JPH06346106A - Production of sintered member - Google Patents

Production of sintered member

Info

Publication number
JPH06346106A
JPH06346106A JP14090993A JP14090993A JPH06346106A JP H06346106 A JPH06346106 A JP H06346106A JP 14090993 A JP14090993 A JP 14090993A JP 14090993 A JP14090993 A JP 14090993A JP H06346106 A JPH06346106 A JP H06346106A
Authority
JP
Japan
Prior art keywords
heat treatment
heat
metal
treated
support member
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
JP14090993A
Other languages
Japanese (ja)
Other versions
JP3442427B2 (en
Inventor
Tatsuhiko Fujinuma
龍彦 藤沼
Manabu Takahashi
学 高橋
Isao Okutomi
功 奥冨
Shigeaki Sekiguchi
薫旦 関口
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.)
Toshiba Corp
Japan Metals and Chemical Co Ltd
Original Assignee
Toshiba Corp
Japan Metals and Chemical Co Ltd
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 Toshiba Corp, Japan Metals and Chemical Co Ltd filed Critical Toshiba Corp
Priority to JP14090993A priority Critical patent/JP3442427B2/en
Publication of JPH06346106A publication Critical patent/JPH06346106A/en
Application granted granted Critical
Publication of JP3442427B2 publication Critical patent/JP3442427B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Abstract

PURPOSE:To produce a sintered member free from structural segregation, surface flaws, contamination or the like by forming the surface of a supporting member of the carbide or oxide of the metal to be heat-treated, thereafter placing the metal to be heat-treated thereon under no pressure and executing heating treatment. CONSTITUTION:At least a part of the surface of a supporting member having a prescribed shape is coated with the metal to be heat-treated, and after that, coating metal is formed of carbide or/and oxide. On the obtd. supporting member for heat treatment, the metal to be heat-treated of a powder formed body or the like is placed and introduced without pressurizing, and heating treatment is executed. In this way, the sinterted member small in the intrusion of gas and impurities and furthermore small in surface flaws can be obtd.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】この発明は、ガス及び不純物の混
入が少なく、かつ表面損傷の少ない焼結部材の製造方法
に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a sintered member in which gas and impurities are less mixed and surface damage is small.

【0002】[0002]

【従来の技術】近年、プラントの大型化、半導体部品を
中心とした電子機器の高集積化やシステムの高機能化が
進行し、材料・部品への要求が過酷化、高度化してきて
いる。この要求に対応すべく素材あるいは部品は、工業
的レベルでの価格を維持した上での高純度化が必須とさ
れている。一般に、これらの素材あるいは部品は、充分
吟味した原材料を用いて、加圧・成型加工の後、所定の
雰囲気レベルの中での溶解法、焼結法、焼結・溶浸法で
得た素材を、加熱処理や、仕上げ加工などの各工程を経
て、目的の製品や半製品としている。ここで、充分吟味
した原材料は、最近の精練技術や粉砕化技術の進展によ
って、目標性能を持つ原材料や粉体を、工業的に容易に
準備することが出来る。例えば、各工程での雰囲気は、
真空、窒素、アルゴン、水素など不活性あるいは、還元
性雰囲気中で作業を行うことのできる高性能設備を経済
的に容易に準備することも出来る。しかし、加熱処理工
程では、処理が行われている瞬間瞬間の諸条件を正確に
定量化し制御することは、工業的レベルでは、容易に準
備することが出来ていない。従って、前記原材料技術が
特に重要となってくる。
2. Description of the Related Art In recent years, as plants have grown in size, electronic devices centering on semiconductor parts have become highly integrated, and systems have become highly functional, demands for materials and parts have become severe and sophisticated. In order to meet this demand, materials or parts are required to be highly purified while maintaining the price at an industrial level. In general, these materials or parts are materials obtained by melting, sintering, sintering / infiltration in a predetermined atmosphere level after pressurizing / molding, using raw materials that have been thoroughly examined. Is subjected to various steps such as heat treatment and finishing to obtain the desired product or semi-finished product. Here, for the raw materials that have been thoroughly examined, it is possible to industrially easily prepare raw materials and powders having the target performance due to the recent progress of refining technology and pulverization technology. For example, the atmosphere in each process is
It is also possible to economically and easily prepare high-performance equipment capable of performing work in an inert or reducing atmosphere such as vacuum, nitrogen, argon, or hydrogen. However, in the heat treatment step, it is not possible to easily prepare, on an industrial level, to accurately quantify and control various conditions at the moment when the treatment is performed. Therefore, the raw material technology becomes particularly important.

