部が前記所定の加圧成形の
温度以下の低い融点を有する潤滑剤からなる混合潤滑剤
とする。なお、本発明でいう所定の加圧成形の温度は、
加圧成形時の金型表面での温度をいうものとする。
The lubricant for warm mold lubrication, which is used by charging and adhering to the surface of the mold when the powder is molded under pressure with a preheated mold, is a lubricant having a melting point higher than a predetermined molding temperature. And 0.5 to 80% by mass, and the balance being a lubricant having a low melting point not higher than the predetermined pressure molding temperature. The predetermined pressure molding temperature in the present invention is:
It means the temperature on the mold surface during pressure molding.

【0018】所定の加圧成形の温度より高い融点を有す
る潤滑剤は、成形時、金型内で未溶融であり金型内で
「ころ」のような固体潤滑剤の働きをし、抜き出し力を
低下させるとともに、さらに、溶融あるいは部分溶融し
た潤滑剤(所定の加圧成形の温度より低い融点を有する
潤滑剤)の金型内での移動を防止し、成形体と金型表面
との摩擦抵抗を低減して抜き出し力の増加を防止する役
割を有している。
A lubricant having a melting point higher than a predetermined pressure molding temperature is unmelted in a mold at the time of molding, acts as a solid lubricant such as a "roller" in the mold, and has a drawing force. And also prevents the molten or partially melted lubricant (lubricant having a melting point lower than the predetermined pressure molding temperature) from moving in the mold, and the friction between the molded body and the mold surface. It has a role of reducing resistance and preventing an increase in extraction force.

【0019】所定の加圧成形の温度より高い融点を有す
る潤滑剤の含有量が、 0.5質量%未満では、加圧成形の
温度より低い融点の潤滑剤が多くなり、潤滑剤が溶融す
る量が多くなり、潤滑剤が移動し金型表面で均一な分布
とならず、成形体と金型表面との摩擦抵抗が増大して抜
き出し力の低減効果が少ない。一方、80質量%を超える
と、金型内で溶融しない潤滑剤の量が多くなりすぎ、金
型表面の潤滑剤の分布が不均一となり、金型潤滑が不十
分で抜き出し力が増加する。このため、温間金型潤滑用
潤滑剤における所定の加圧成形の温度より高い融点を有
する潤滑剤の配合量は、 0.5〜80質量%の範囲に限定し
た。
If the content of the lubricant having a melting point higher than the predetermined pressure molding temperature is less than 0.5% by mass, the amount of the lubricant having a melting point lower than the pressure molding temperature increases, and the amount of the lubricant to be melted is reduced. As a result, the lubricant moves and does not form a uniform distribution on the surface of the mold, the frictional resistance between the molded body and the surface of the mold increases, and the effect of reducing the extraction force is small. On the other hand, if it exceeds 80% by mass, the amount of the lubricant that does not melt in the mold becomes too large, the distribution of the lubricant on the mold surface becomes uneven, and the mold lubrication is insufficient and the extraction force increases. For this reason, the blending amount of the lubricant having a melting point higher than the predetermined pressure molding temperature in the warm mold lubricant is limited to the range of 0.5 to 80% by mass.

【0020】金型潤滑用潤滑剤における残部は、所定の
加圧成形の温度以下の低い融点を有する潤滑剤である。
所定の加圧成形の温度以下の低い融点を有する潤滑剤
は、加圧成形の温度で、溶融あるいは部分溶融し、金型
表面でグリースのような状態になり、抜き出し力を下げ
る効果を有している。温間金型潤滑用潤滑剤における所
定の加圧成形の温度より高い融点を有する潤滑剤は、金
属石鹸、熱可塑性樹脂、熱可塑性エラストマー、層状の
結晶構造を有する無機潤滑剤または有機潤滑剤のうちか
ら選ばれた1種または2種以上とするのが好ましい。所
定の加圧成形の温度に応じ、下記した潤滑剤から適宜選
択できる。
The remainder of the lubricant for mold lubrication is a lubricant having a low melting point not higher than a predetermined pressure molding temperature.
Lubricant having a low melting point below the predetermined pressure molding temperature, melts or partially melts at the pressure molding temperature, has a grease-like state on the mold surface, and has the effect of lowering the extraction force. ing. Lubricants having a melting point higher than the predetermined pressure molding temperature in warm mold lubricating lubricants include metal soaps, thermoplastic resins, thermoplastic elastomers, and inorganic or organic lubricants having a layered crystal structure. It is preferable to use one or two or more selected from them. The lubricant can be appropriately selected from the following lubricants according to the predetermined pressure molding temperature.

【0021】金属石鹸としては、ステアリン酸リチウ
ム、ヒドロキシステアリン酸リチウム等が好ましい。ま
た、熱可塑性樹脂としては、ポリスチレン、ポリアミ
ド、フッ素樹脂等が好適である。熱可塑性エラストマー
としては、ポリスチレン系エラストマー、ポリアミド系
エラストマー等が好適である。また、層状の結晶構造を
有する無機潤滑剤としては、黒鉛、MoS2、フッ化炭素の
いずれでも良く、粒度は細かいほど、抜き出し力の低減
に有効である。層状の結晶構造を有する有機潤滑剤とし
ては、メラミン−シアヌル酸付加物(MCA )、N −アル
キルアスパラギン酸−β−アルキルエステルのいずれも
使用することができる。
As the metal soap, lithium stearate, lithium hydroxystearate and the like are preferable. Further, as the thermoplastic resin, polystyrene, polyamide, fluororesin and the like are preferable. As the thermoplastic elastomer, a polystyrene-based elastomer, a polyamide-based elastomer, and the like are preferable. Further, the inorganic lubricant having a layered crystal structure may be any of graphite, MoS 2 , and fluorocarbon. The finer the particle size, the more effective it is in reducing the extraction force. As the organic lubricant having a layered crystal structure, any of melamine-cyanuric acid adduct (MCA) and N-alkyl aspartic acid-β-alkyl ester can be used.