【0003】即ち、本発明者が、目標性能を持つ健全な
素材あるいは部品を得ることを目的に、前記の各工程を
検討したところ、(イ)前記原材料技術のうちで、特に
加圧・成型加工技術に起因すると考えられる被成型体の
特性ばらつきや、(ロ)溶解、焼結など加熱処理中に素
材あるいは部品と共に加熱して用いる溶解用るつぼ、焼
結用ボートの物理的、化学的状態などの影響によって、
得られる素材あるいは部品(製品)の品質(例えば表面
状態の健全性)が、影響を受けていることが判った。
That is, the present inventor examined each of the above steps for the purpose of obtaining a sound material or part having a target performance. Variations in the characteristics of the molded product that are thought to be due to processing technology, and (b) the physical and chemical states of the melting crucible and sintering boat that are used by heating together with the material or parts during heat treatment such as melting and sintering. By the influence of
It has been found that the quality of the obtained material or part (product) (for example, the soundness of the surface condition) is affected.

【0004】粉末冶金用原料粉には、銅、鉄、ニッケ
ル、クロム、チタン、タングステン、タンタルなどの金
属粉、ステンレスなどの合金粉が一般的に用いられてい
る。これらの粉末冶金用原料粉を用いて、素材あるいは
部品を製造する時に行われる加熱処理には、一般に該素
材あるいは部品を加熱処理中に支えておくために、熱処
理用支持部材(容器、るつぼ、ボートなど)が不可欠で
ある。このように、該素材あるいは部品は、熱処理用支
持部材(以下、熱処理用容器とも云う)に挿入するか載
置して加熱処理を行い製品あるいは半製品とするため、
前記該素材あるいは部品は、熱処理用容器材質である黒
鉛と、加熱処理中直接的に接触することになり、該素材
あるいは部品と炭素とが、冶金的反応を呈する場合が見
られる。その結果、該素材あるいは部品が熱処理用容器
から、健全な形態で取り出せず損傷を受けるのみならず
熱処理用容器を破壊する等、表面形状的な不都合さがみ
られる場合がある。これらは製品として致命的損害とな
るばかりか、経済的損失も重大な問題となる。
As the raw material powder for powder metallurgy, metal powders such as copper, iron, nickel, chromium, titanium, tungsten and tantalum, and alloy powders such as stainless steel are generally used. Using these powder metallurgy raw material powders, in the heat treatment performed when manufacturing the material or component, in order to generally support the material or component during the heat treatment, a heat treatment support member (container, crucible, Boats) are essential. In this way, the material or component is inserted into or placed on a heat treatment support member (hereinafter, also referred to as a heat treatment container) and heat-treated to obtain a product or a semi-finished product.
The material or part comes into direct contact with graphite, which is the material for the heat treatment container, during the heat treatment, and there are cases in which the material or part and metal exhibit a metallurgical reaction. As a result, the material or part may not be taken out of the heat treatment container in a sound form and may be damaged, or the heat treatment container may be destroyed, resulting in surface shape inconvenience. These are not only fatal damages as products, but also economic loss is a serious problem.

【0005】一方、熱処理用容器材質として、酸化カル
シウム(カルシア)又は酸化イットリウム(イットリ
ア)製熱処理用容器を選択したときには、上記炭素の場
合のような著しい冶金的反応は見られず、表面形状的に
は損傷がない焼結部材が得られる。しかし、通常の黒鉛
又は酸化カルシウム(カルシア)又は酸化イットリウム
(イットリア)製熱処理用容器は、多孔性でありその表
面および内部には多量の水分、ガスが存在しているた
め、この水分、ガスが加熱処理中直接的に該素材あるい
は部品表面を汚染する不都合さがみられる場合がある。
特にこれらの表面は、吸着物が十分少なくなるほど平滑
に仕上げることが出来ず、表面に水分、ガス、その他表
面付着物が存在しやすい。また、表面形状的な不都合さ
がなくても、成型技術に起因する被成型体内部でのガス
の巻き込みや、成型圧力分布の不均一性のための焼結の
不均一化による組織上の偏析など、内面的な不都合さが
残る。さらに、冶金的反応に伴って熱処理用容器中の不
純物が該素材あるいは部品中に拡散、侵入し、加熱処理
後の該素材あるいは部品の純度を低下させる不都合さが
みられる場合がある。このような不都合さは、健全な素
材あるいは部品の製造に対して障害となり、問題となっ
ている。
On the other hand, when a heat treatment container made of calcium oxide (calcia) or yttrium oxide (yttria) is selected as the material for the heat treatment container, no remarkable metallurgical reaction as in the case of the above carbon is observed, and the surface shape A sintered member having no damage can be obtained. However, a normal graphite or calcium oxide (calcia) or yttrium oxide (yttria) container for heat treatment is porous, and a large amount of water and gas are present on the surface and inside thereof. There may be some inconvenience of directly contaminating the material or component surface during the heat treatment.
In particular, these surfaces cannot be finished so smooth that adsorbates are sufficiently reduced, and water, gas, and other surface deposits tend to be present on the surfaces. In addition, even if there is no inconvenience in terms of surface shape, gas entrapment inside the molded body due to molding technology and segregation on the structure due to uneven sintering due to uneven molding pressure distribution Such internal disadvantages remain. Further, there is a case in which impurities in the heat treatment container diffuse and invade into the material or the component due to the metallurgical reaction, and the purity of the material or the component after the heat treatment may be lowered. Such inconvenience hinders the production of sound materials or parts and poses a problem.