【0022】一方、温間金型潤滑用潤滑剤における所定
の加圧成形の温度以下の低い融点を有する潤滑剤は、所
定の加圧成形の温度で金型表面で溶融あるいは部分溶融
する低融点で帯電しやすい潤滑剤とするのが望ましい。
このような潤滑剤としては、金属石鹸、アミド系ワック
ス、ポリエチレンおよびこれらのうちの2種以上の共溶
融物のうちから選ばれた1種または2種以上とするのが
好ましい。所定の加圧成形の温度に応じ、下記した潤滑
剤から選択できる。金属石鹸としては、ステアリン酸亜
鉛、ステアリン酸カルシウムが好適であり、アミド系ワ
ックスとしては、エチレンビスステアロアミド、ステア
リン酸モノアミド等が好適であり、共溶融物としては、
エチレンビスステアロアミドとポリエチレンの共溶融
物、エチレンビスステアロアミドとステアリン酸亜鉛の
共溶融物、エチレンビスステアロアミドとステアリン酸
カルシウムの共溶融物が好適である。
On the other hand, a lubricant having a low melting point not higher than a predetermined pressure molding temperature in a warm mold lubrication lubricant has a low melting point which melts or partially melts on a mold surface at a predetermined pressure molding temperature. It is desirable to use a lubricant which is easily charged with a lubricant.
As such a lubricant, it is preferable to use one or more selected from metal soap, amide wax, polyethylene and a co-melt of two or more thereof. The following lubricants can be selected according to the predetermined pressure molding temperature. As the metal soap, zinc stearate and calcium stearate are preferable, and as the amide-based wax, ethylenebisstearamide, stearic acid monoamide, and the like are preferable.
A co-melt of ethylene bis-stearamide and polyethylene, a co-melt of ethylene bis-stearamide and zinc stearate, and a co-melt of ethylene bis-stearamide and calcium stearate are preferred.

【0023】ついで、金型潤滑用潤滑剤を帯電付着され
た金型に、加熱された鉄基粉末混合物を装入し、加圧成
形し、成形体とする。鉄基粉末混合物の加熱温度は、70
〜200 ℃とするのが好ましい。加熱温度が70℃未満で
は、鉄粉の降伏応力が高く、成形体の密度が低下する。
一方、加熱温度が200 ℃を超えても実質的に密度の増加
はなく、鉄粉の酸化の懸念が生じるため、鉄基粉末混合
物の加熱温度は、70〜200 ℃の範囲とするのが望まし
い。
Next, the heated iron-based powder mixture is charged into a mold to which a lubricant for mold lubrication has been charged and then molded under pressure to obtain a molded body. The heating temperature of the iron-based powder mixture is 70
The temperature is preferably set to 200 ° C. If the heating temperature is lower than 70 ° C., the yield stress of the iron powder is high, and the density of the compact decreases.
On the other hand, even if the heating temperature exceeds 200 ° C., there is substantially no increase in density, and there is a concern that iron powder may be oxidized. .

【0024】鉄基粉末混合物は、鉄基粉末に潤滑剤(粉
末成形用潤滑剤)あるいはさらに合金用粉末を混合した
ものである。鉄基粉末と粉末成形用潤滑剤あるいはさら
に合金用粉末との混合は、とくに限定する必要はなく、
通常公知の混合方法がいずれも好適に利用できる。なか
でも、鉄基粉末に合金用粉末を混合する場合には、含有
粉末の偏析を避けるため、鉄基粉末、合金用粉末に粉末
成形用潤滑剤の1部を加えて1次混合したのち、さらに
粉末成形用前記潤滑剤のうち少なくとも1種の潤滑剤の
融点以上に加熱しつつ撹拌して、前記粉末成形用潤滑剤
のうち少なくとも1種の潤滑剤を溶融し、溶融後の混合
物を撹拌しながら冷却し、前記鉄基粉末表面に溶融した
潤滑剤を固着させることによって前記合金用粉末を付着
させた後、粉末成形用潤滑剤の残部を加えて2次混合す
る混合方法が好ましい。
The iron-based powder mixture is obtained by mixing a lubricant (powder-forming lubricant) or an alloy powder with iron-based powder. The mixing of the iron-based powder and the powder molding lubricant or further the alloy powder does not need to be particularly limited,
Generally, any known mixing method can be suitably used. Among them, when the alloy powder is mixed with the iron-based powder, in order to avoid segregation of the contained powder, one part of the powder-forming lubricant is added to the iron-based powder and the alloy powder, and the mixture is primarily mixed. Further, the mixture is stirred while being heated to at least the melting point of at least one of the lubricants for powder molding to melt at least one of the lubricants for powder molding, and the mixture after melting is stirred. Preferably, a cooling method is performed in which the alloying powder is attached by cooling while cooling and fixing the molten lubricant on the surface of the iron-based powder, and then the remaining portion of the powder forming lubricant is added and secondarily mixed.

【0025】本発明における鉄基粉末は、アトマイズ鉄
粉または還元鉄粉などの純鉄粉、または部分拡散合金化
鋼粉、完全合金化鋼粉、またはこれらの混合粉が好まし
い。鉄基粉末混合物に含まれる粉末成形用潤滑剤の含有
量は、鉄基粉末混合物全体に対し0.05〜0.40質量%とす
るのが好ましい。粉末成形用潤滑剤の含有量が0.05質量
%未満では、鉄基混合粉末の流動性が悪く金型表面へ均
一に充填されないため、成形体の密度が低下する。一
方、粉末成形用潤滑剤含有量が0.40質量%を超えると、
焼結後気孔率が高くなり成形体密度が低下する。
The iron-based powder in the present invention is preferably pure iron powder such as atomized iron powder or reduced iron powder, partially diffusion alloyed steel powder, fully alloyed steel powder, or a mixed powder thereof. The content of the powder-forming lubricant contained in the iron-based powder mixture is preferably 0.05 to 0.40% by mass based on the entire iron-based powder mixture. If the content of the lubricant for powder molding is less than 0.05% by mass, the fluidity of the iron-based mixed powder is poor and the powder is not evenly filled on the mold surface, so that the density of the molded body is reduced. On the other hand, when the powder molding lubricant content exceeds 0.40% by mass,
After sintering, the porosity increases and the density of the compact decreases.

【0026】鉄基粉末混合物に含まれる粉末成形用潤滑
剤は、所定の加圧成形の温度以下の低い融点をもつ潤滑
剤と所定の加圧成形の温度より高い融点をもつ潤滑剤と
からなる混合潤滑剤とする。所定の加圧成形の温度以下
の低い融点をもつ潤滑剤の含有量は、含まれる粉末成形
用潤滑剤全量の10〜75質量%とし、残部の25〜90質量%
を所定の加圧成形の温度より高い融点とからなる潤滑剤
とする。所定の加圧成形の温度以下の低い融点をもつ潤
滑剤は、加圧成形時に溶融し、粉末粒子間に毛細管力に
より浸透して、粉末粒子内部に均等に分散し、粒子相互
の接触抵抗を低減し、粒子再配列を促進して成形体の高
密度化を促進する効果を有する。所定の加圧成形の温度
以下の低い融点をもつ潤滑剤の含有量が、10質量%未満
では、粉末粒子内部に潤滑剤が均等に分散せず、成形体
密度が低下する。また、75質量%を超えると、成形体の
密度が増加するにしたがい、溶融した潤滑剤が成形体表
面へ絞り出され、表面に、潤滑剤の逃げ道が形成され、
成形体表面に多数の粗大な空孔が形成されて、焼結部材
の強度低下を招く。
The powder-forming lubricant contained in the iron-based powder mixture is composed of a lubricant having a low melting point below a predetermined pressing temperature and a lubricant having a melting point higher than a predetermined pressing temperature. It is a mixed lubricant. The content of the lubricant having a low melting point not higher than the predetermined pressure molding temperature should be 10 to 75% by mass of the total amount of the powder molding lubricant included, and the remaining 25 to 90% by mass.
Is a lubricant having a melting point higher than a predetermined pressure molding temperature. Lubricant having a low melting point below the temperature of the specified pressure molding melts at the time of pressure molding, penetrates between the powder particles by capillary force, is evenly dispersed inside the powder particles, and reduces the contact resistance between the particles. This has the effect of reducing the particle size and accelerating the rearrangement of particles to promote the densification of the molded article. If the content of the lubricant having a low melting point at or below the predetermined pressure molding temperature is less than 10% by mass, the lubricant is not evenly dispersed inside the powder particles, and the density of the compact decreases. Further, when the content exceeds 75% by mass, as the density of the molded body increases, the molten lubricant is squeezed out to the surface of the molded body, and an escape path for the lubricant is formed on the surface,
A large number of coarse pores are formed on the surface of the molded body, which causes a reduction in the strength of the sintered member.

【0027】鉄基粉末混合物に含まれる、所定の加圧成
形の温度より高い融点をもつ潤滑剤は、成形時、固体と
して存在し、溶融した潤滑剤がはじかれる鉄基粉末粒子
表面の凸部において「ころ」として作用して、粒子の再
配列を促進し、成形体の密度を増加させる効果を有す
る。鉄基粉末混合物に含まれる粉末成形用潤滑剤のう
ち、所定の加圧成形の温度より高い融点をもつ潤滑剤と
しては、金属石鹸、熱可塑性樹脂、熱可塑性エラストマ
ー、層状の結晶構造を有する無機または有機潤滑剤のう
ちから選ばれた1種または2種以上とするのが好まし
い。所定の加圧成形の温度に応じ、下記した潤滑剤から
適宜選択できる。
The lubricant contained in the iron-based powder mixture and having a melting point higher than a predetermined pressure molding temperature exists as a solid at the time of molding, and the protrusions on the surface of the iron-based powder particles from which the molten lubricant is repelled. Has the effect of promoting the rearrangement of the particles and increasing the density of the molded body. Among the powder molding lubricants contained in the iron-based powder mixture, lubricants having a melting point higher than a predetermined pressure molding temperature include metal soaps, thermoplastic resins, thermoplastic elastomers, and inorganic materials having a layered crystal structure. Alternatively, it is preferable to use one or more selected from organic lubricants. The lubricant can be appropriately selected from the following lubricants according to the predetermined pressure molding temperature.

【0028】金属石鹸としては、ステアリン酸リチウ
ム、ヒドロキシステアリン酸リチウム等が好ましい。ま
た、熱可塑性樹脂としては、ポリスチレン、ポリアミ
ド、フッ素樹脂等が好適である。熱可塑性エラストマー
としては、ポリスチレン系エラストマー、ポリアミド系
エラストマー等が好適である。また、層状の結晶構造を
有する無機潤滑剤としては、黒鉛、MoS2、フッ化炭素の
いずれでも良く、粒度は細かいほど、抜き出し力の低減
に有効である。層状の結晶構造を有する有機潤滑剤とし
ては、メラミン−シアヌル酸付加物(MCA )、N-アルキ
ルアスパラギン酸−β- アルキルエステルのいずれも使
用することができる。
As the metal soap, lithium stearate, lithium hydroxystearate and the like are preferable. Further, as the thermoplastic resin, polystyrene, polyamide, fluororesin and the like are preferable. As the thermoplastic elastomer, a polystyrene-based elastomer, a polyamide-based elastomer, and the like are preferable. Further, the inorganic lubricant having a layered crystal structure may be any of graphite, MoS 2 , and fluorocarbon. The finer the particle size, the more effective it is in reducing the extraction force. As the organic lubricant having a layered crystal structure, any of melamine-cyanuric acid adduct (MCA) and N-alkyl aspartic acid-β-alkyl ester can be used.