【0006】[0006]

【発明が解決しようとする課題】上述した従来技術の問
題点を整理して述べる。問題点1;焼結部材の製造にお
いて、熱処理に先立ち、原料粉体を混合した後、成型プ
レス機械によって、所定形状に圧粉成型したものを、焼
結、熱処理に供することが行われている。該原料粉体を
圧粉成型することによって、熱処理時(焼結時)の取り
扱い作業性の向上、該原料粉体容積の縮小化、焼結性の
向上、焼結後の部材の高密度化など多くの利益を得てい
る。
The problems of the above-mentioned prior art will be summarized and described. Problem 1; In the production of a sintered member, prior to heat treatment, raw material powders are mixed, and then a powder compacted into a predetermined shape by a molding press machine is subjected to sintering and heat treatment. . By compacting the raw material powder, the workability during heat treatment (sintering) is improved, the volume of the raw material powder is reduced, the sinterability is improved, and the density of the member after sintering is increased. And many other benefits.

【0007】しかし、成型プレス機械によって粉体を圧
縮するため、内部にガスの残存が避けられず熱処理時
(焼結時)に、焼結体を変色、酸化させたり、このガス
の体積膨張による焼結体の膨れ、変形現象を呈する等の
不具合が見られる場合がある。これらはいずれも成型時
のガスの閉じ込めに原因し、焼結時にガスが十分外部に
出される前に、焼結の進行によって出口が閉じられるた
めと考えられる。また、金型への装填時の該原料粉体の
流動性の差異や、成型時の成型技術に係わる成型圧力の
該原料粉体への圧力伝達の差異等で、密度等のばらつき
の少ない均一な成型体または/および焼結体の製作は、
困難となっている。これは、個々の成型体の成型作業時
に、各成型体に与えられる加圧力に、ばらつきが存在し
ているのみでなく、前述した流動性の相違による加圧後
の成型体内部の場所による圧力分布の相違に原因してい
ると考えられる。
However, since the powder is compressed by the molding press machine, the gas is unavoidably left inside and the sintered body is discolored or oxidized during the heat treatment (sintering), or the volume expansion of the gas is caused. Problems such as swelling and deformation of the sintered body may be observed. All of these are considered to be due to the confinement of gas during molding, and the outlet is closed due to the progress of sintering before the gas is sufficiently discharged to the outside during sintering. Also, due to the difference in the fluidity of the raw material powder when loaded into the mold, the difference in the pressure transmission to the raw material powder of the molding pressure related to the molding technology at the time of molding, etc., there is little variation in density and the like. The production of various molded bodies and / or sintered bodies is
It has become difficult. This is because the pressure applied to each molded product during the molding operation of each molded product is not uniform, but the pressure due to the location inside the molded product after pressurization due to the difference in fluidity described above. It is thought that this is due to the difference in distribution.

【0008】問題点2;上記成型体の焼結時において、
熱処理中の該成型体を収納する容器として、炭素製熱処
理用容器が知られている。これは、高温下での炭素(カ
ーボン)の優れた還元力と、多くの金属との低い濡れ性
を利用したもので、工業的に多用されている。
Problem 2; At the time of sintering the molded body,
A carbon heat treatment container is known as a container for accommodating the molded body under heat treatment. This utilizes the excellent reducing power of carbon at high temperatures and the low wettability with many metals, and is widely used industrially.

【0009】しかし、炭素製熱処理用容器は、上記した
利点があるものの、一方、熱処理する素材あるいは部品
の材種によっては、両者間で著しい冶金的反応を生じ
て、健全な状態での素材あるいは部品の製造に対して障
害となっている。例えば、素材あるいは部品として、
鉄、クロム、チタン等を選択した場合には、鉄炭化物、
クロム炭化物、チタン炭化物の生成によって、素材ある
いは部品表面の損傷、熱処理用容器の破壊が見られ好ま
しくない。このような冶金的反応を抑止する技術とし
て、両者間に酸化アルミニウム微粒子層を介在させる技
術が開発されている。しかし、微粒子間隙あるいは微粒
子表面に存在している水分、ガスによって、鉄、クロ
ム、チタン等は何らかの影響を受け、やはり、健全な状
態での素材あるいは部品の製造に対して障害となる場合
がある。
[0009] However, although the carbon heat treatment container has the above-mentioned advantages, on the other hand, depending on the material to be heat treated or the kind of parts, a remarkable metallurgical reaction occurs between the two and the material in a sound state or It is an obstacle to the manufacture of parts. For example, as materials or parts,
If you select iron, chromium, titanium, etc., iron carbide,
The formation of chromium carbide and titanium carbide undesirably damages the surface of the material or parts and destroys the heat treatment container. As a technique for suppressing such metallurgical reaction, a technique for interposing an aluminum oxide fine particle layer between the two has been developed. However, iron, chromium, titanium, etc. may be affected by moisture or gas existing in the gaps between fine particles or on the surface of fine particles, which may be an obstacle to the production of materials or parts in a sound state. .