【0029】鉄基粉末混合物に含まれる粉末成形用潤滑
剤のうち、所定の加圧成形の温度以下の低い融点をもつ
潤滑剤としては、金属石鹸、アミド系ワックス、ポリエ
チレンおよびこれらのうちの少なくとも2種以上の共溶
融物のうちから選ばれた1種または2種以上とするのが
好ましい。所定の加圧成形の温度に応じ、下記した潤滑
剤から適宜選択できる。
Among the powder-forming lubricants contained in the iron-based powder mixture, lubricants having a low melting point not higher than a predetermined pressure molding temperature include metal soap, amide wax, polyethylene and at least one of these. It is preferable to use one or more selected from two or more co-melts. The lubricant can be appropriately selected from the following lubricants according to the predetermined pressure molding temperature.

【0030】金属石鹸としては、ステアリン酸亜鉛、ス
テアリン酸カルシウム等が好ましい。また、アミド系ワ
ックスとしては、エチレンビスステアロアミド、ステア
リン酸モノアミド等が好適である。共溶融物としては、
エチレンビスステアロアミドとポリエチレンの共溶融
物、エチレンビスステアロアミドとステアリン酸亜鉛の
共溶融物、エチレンビスステアロアミドとステアリン酸
カルシウムの共溶融物等が好適である。また、成形温度
によっては、これらの潤滑剤の一部を加圧成形温度より
高い融点をもつ潤滑剤として使用することもできる。
As the metal soap, zinc stearate, calcium stearate and the like are preferable. Further, as the amide wax, ethylene bis stearoamide, stearic acid monoamide, and the like are preferable. As a co-melt,
A co-melt of ethylene bis-stearamide and polyethylene, a co-melt of ethylene bis-stearamide and zinc stearate, a co-melt of ethylene bis-stearamide and calcium stearate, and the like are preferable. Further, depending on the molding temperature, some of these lubricants can be used as a lubricant having a melting point higher than the pressure molding temperature.

【0031】鉄基粉末混合物に合金用粉末として含まれ
る黒鉛は、焼結体を強化する効果を有する。黒鉛の含有
量が少ないと焼結体強化の効果が充分でなく、一方、多
すぎると初析セメンタイトが析出して強度が低下する。
このようなことから、鉄基粉末混合物中に含有される黒
鉛は、鉄基粉末混合物全量に対し、0.5 〜1.2 質量%と
するのが好ましい。
Graphite contained as an alloy powder in the iron-based powder mixture has the effect of strengthening the sintered body. If the graphite content is small, the effect of strengthening the sintered body is not sufficient, while if it is too large, pro-eutectoid cementite precipitates and the strength is reduced.
For this reason, the amount of graphite contained in the iron-based powder mixture is preferably 0.5 to 1.2% by mass based on the total amount of the iron-based powder mixture.

【0032】本発明では、上記した製造方法で得られた
高密度鉄基粉末成形体に焼結処理を施し、高密度の鉄基
焼結体を得る。本発明における焼結処理は、とくに限定
する必要はなく、通常公知の焼結処理方法がいずれも好
適に使用できる。また、焼結後急冷して強度を高める方
法(シンターハードニング)も使用できる。
In the present invention, the high-density iron-based powder compact obtained by the above-described production method is subjected to a sintering treatment to obtain a high-density iron-based sintered body. The sintering treatment in the present invention does not need to be particularly limited, and any generally known sintering treatment method can be suitably used. Further, a method of increasing the strength by quenching after sintering (sinter hardening) can also be used.

【0033】[0033]

【実施例】(実施例1)鉄基粉末として、アトマイズ純
鉄粉にNi、Mo、Cuが拡散付着した、Fe-4Ni-0.5Mo-1.5Cu
組成の部分合金化鋼粉を用いた。この部分合金化鋼粉
に、0.5 質量%の黒鉛粉と、表1に示す各種潤滑剤を高
速ミキサーによる加熱混合法で混合し、鉄基粉末混合物
とした。
[Example] (Example 1) Fe-4Ni-0.5Mo-1.5Cu in which Ni, Mo, and Cu are diffused and attached to atomized pure iron powder as an iron-based powder.
A partially alloyed steel powder of the composition was used. This partially alloyed steel powder was mixed with 0.5% by mass of graphite powder and various lubricants shown in Table 1 by a heating and mixing method using a high-speed mixer to obtain an iron-based powder mixture.

【0034】まず、加圧成形用の金型を表1に示す温度
に予熱し、金型潤滑装置:Gasbarre 社製)を用いて帯
電させた温間金型潤滑用潤滑剤を金型内に噴霧導入し、
金型表面に帯電付着させた。なお、温間金型潤滑用潤滑
剤は、表2に示す各種潤滑剤から選択し、加圧成形温度
以下の低い融点をもつ潤滑剤と、加圧成形温度より高い
融点をもつ潤滑剤とを表1に示すように混合したものを
使用した。なお、金型表面の温度を測定し、加圧成形の
温度とした。
First, a mold for pressure molding is preheated to the temperature shown in Table 1, and a lubricant for warm mold lubrication charged using a mold lubrication device (manufactured by Gasbarre) is placed in the mold. Spray introduction,
It was charged and adhered to the mold surface. The lubricant for warm mold lubrication is selected from various lubricants shown in Table 2, and a lubricant having a melting point lower than the pressing temperature and a lubricant having a melting point higher than the pressing temperature. A mixture as shown in Table 1 was used. In addition, the temperature of the mold surface was measured and set as the temperature for pressure molding.

【0035】ついで、このように処理された金型に、加
熱した鉄基粉末混合物を充填したのち、加圧成形し、10
×10×55mmの直方体の成形体とした。なお、加圧力は、
7t/cm2(686 MPa )とした。また、加圧成形条件を表1
に示す。また、鉄基粉末混合物に含まれる粉末成形用潤
滑剤は、表2に示す各種潤滑剤から選択し、加圧成形温
度以下の低い融点をもつ潤滑剤と、加圧成形温度より高
い融点をもつ潤滑剤とを表1に示すように混合したもの
である。
Next, the mold thus treated is filled with the heated iron-based powder mixture, and then molded under pressure.
A rectangular parallelepiped molded product of × 10 × 55 mm was obtained. The pressing force is
It was set to 7 t / cm 2 (686 MPa). Table 1 shows the pressure molding conditions.
Shown in The powder molding lubricant contained in the iron-based powder mixture is selected from various lubricants shown in Table 2, and has a lower melting point than the pressing temperature and a higher melting point than the pressing temperature. A lubricant was mixed as shown in Table 1.

【0036】なお、従来例として、金型潤滑用潤滑剤を
塗布しない金型に、加熱した鉄基粉末混合物を充填し、
加圧成形し、同様の直方体の成形体とした例を従来例と
した(成形体No.38 )。成形後、成形体を抜き出す時の
抜き出し力を測定した。また、これら成形体について、
アルキメデス法で密度を測定した。なお、アルキメデス
法とは、被測定物である成形体をエタノール中に浸漬し
て体積を測定することにより密度を測定する方法であ
る。さらに、これら成形体の外観を目視で観察し、疵、
割れ等の欠陥の有無を調査した。また、これら成形体を
中央部で切断し、樹脂に埋め込んで研磨し、断面におけ
る空孔の有無を光学顕微鏡で観察した。
As a conventional example, a heated die-based powder mixture is filled into a mold to which no lubricant for mold lubrication is applied.
An example in which pressure molding was performed to obtain a similar rectangular parallelepiped molded body was taken as a conventional example (molded body No. 38). After the molding, the extraction force at the time of extracting the molded body was measured. In addition, about these molded objects,
The density was measured by the Archimedes method. The Archimedes method is a method of measuring the density by immersing a molded object to be measured in ethanol and measuring the volume. Furthermore, the appearance of these molded articles was visually observed,
The existence of defects such as cracks was investigated. These molded products were cut at the center, embedded in a resin and polished, and the presence or absence of voids in the cross section was observed with an optical microscope.

【0037】抜き出し力、成形体密度、成形体の外観お
よび成形体断面の性状についての結果を表1に示す。
Table 1 shows the results of the extraction force, the density of the compact, the appearance of the compact, and the properties of the cross section of the compact.

【0038】[0038]

【表1】 [Table 1]

【0039】[0039]

【表2】 [Table 2]

【0040】[0040]

【表3】 [Table 3]

【0041】[0041]

【表4】 [Table 4]

【0042】[0042]

【表5】 [Table 5]

【0043】本発明例は、いずれも成形後の抜き出し力
が20MPa 以下と低く、さらに7.4 Mg/m3 以上の高密度を
有する成形体となっている。さらに、成形体には加熱に
よる表面酸化はもとより、疵、割れ等の欠陥は認められ
なかった。また、成形体の断面性状は、正常で、粗大な
空孔は認められなかった。本発明の範囲を外れる比較
例、従来例は、抜き出し力が20MPa を超えて高いか、密
度が7.35Mg/m3 未満と低いか、あるいは成形体断面の表
面付近に粗大な空孔が観察された。
Each of the examples of the present invention is a compact having a low withdrawal force after molding of 20 MPa or less and a high density of 7.4 Mg / m 3 or more. Further, defects such as flaws, cracks, etc. were not observed on the molded body, in addition to surface oxidation by heating. Also, the cross-sectional properties of the molded product were normal, and no coarse pores were recognized. Comparative Example, the conventional example outside the scope of the present invention, extraction force is higher or exceed 20 MPa, density 7.35 mg / m 3 and less than or less, or coarse voids are observed in the vicinity of the surface of the molded body section Was.

【0044】本発明によれば、外観性状、断面性状いず
れも良好である、高密度の成形体を抜き出し力が低く成
形できるという効果がある。 (実施例2)鉄基粉末として、アトマイズ純鉄粉に、
Ni、Mo、Cuが拡散付着した、Fe-4Ni-0.5Mo-1.5Cu組成の
部分合金化鋼粉a、アトマイズ純鉄粉に、Ni、Moが拡
散付着した、Fe-2Ni-1Mo組成の部分合金化鋼粉b、C
r、Mo、Vを予合金した、Fe-3Cr-0.3Mo-0.3V組成のプ
レアロイ鋼粉c、Cr、Mo、Vを予合金した、Fe-1Cr-
0.3Mo-0.3V組成のプレアロイ鋼粉d、アトマイズ鉄
粉e、還元鉄粉fを用いた。なお、アトマイズ鉄粉と
は、溶鋼を高圧水で噴霧して得られた鉄基粉末であり、
還元鉄粉とは、酸化鉄を還元して得られた鉄基粉末であ
る。
According to the present invention, there is an effect that a high-density molded body having good appearance properties and cross-sectional properties can be formed with low extraction force. (Example 2) As an iron-based powder, atomized pure iron powder was used.
Part of Fe-2Ni-1Mo composition where Ni, Mo and Cu are diffused and adhered, and Ni and Mo are diffused and adhered to Fe-4Ni-0.5Mo-1.5Cu composition alloyed steel powder a and atomized pure iron powder. Alloyed steel powder b, C
Prealloyed Fe-3Cr-0.3Mo-0.3V pre-alloyed steel powder c, Cr, Mo, V pre-alloyed with r, Mo, V, Fe-1Cr-
Prealloyed steel powder d, atomized iron powder e, and reduced iron powder f having a composition of 0.3Mo-0.3V were used. In addition, atomized iron powder is an iron-based powder obtained by spraying molten steel with high-pressure water,
The reduced iron powder is an iron-based powder obtained by reducing iron oxide.