【0010】問題点3;熱処理用容器として、窒化硼素
など窒化物製熱処理用容器、酸化カルシウム、酸化イッ
トリウムなど酸化物製熱処理用容器が知られている。こ
れは、窒化物、酸化物が高温下で多くの金属と濡れ難い
という固有の性質を利用したもので、工業的に用いられ
ている。
Problem 3; As heat treatment vessels, heat treatment vessels made of nitride such as boron nitride and heat treatment vessels made of oxide such as calcium oxide and yttrium oxide are known. This utilizes the unique property that nitrides and oxides are difficult to wet with many metals at high temperatures, and is used industrially.

【0011】しかし、窒化物熱処理用容器では、上記し
た利点があるものの、一方、雰囲気によっては使用が制
限されたり、比較的分解温度が低いなどの問題点が存在
する。また、酸化物製熱処理用容器でも前記したように
表面吸着ガス、不純物の影響を避けることが出来ない。
However, although the nitride heat treatment container has the above-mentioned advantages, there are problems that the use is restricted depending on the atmosphere and the decomposition temperature is relatively low. Further, the influence of the surface adsorption gas and impurities cannot be avoided even in the oxide heat treatment container as described above.

【0012】そこで、この発明は、組織的偏析、表面的
損傷、汚染等の障害のない焼結部材を得ることができる
焼結部材の製造方法を提供することを目的とする。
[0012] Therefore, an object of the present invention is to provide a method for producing a sintered member, which can obtain a sintered member free from structural segregation, surface damage, contamination and the like.

【0013】[0013]

【課題を解決するための手段】上記課題を解決するため
に、この発明は、第1に、所定形状を有する支持部材表
面の少なくとも一部分を、被熱処理金属の炭化物又は/
及び酸化物とした熱処理用支持部材を得る第1の工程
と、該熱処理用支持部材に被熱処理金属を加圧せず載
置、導入して加熱処理する第2の工程とを有することを
要旨とする。
In order to solve the above-mentioned problems, the present invention firstly proposes that at least a part of the surface of a supporting member having a predetermined shape is made of a carbide of a heat-treated metal or /
And a first step of obtaining a support member for heat treatment made of an oxide, and a second step of placing and introducing a metal to be heat-treated on the support member for heat treatment without applying pressure, and performing heat treatment. And

【0014】第2に、所定形状を有する支持部材表面の
少なくとも一部分を、被熱処理金属で被覆した後、該被
覆した被熱処理金属の少なくとも一部分を、当該被熱処
理金属の炭化物又は/及び酸化物とした熱処理用支持部
材を得る第1の工程と、該熱処理用支持部材に被熱処理
金属を加圧せず載置、導入して加熱処理する第2の工程
とを有することを要旨とする。
Second, after at least a part of the surface of the supporting member having a predetermined shape is coated with the heat-treatable metal, at least a part of the coated heat-treatable metal is treated with a carbide or / and an oxide of the heat-treatable metal. The gist of the present invention is to have a first step of obtaining the heat treatment support member described above, and a second step of placing and introducing the metal to be heat treated onto the heat treatment support member without applying pressure, and performing heat treatment.

【0015】第3に、所定形状を有する支持部材表面の
少なくとも一部分を、炭化クロム又は/及び酸化クロム
とした熱処理用支持部材を得る第1の工程と、該熱処理
用支持部材に原材料Crを加圧せず載置、導入して加熱
処理する第2の工程とを有することを要旨とする。
Thirdly, the first step of obtaining a heat treatment support member in which at least a part of the surface of the support member having a predetermined shape is made of chromium carbide and / or chromium oxide, and a raw material Cr is added to the heat treatment support member. The gist of the present invention is to have a second step of placing and introducing without pressing and heat treatment.

【0016】第4に、所定形状を有する支持部材表面の
少なくとも一部分を、Crで被覆した熱処理用支持部材
を得る第1の工程と、該熱処理用支持部材に原材料Cr
を加圧せず載置、導入して加熱処理する第2の工程とを
有することを要旨とする。
Fourth, a first step of obtaining a heat treatment support member in which at least a part of the surface of the support member having a predetermined shape is coated with Cr, and the raw material Cr is used for the heat treatment support member.
The second step is to place, introduce and heat-treat without heating.

【0017】第5に、所定形状を有する支持部材表面の
少なくとも一部分を、Crで被覆し、該被覆したCrの
少なくとも一部分を、炭化クロム又は/及び酸化クロム
とした熱処理用支持部材を得る第1の工程と、該熱処理
用支持部材に原材料Crを加圧せず載置、導入して加熱
処理する第2の工程とを有することを要旨とする。
Fifth, at least a part of the surface of the supporting member having a predetermined shape is coated with Cr, and at least a part of the coated Cr is chromium carbide or / and chromium oxide to obtain a supporting member for heat treatment. And the second step of placing the raw material Cr on the support member for heat treatment without applying pressure, introducing the raw material Cr, and performing heat treatment.