【0045】これら部分合金化鋼粉a、部分合金化鋼粉
b、プレアロイ鋼粉c、プレアロイ鋼粉d、アトマイズ
鉄粉e、還元鉄粉fそれぞれに、表3に示す含有量の黒
鉛と、表3に示す各種潤滑剤とを高速ミキサーによる加
熱混合法で混合し、鉄基粉末混合物とした。なおアトマ
イズ鉄粉eおよび還元鉄粉fの場合には0.8 質量%の黒
鉛に加えて、2.0 質量%のCu粉を混合した。黒鉛の含有
量は、鉄基粉末と黒鉛あるいはさらに合金粉末との合計
量に対する質量比である。
Each of the partially alloyed steel powder a, the partially alloyed steel powder b, the prealloyed steel powder c, the prealloyed steel powder d, the atomized iron powder e, and the reduced iron powder f, Various lubricants shown in Table 3 were mixed by a heating and mixing method using a high-speed mixer to obtain an iron-based powder mixture. In the case of atomized iron powder e and reduced iron powder f, 2.0% by mass of Cu powder was mixed in addition to 0.8% by mass of graphite. The graphite content is a mass ratio to the total amount of the iron-based powder and the graphite or further the alloy powder.

【0046】まず、加圧成形用の金型を表3に示す温度
に予熱し、金型潤滑装置:Gasbarre 社製)を用いて帯
電させた温間金型潤滑用潤滑剤を金型内に噴霧導入し、
金型表面に帯電付着させた。なお、温間金型潤滑用潤滑
剤は、表2に示す各種潤滑剤から選択し、加圧成形温度
以下の低い融点をもつ潤滑剤と、加圧成形温度より高い
融点をもつ潤滑剤とを表3に示すように混合したものを
使用した。なお、金型表面の温度を測定し、加圧成形の
温度とした。
First, a mold for pressure molding was preheated to the temperature shown in Table 3, and a lubricant for warm mold lubrication charged using a mold lubrication device (manufactured by Gasbarre) was placed in the mold. Spray introduction,
It was charged and adhered to the mold surface. The lubricant for warm mold lubrication is selected from various lubricants shown in Table 2, and a lubricant having a melting point lower than the pressing temperature and a lubricant having a melting point higher than the pressing temperature. A mixture as shown in Table 3 was used. In addition, the temperature of the mold surface was measured and set as the temperature for pressure molding.

【0047】ついで、このように処理された金型に、加
熱した鉄基粉末混合物を充填したのち、加圧成形し、10
×10×55mmの直方体の成形体とした。なお、加圧力は、
7t/cm2(686 MPa )とした。加圧成形条件を表3に示
す。また、鉄基粉末混合物に含まれる粉末成形用潤滑剤
は、表2に示す各種潤滑剤から選択し、加圧成形温度以
下の低い融点をもつ潤滑剤と、加圧成形温度より高い融
点をもつ潤滑剤とを表3に示すように混合したものであ
る。
Next, after filling the heated iron-based powder mixture into the mold thus treated, the mixture was pressed and molded.
A rectangular parallelepiped molded product of × 10 × 55 mm was obtained. The pressing force is
It was set to 7 t / cm 2 (686 MPa). Table 3 shows the pressure molding conditions. The powder molding lubricant contained in the iron-based powder mixture is selected from various lubricants shown in Table 2, and has a lower melting point than the pressing temperature and a higher melting point than the pressing temperature. The lubricant was mixed with the lubricant as shown in Table 3.

【0048】これら鉄基粉末成形体について、実施例1
と同様にアルキメデス法で密度を測定した。ついで、こ
れら鉄基粉末成形体に、N2 −10%H2 雰囲気中で、11
30℃×20min の焼結処理を施し、鉄基焼結体とした。得
られた鉄基焼結体について、まず、アルキメデス法で密
度を測定した。また、これらの鉄基焼結体から、機械加
工により平行部径5mm×長さ15mmの小型丸棒試験片を採
取し、引張試験を実施し、引張強さを測定した。
Example 1 of these iron-based powder compacts
The density was measured by the Archimedes method in the same manner as described above. Then, these iron-based powder compacts were added to an N 2 -10% H 2 atmosphere in an atmosphere of 11%.
A sintering process was performed at 30 ° C. for 20 minutes to obtain an iron-based sintered body. First, the density of the obtained iron-based sintered body was measured by the Archimedes method. Further, from these iron-based sintered bodies, small round bar test pieces having a parallel part diameter of 5 mm and a length of 15 mm were sampled by machining, and a tensile test was performed to measure the tensile strength.

【0049】なお、金型潤滑用潤滑剤を塗布しない金型
に、加熱した鉄基粉末混合物を充填し、加圧成形し、同
様の直方体の成形体とし、さらに焼結処理を施し鉄基焼
結体とした例を従来例とした。それらの結果を表3に示
す。
The heated iron-based powder mixture was filled in a mold to which no lubricant for mold lubrication was applied, and was pressed and molded to obtain a similar rectangular parallelepiped compact. The example of the union was taken as a conventional example. Table 3 shows the results.

【0050】[0050]

【表6】 [Table 6]

【0051】本発明例は、金型潤滑を行わない従来例
(焼結体No. 2-12)と比べ、高い密度が得られ、しかも
高引張強さを有している。
The example of the present invention has higher density and higher tensile strength than the conventional example (sintered body No. 2-12) in which mold lubrication is not performed.

【0052】[0052]

【発明の効果】本発明によれば、外観性状、断面性状い
ずれも良好である、高密度の成形体を1回の成形で容易
に製造でき、しかも成形後の抜き出し力が低く、金型を
長寿命化することができ、さらに高密度の焼結体が容易
に得られるという産業上格段の効果を奏する。
According to the present invention, it is possible to easily produce a high-density molded article having good appearance and cross-sectional properties in a single molding operation, and furthermore, it has a low withdrawal force after molding, so that a mold can be manufactured. This has an industrially remarkable effect that the life can be prolonged and a high-density sintered body can be easily obtained.