【0018】第6に、上記第1乃至第5の構成におい
て、前記所定形状を有する支持部材の材質は、炭素であ
ることを要旨とする。
Sixthly, in the first to fifth structures, the material of the supporting member having the predetermined shape is carbon.

【0019】第7に、上記第1乃至第5の構成におい
て、前記所定形状を有する支持部材の材質は、酸化カル
シウムであることを要旨とする。
Seventhly, in the above-described first to fifth structures, the material of the supporting member having the predetermined shape is calcium oxide.

【0020】第8に、上記第1乃至第5の構成におい
て、前記所定形状を有する支持部材の材質は、酸化イッ
トリウムであることを要旨とする。
Eighthly, in the above-mentioned first to fifth structures, the gist is that the material of the supporting member having the predetermined shape is yttrium oxide.

【0021】[0021]

【作用】上記構成において、第1に、支持部材表面の少
なくとも一部分を、被熱処理金属の炭化物又は/及び酸
化物として、これに被熱処理金属を載置、導入すること
により、加熱処理中に、熱処理用支持部材材質と被熱処
理金属とが直接接触するのを避けることが可能となる。
この結果、両者間の冶金的反応が生じることがなく、焼
結部材は表面的損傷及び汚染を受けることがなくなる。
また、被熱処理金属は加圧せずに、熱処理用支持部材上
に載置、導入することにより、加圧成型に起因する成型
圧力分布の不均一性等のための焼結の不均一化による組
織的偏析の発生を防止することが可能となる。
In the above structure, first, at least a part of the surface of the supporting member is treated as a carbide or / and an oxide of the metal to be heat treated, and the metal to be heat treated is placed and introduced into the metal to be heat treated, It is possible to avoid direct contact between the heat treatment support member material and the heat treated metal.
As a result, there is no metallurgical reaction between the two, and the sintered member is not subject to surface damage or contamination.
In addition, by placing and introducing the metal to be heat-treated on the support member for heat treatment without applying pressure, it is possible to make the sintering non-uniform due to the non-uniformity of the molding pressure distribution caused by pressure molding. It is possible to prevent the occurrence of systematic segregation.

【0022】第2に、熱処理用支持部材の表面部は、支
持部材表面の少なくとも一部分を被熱処理金属で被覆し
た後、その被覆した被熱処理金属の少なくとも一部分を
当該被熱処理金属の炭化物又は/及び酸化物としても、
前記と同様に、熱処理用支持部材材質と被熱処理金属と
の間の冶金的反応を防止することが可能となる。
Secondly, in the surface portion of the support member for heat treatment, after at least a part of the surface of the support member is coated with the metal to be heat treated, at least a part of the coated metal to be heat treated is a carbide or / and / or metal of the metal to be heat treated. As an oxide,
Similar to the above, it becomes possible to prevent the metallurgical reaction between the material for the heat treatment supporting member and the metal to be heat treated.

【0023】第3に、Cr製耐食焼結部材の製造に際し
ては、前記第1の場合と同様の主旨で、支持部材表面の
少なくとも一部分を炭化クロム又は/及び酸化クロムと
することにより、熱処理用支持部材材質と原材料Crと
の間の冶金的反応を防止することが可能となる。
Thirdly, in the production of the Cr corrosion-resistant sintered member, for the same purpose as in the first case, at least a part of the surface of the supporting member is made of chromium carbide or / and chromium oxide, so that the heat treatment is performed. It becomes possible to prevent a metallurgical reaction between the support member material and the raw material Cr.

【0024】第4に、Cr製耐食焼結部材の製造に際
し、支持部材表面の少なくとも一部分をCr膜で被覆し
ても、上記と同様に、熱処理用支持部材材質と原材料C
rとの間の冶金的反応を防止することが可能となる。
Fourthly, in the production of the Cr corrosion resistant sintered member, even if at least a part of the surface of the supporting member is covered with a Cr film, the supporting member material for heat treatment and the raw material C are similarly used.
It is possible to prevent metallurgical reactions with r.

【0025】第5に、Cr製耐食焼結部材の製造に際
し、前記第2の場合と同様の主旨で、支持部材表面の少
なくとも一部分をCr膜で被覆した後、そのCr被膜の
少なくとも一部分を炭化クロム又は/及び酸化クロムと
しても、熱処理用支持部材材質と原材料Crとの間の冶
金的反応を防止することが可能となる。
Fifth, in the production of a Cr corrosion-resistant sintered member, for the same purpose as in the second case, after at least a part of the surface of the supporting member is covered with a Cr film, at least a part of the Cr film is carbonized. Even if chromium and / or chromium oxide is used, it is possible to prevent a metallurgical reaction between the heat treatment support member material and the raw material Cr.

【0026】第6に、支持部材の材質は、高温下での優
れた還元力と、多くの金属との低い濡れ性を有する炭素
とすることにより、上記した焼結部材の表面的損傷及び
汚染の防止作用をより良く達成することが可能となる。
Sixth, the supporting member is made of carbon, which has excellent reducing power at high temperature and low wettability with many metals, so that the above-mentioned surface damage and contamination of the sintered member are caused. It is possible to achieve a better prevention effect of.