フロントページの続き (72)発明者 上ノ薗 聡 千葉県千葉市中央区川崎町1番地 川崎製 鉄株式会社技術研究所内 Fターム(参考) 4K018 CA07 CA09 Continuation of the front page (72) Inventor Satoshi Uenozono 1 Kawasaki-cho, Chuo-ku, Chiba-shi, Chiba F-term in Kawasaki Steel Engineering Co., Ltd. F-term (reference) 4K018 CA07 CA09

Claims (11)

【特許請求の範囲】[Claims] 【請求項1】 粉末を金型で加圧成形する際に予熱され
た金型表面に帯電付着させて使用する温間金型潤滑用潤
滑剤であって、所定の加圧成形の温度より高い融点を有
する潤滑剤と、前記所定の加圧成形の温度以下の低い融
点を有する潤滑剤との混合物であることを特徴とする温
間金型潤滑用潤滑剤。
Claims 1. A lubricant for warm mold lubrication, which is used by charging and adhering a powder to the surface of a preheated mold when the powder is compacted by a mold, wherein the lubricant is higher than a predetermined pressure molding temperature. A lubricant for a warm mold lubrication, which is a mixture of a lubricant having a melting point and a lubricant having a low melting point not higher than the predetermined pressure forming temperature.
【請求項2】 粉末を金型で加圧成形する際に予熱され
た金型表面に帯電付着させて使用する温間金型潤滑用潤
滑剤であって、所定の加圧成形の温度より高い融点を有
する潤滑剤を 0.5〜80質量%含有し、残部が前記所定の
加圧成形の温度以下の低い融点を有する潤滑剤であるこ
とを特徴とする温間金型潤滑用潤滑剤。
2. A lubricant for warm mold lubrication, which is used by charging and adhering a powder to the surface of a preheated mold when the powder is compacted by a mold, wherein the lubricant is higher than a predetermined pressure molding temperature. A lubricant for warm mold lubrication, comprising a lubricant having a melting point of 0.5 to 80% by mass, and a balance having a low melting point not higher than the predetermined pressure forming temperature.
【請求項3】 前記所定の加圧成形の温度より高い融点
を有する潤滑剤が、金属石鹸、熱可塑性樹脂、熱可塑性
エラストマー、層状の結晶構造を有する無機または有機
潤滑剤のうちから選ばれた1種または2種以上であるこ
とを特徴とする請求項1または2に記載の温間金型潤滑
用潤滑剤。
3. The lubricant having a melting point higher than the predetermined pressure molding temperature is selected from metal soap, thermoplastic resin, thermoplastic elastomer, and inorganic or organic lubricant having a layered crystal structure. The lubricant for warm mold lubrication according to claim 1, wherein the lubricant is at least one kind.
【請求項4】 前記所定の加圧成形の温度以下の低い融
点を有する潤滑剤が、金属石鹸、アミド系ワックス、ポ
リエチレンおよびこれらのうちの2種以上の共溶融物の
うちから選ばれた1種または2種以上であることを特徴
とする請求項1ないし3のいずれかに記載の温間金型潤
滑用潤滑剤。
4. The lubricant having a low melting point not higher than the predetermined pressure forming temperature is selected from metal soap, amide wax, polyethylene and a co-melt of two or more of these. 4. The lubricant for warm mold lubrication according to claim 1, wherein the lubricant is a kind or two or more kinds.
【請求項5】 鉄基粉末と、粉末成形用潤滑剤とを含む
鉄基粉末混合物であって、前記粉末成形用潤滑剤が、粉
末成形用潤滑剤全量に対して10〜75質量%の、加圧成形
の温度以下の低い融点を有する潤滑剤を含み、残部が、
加圧成形の温度より高い融点を有する潤滑剤であること
を特徴とする温間金型潤滑成形用鉄基粉末混合物。
5. An iron-based powder mixture comprising an iron-based powder and a powder-forming lubricant, wherein the powder-forming lubricant contains 10 to 75% by mass of the total amount of the powder-forming lubricant. Including a lubricant having a low melting point below the temperature of pressure molding, the remainder is
An iron-based powder mixture for warm mold lubrication molding, which is a lubricant having a melting point higher than the temperature of pressure molding.
【請求項6】 前記粉末成形用潤滑剤の含有量が、0.05
〜0.40質量%であることを特徴とする請求項5に記載の
温間金型潤滑成形用鉄基粉末混合物。
6. The content of the powder molding lubricant is 0.05%.
The iron-based powder mixture for warm mold lubrication molding according to claim 5, characterized in that the content of the iron-based powder is -0.40% by mass.
【請求項7】 金型に、加熱した鉄基粉末混合物を充填
したのち、所定の温度で加圧成形する鉄基粉末成形体の
製造方法において、前記金型を、予熱され、表面に、温
間金型潤滑用潤滑剤を帯電付着させた金型とし、前記温
間金型潤滑用潤滑剤を、 0.5〜80質量%の、所定の加圧
成形の温度より高い融点をもつ潤滑剤を含み、残部が所
定の加圧成形の温度以下の低い融点をもつ潤滑剤である
潤滑剤とし、さらに前記鉄基粉末混合物が鉄基粉末と粉
末成形用潤滑剤とを含み、前記粉末成形用潤滑剤が粉末
成形用潤滑剤全量に対し10〜75質量%の、所定の加圧成
形の温度以下の低い融点をもつ潤滑剤を含み、残部が所
定の加圧成形の温度より高い融点をもつ潤滑剤である潤
滑剤とすることを特徴とする高密度鉄基粉末成形体の製
造方法。
7. A method of manufacturing an iron-based powder compact in which a mold is filled with a heated iron-based powder mixture and then press-molded at a predetermined temperature, the mold is preheated, and a surface is heated. A mold having lubricating lubricant between the molds charged thereon, wherein the lubricant for warm mold lubrication contains 0.5 to 80% by mass of a lubricant having a melting point higher than a predetermined pressing temperature. The remainder being a lubricant having a low melting point not higher than a predetermined pressure molding temperature, wherein the iron-based powder mixture further contains an iron-based powder and a powder-forming lubricant, and the powder-forming lubricant Contains 10 to 75% by mass of the total amount of the lubricant for powder molding and has a melting point lower than the predetermined pressing temperature, and the remainder has a melting point higher than the predetermined pressing temperature. A method for producing a high-density iron-based powder compact, characterized by using a lubricant as described above.
【請求項8】 前記温間金型潤滑用潤滑剤における前記
所定の加圧成形の温度より高い融点を有する潤滑剤が、
金属石鹸、熱可塑性樹脂、熱可塑性エラストマー、層状
の結晶構造を有する無機または有機潤滑剤のうちから選
ばれた1種または2種以上であることを特徴とする請求
項7に記載の高密度鉄基粉末成形体の製造方法。
8. A lubricant having a melting point higher than the predetermined pressure forming temperature in the warm mold lubrication lubricant,
The high-density iron according to claim 7, wherein the iron is one or more selected from a metal soap, a thermoplastic resin, a thermoplastic elastomer, and an inorganic or organic lubricant having a layered crystal structure. A method for producing a base powder compact.
【請求項9】 前記温間金型潤滑用潤滑剤における前記
所定の加圧成形の温度以下の低い融点を有する潤滑剤
が、金属石鹸、アミド系ワックス、ポリエチレンおよび
これらのうちの2種以上の共溶融物のうちから選ばれた
1種または2種以上であることを特徴とする請求項7ま
たは8に記載の高密度鉄基粉末成形体の製造方法。
9. A lubricant having a low melting point not higher than the predetermined pressure molding temperature in the warm mold lubricating lubricant is metal soap, amide wax, polyethylene, and two or more of these. The method for producing a high-density iron-based powder molded body according to claim 7 or 8, wherein at least one kind is selected from co-melts.
【請求項10】 前記温間成形用潤滑剤の含有量が、0.
05〜0.40質量%であことを特徴とする請求項7ないし9
のいずれかに記載の高密度鉄基粉末成形体の製造方法。
10. The content of the warm forming lubricant is 0.
10. The composition according to claim 7, wherein the content is from 0.05 to 0.40% by mass.
The method for producing a high-density iron-based powder compact according to any one of the above.
【請求項11】 請求項7ないし10のいずれかに記載の
高密度鉄基粉末成形体の製造方法により製造された鉄基
粉末成形体に、さらに焼結処理を施し鉄基焼結体とする
ことを特徴とする高密度鉄基焼結体の製造方法。
11. The iron-based powder compact produced by the method for producing a high-density iron-based powder compact according to claim 7 is further subjected to a sintering process to obtain an iron-based sintered compact. A method for producing a high-density iron-based sintered body, characterized in that:
JP30859099A 1999-02-05 1999-10-29 Lubricant for warm mold lubrication, high-density iron-based powder molded body, and method for producing high-density iron-based sintered body Expired - Fee Related JP3931503B2 (en)