【0027】第7、第8に、支持部材の材質は、高温下
での多くの金属と低い濡れ性を有する酸化カルシウム又
は酸化イットリウムとすることにより、上記第6の場合
とほぼ同様の作用を得ることが可能となる。
Seventh and eighth, by using calcium oxide or yttrium oxide, which has low wettability with many metals at high temperature, as the material of the supporting member, the same effect as in the case of the sixth case can be obtained. It becomes possible to obtain.

【0028】[0028]

【実施例】以下、この発明の実施例を、表1を参照し
て、具体的な例によって説明する。本実施例の製造方法
の主旨は、対象とする被熱処理金属(原材料粉末)に外
圧力を与えることなく、所定の表面条件を満たした熱処
理用支持部材に載置、導入した後、被熱処理金属を熱処
理用支持部材と共に加熱・焼結して、焼結部材を得るこ
とにある。従って、対象とする被熱処理金属の種類を、
特に限定する必要はなく、ここでは、まずCrを被熱処
理金属の代表金属として選定し、具体的に説明する。
EXAMPLES Examples of the present invention will be described below with reference to Table 1 by way of specific examples. The main purpose of the manufacturing method of this embodiment is to place the target metal to be heat-treated (raw material powder) on a heat-treatment supporting member satisfying a predetermined surface condition without applying an external pressure, and after introducing the heat-treated metal Is to heat and sinter together with the support member for heat treatment to obtain a sintered member. Therefore, the type of target heat treated metal is
It is not particularly limited, and here, Cr is first selected as a representative metal of the heat-treated metals and specifically described.

【0029】実験;表面を極めて清浄化した、厚さ3
mmの高純度Cr板を使用して、金属Cr板製熱処理用容
器を作製した。アーク溶解後鍛造して得たCrケーキを
使用して、Cr製耐触フランジ部品を製作した。前記金
属Cr板製熱処理用容器に、上記Cr製耐触フランジ部
品を直接接触する状態で入れて、真空中810℃の加熱
処理を行う実験を行った。その結果、Cr板製熱処理用
容器とCr製耐触フランジ部品との間は、強固な相互拡
散現象が見られ、Cr製耐触フランジ部品を損傷なく容
器から取出すことは出来ず、健全なCr製耐触フランジ
部品を得ることは出来なかった。但しCr製耐触フラン
ジ部品の表面汚染および内部への不純物の侵入は全く無
かった。
Experiment: Surface was extremely cleaned, thickness 3
Using a high purity Cr plate of mm, a heat treatment container made of a metal Cr plate was prepared. Using Cr cake obtained by forging after arc melting, Cr anti-corrosion flange parts were manufactured. An experiment was conducted in which the Cr anticorrosion flange component was placed in direct contact with the metal Cr plate heat treatment container and heat-treated at 810 ° C. in vacuum. As a result, a strong interdiffusion phenomenon was observed between the Cr plate heat treatment container and the Cr anti-corrosion flange parts, and the Cr anti-corrosion flange parts could not be taken out from the container without damage, and sound Cr It was not possible to obtain a manufactured anti-corrosion flange part. However, there was absolutely no surface contamination of the Cr anti-corrosion flange parts and no penetration of impurities into the inside.