Priority Applications (6)

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JP30859099A JP3931503B2 (en) 1999-02-05 1999-10-29 Lubricant for warm mold lubrication, high-density iron-based powder molded body, and method for producing high-density iron-based sintered body
CA2356253A CA2356253C (en) 1999-10-29 2000-08-01 A die lubricant comprising a higher-melting and a lower-melting lubricants
EP00948302A EP1145788B1 (en) 1999-10-29 2000-08-01 Lubricating agent for mold at elevated temperature and method for producing high density iron-based sintered compact
PCT/JP2000/005089 WO2001032337A1 (en) 1999-10-29 2000-08-01 Lubricating agent for mold at elevated temperature, iron-based powder composition for elevated temperature compaction with lubricated mold and high density formed product from iron-based powder composition, and method for producing high density iron-based sintered compact
US09/631,033 US6355208B1 (en) 1999-10-29 2000-08-02 Die lubricant and iron-based powder mixture for warm compaction with die lubrication, and processes for producing high-density iron-based green and sintered compacts
TW089115743A TW486396B (en) 1999-10-29 2000-08-04 Manufacture of lubricant for warm die lubrication, iron- base powder mixture for warm die lubricating compaction, high density green compact of iron-base powder, and high density iron-base sintered compact

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JP2940599 1999-02-05
JP11-29405 1999-02-05
JP30859099A JP3931503B2 (en) 1999-02-05 1999-10-29 Lubricant for warm mold lubrication, high-density iron-based powder molded body, and method for producing high-density iron-based sintered body

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1199124A1 (en) * 2000-03-28 2002-04-24 Kawasaki Steel Corporation Lubricant for die lubrication and method for producing high density product of forming of iron base powder
WO2005051577A1 (en) * 2003-11-25 2005-06-09 Mitsubishi Materials Pmg Corporation Raw material powder for warm compaction and method of warm compaction
US7459032B2 (en) 2001-06-13 2008-12-02 Kabushiki Kaisha Toyota Chuo Kenkyusho Pressurizing forming process and pressurized-and-formed member

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1199124A1 (en) * 2000-03-28 2002-04-24 Kawasaki Steel Corporation Lubricant for die lubrication and method for producing high density product of forming of iron base powder
EP1199124A4 (en) * 2000-03-28 2003-05-14 Kawasaki Steel Co Lubricant for die lubrication and method for producing high density product of forming of iron base powder
US6861028B2 (en) 2000-03-28 2005-03-01 Kawasaki Steel Corporation Lubricants for die lubrication and manufacturing method for high density iron-based powder compacts
US7459032B2 (en) 2001-06-13 2008-12-02 Kabushiki Kaisha Toyota Chuo Kenkyusho Pressurizing forming process and pressurized-and-formed member
WO2005051577A1 (en) * 2003-11-25 2005-06-09 Mitsubishi Materials Pmg Corporation Raw material powder for warm compaction and method of warm compaction
US7582255B2 (en) 2003-11-25 2009-09-01 Mitsubishi Materials Pmg Corporation Warm molding raw material powder and warm molding method
KR101162129B1 (en) 2003-11-25 2012-07-03 가부시키가이샤 다이야멧트 Raw material powder for warm compaction and method of warm compaction

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