【0030】実験;表面を極めて清浄化した厚さ3mm
の高純度Cr板を使用して、金属Cr板製熱処理用容器
を作製した。十分脱ガス処理したCr粉を4トン/cm2
でプレスした直径42mmのCr粉製耐蝕性歯車部品を製
作した。前記金属Cr板製熱処理用容器に、上記Cr粉
製耐蝕性歯車部品を直接接触する状態で入れて、真空中
810℃の加熱処理を行う実験を行った。その結果、C
r製歯車部品では、同実験と同じ加熱処理を与えたに
も拘らず、Cr板製熱処理用容器とCr粉製歯車部品と
の間には、実験の場合のような、強固な相互拡散現象
が見られず、実験の場合より損傷の程度は低くCr部
品を容器から取出すことが出来た。しかし、局所的な溶
着部分が引きはずし跡として残った。なお、表面汚染お
よび内部への不純物の侵入は実験と同様に、全く無か
った。即ち、本発明者らは、両実験によって取出し
時の素材あるいは部品の表面損傷問題の相違を除くと、
表面汚染および内部への不純物の侵入の観点からは、被
熱処理金属(原材料)と同じ材質の高純度金属が熱処理
用容器(熱処理用支持部材)として、有用である観察知
見を得た。しかも、後者実験の場合の方が、表面損傷
問題が軽微であった事実を考察すると、後者の実験に
先立ち、Cr粉は十分脱ガス処理し加熱処理に供した
が、それにも拘らず、なおCr粉に残存していた適度の
表面ガスが、表面を極めて清浄化した熱処理用容器の表
面に作用し、濡れにくい状態の被膜を適度に生成したと
考えられる。微少分析の結果生成物は、Cr,O,Cの
化合物であった。
Experiment: thickness of 3 mm with extremely clean surface
A high-purity Cr plate of No. 3 was used to prepare a metal Cr plate heat treatment container. 4 ton / cm 2 of fully degassed Cr powder
Corrosion resistant gear parts made of Cr powder with a diameter of 42 mm pressed by. An experiment was conducted in which the above-mentioned Cr powder corrosion-resistant gear part was placed in direct contact with the metal Cr plate heat treatment container and subjected to heat treatment at 810 ° C. in a vacuum. As a result, C
Although the r-made gear parts were subjected to the same heat treatment as in the same experiment, a strong mutual diffusion phenomenon was observed between the Cr plate heat treatment container and the Cr powder-made gear parts as in the case of the experiment. No damage was observed, and the degree of damage was lower than in the case of the experiment, and the Cr part could be taken out from the container. However, the locally welded part remained as a trip mark. As with the experiment, neither surface contamination nor penetration of impurities into the interior was observed. That is, the present inventors, except for the difference in the surface damage problem of the material or parts at the time of extraction by both experiments,
From the viewpoint of surface contamination and invasion of impurities into the inside, it was found that a high-purity metal having the same material as the heat-treated metal (raw material) is useful as a heat treatment container (heat treatment support member). Moreover, considering the fact that the surface damage problem was minor in the latter experiment, the Cr powder was sufficiently degassed and subjected to heat treatment prior to the latter experiment, but nevertheless, It is considered that the appropriate amount of surface gas remaining in the Cr powder acted on the surface of the heat treatment container whose surface was extremely cleaned, and appropriately produced a film that was difficult to wet. As a result of microanalysis, the product was a compound of Cr, O and C.

【0031】実験,実施例1;実験、のいずれ
も、予め製造したCr素材(インゴット)からフランジ
部品(実験)、歯車部品(実験)を製造、加工し
て、被熱処理金属として供試しているので、最終製品に
到達する迄の工数の中にCr素材(インゴット)を製作
する工程が含まれる結果、最終製品価格に影響を与え
る。また実験の様に、粉末成型体(Cr粉)を被熱処
理金属とした時には、ポア、ガスの存在量や存在場所に
ばらつきが生じやすく、特に閉じられた内部にガスが存
在していた場合、熱処理時に爆発的なガス放出が起り、
表面損傷の原因ともなっている場合がある。そこで、熱
処理中に内部より単間にガス放出が行える様にするため
に、使用する被熱処理金属の状態を、実験の場合の様
なCr素材(インゴット)即ちあらかじめ塊状とした
り、実験の場合の様な粉末成型体即ちあらかじめ塊状
の状態とせず、実験として、ガス放出が簡単に行える
様にするために、粉末状のままで熱処理用容器に導入し
た実験を試みた。実験の示唆によって、熱処理用容器
は、炭素を素材としてその表面に、被熱処理金属と同じ
Crを厚さ0.1μmイオンプレーティング法で被覆し
た。その結果、ガスおよび不純物のより少ない、表面損
傷のより少ない焼結部材を得た(実験、実施例1)。
なお、熱処理用容器として、実験、のように厚さ3
mmの高純度Cr板を使用した金属Cr板製熱処理用容器
を使用したところ、金属Cr板の品質ばらつきに起因す
ると考えられる被熱処理金属中のガス量に、ばらつきが
発生する傾向にあった(実験 比較例1)。
In each of the experiment and the example 1; the experiment, a flange part (experiment) and a gear part (experiment) were manufactured and processed from a pre-produced Cr material (ingot) and used as a heat-treated metal. Therefore, as a result of including the step of manufacturing the Cr material (ingot) in the man-hours required to reach the final product, the price of the final product is affected. Also, as in the experiment, when the powder compact (Cr powder) is used as the heat-treated metal, the amount and location of pores and gas are likely to vary, especially when gas is present in the closed interior. Explosive gas release during heat treatment,
It may also cause surface damage. Therefore, in order to allow the gas to be released from the inside during the heat treatment in a singular manner, the state of the heat-treated metal to be used is made of a Cr material (ingot) as in the case of the experiment, that is, a lump in advance, or in the case of the experiment. In order to make it possible to easily release gas, an experiment was carried out in which the powder compact was introduced into the heat treatment container as it was in order to make it easy to discharge gas. According to the suggestion of the experiment, the heat treatment container was made of carbon as a raw material, and the surface thereof was coated with the same Cr as the heat-treated metal by an ion plating method with a thickness of 0.1 μm. As a result, a sintered member having less gas and impurities and less surface damage was obtained (experiment, Example 1).
As a container for heat treatment, the thickness of 3
When a heat treatment container made of a metal Cr plate using a high-purity Cr plate of mm was used, the amount of gas in the heat-treated metal, which is considered to be due to the quality variation of the metal Cr plate, tended to vary ( Experiment Comparative Example 1).

【0032】実験 実施例2;さらに本発明者らは、
上記実験では、使用した高純度Cr板製熱処理用容
器の表面を極めて清浄化して使用したが、被熱処理金属
の状態の差異によって、その結果に相違がでたものと上
記結果を考察した。そこで本発明者らは、実験とし
て、炭素製熱処理用容器の表面にあらかじめ、スパッタ
リング法で、厚さが0.1μm程度の極薄いCr被膜を
生成させた熱処理用容器を作製した。この熱処理用容器
を用いて、実験と同様の加熱処理を行ったところ、熱
処理用容器から表面損傷なく、健全な状態で被熱処理金
属(実施例2)を取出せた上、該部品は、表面汚染およ
び内部への不純物の侵入は全く無かった。
Experimental Example 2;
In the above experiment, the surface of the high-purity Cr plate heat treatment container used was extremely cleaned before use, but the above results were considered to be different due to the difference in the state of the heat-treated metal. Therefore, as an experiment, the present inventors produced a heat treatment container in which an extremely thin Cr coating having a thickness of about 0.1 μm was previously formed on the surface of the carbon heat treatment container by a sputtering method. When this heat treatment container was used to perform the same heat treatment as in the experiment, the heat-treated metal (Example 2) could be taken out from the heat treatment container in a sound state without surface damage, and the component was not contaminated by surface contamination. There was no intrusion of impurities into the interior.

【0033】実験 実施例3,4;実験として、炭
素の表面に厚さ0.1μm程度の極薄いCr被膜を生成
させた後、その表面をスパッタリング法で、雰囲気を調
整しながら、Cr2 3 として、(Cr−Cr2 3
被膜を炭素の上に生成させた熱処理用容器を作製した
(実施例3)。また、同様にして厚さ0.1μm程度の
極薄い(Cr−Cr3 2 )被膜を炭素の上に生成させ
た熱処理用容器を作製した(実施例4)。これらの熱処
理用容器を用いて、実験と同様の加熱処理を行った
ところ、熱処理用容器から表面損傷なく、健全な状態で
被熱処理金属Crを取出すことが出来た上、該部品は、
表面汚染および内部への不純物の侵入は全く無かった
(実施例3,4)。
Experiments 3 and 4; As an experiment, an extremely thin Cr film having a thickness of about 0.1 μm was formed on the surface of carbon, and then the surface was subjected to sputtering to control the atmosphere and Cr 2 O. 3 as (Cr-Cr 2 O 3 )
A heat treatment container having a coating formed on carbon was produced (Example 3). Further, in the same manner, a container for heat treatment was produced in which an extremely thin (Cr—Cr 3 C 2 ) coating having a thickness of about 0.1 μm was formed on carbon (Example 4). When heat treatment similar to the experiment was performed using these heat treatment vessels, the heat-treated metal Cr could be taken out from the heat treatment vessel in a sound state without surface damage, and the parts were
There was no surface contamination or intrusion of impurities into the interior (Examples 3 and 4).

【0034】実験,実施例5、比較例2;実験とし
て、真空蒸着法で、雰囲気を調整しながら、厚さ100
μm程度の(Cr−Cr2 3 )被膜を炭素の上に生成
させた熱処理用容器を作製した。この熱処理用容器を用
いて、実験と同様の加熱処理を行ったところ、熱処
理用容器から表面損傷なく、健全な状態で被熱処理金属
Crを取出すことが出来た上、該部品は、表面汚染およ
び内部への不純物の侵入は、全くなかった(実施例
5)。また、スパッタリング法で、雰囲気を調整しなが
ら、厚さが0.01μm程度の(Cr−Cr2 3 )被
膜を炭素の上に生成させた熱処理用容器を作製した。こ
の熱処理用容器を用いて、実験と同様の加熱処理を
行ったところ、軽度の表面損傷を受けていたが、ほぼ健
全な状態で被熱処理金属Crを、熱処理用容器から、取
出すことができた。しかし、被膜の厚さが必要量なかっ
たことに起因し、黒鉛の表面や内部に存在する水分、ガ
スが、熱処理中の被熱処理金属Crにまで拡散し、これ
らの表面変色、汚染および内部への不純物侵入を招き、
健全なCr部品を得ることは出来なかった(比較例
2)。
Experiment, Example 5, Comparative Example 2; As an experiment, a thickness of 100 was obtained by vacuum evaporation while adjusting the atmosphere.
A container for heat treatment was produced in which a (Cr—Cr 2 O 3 ) coating of about μm was formed on carbon. When this heat treatment container was used to perform the same heat treatment as in the experiment, it was possible to take out the heat-treated metal Cr in a sound state from the heat treatment container in a sound state, and at the There was no intrusion of impurities into the inside (Example 5). Further, a heat treatment container in which a (Cr—Cr 2 O 3 ) coating having a thickness of about 0.01 μm was formed on carbon was prepared by adjusting the atmosphere by a sputtering method. When this heat treatment container was used to perform the same heat treatment as in the experiment, it was found that the metal Cr to be heat treated could be taken out from the heat treatment container in a substantially sound state although it was slightly damaged by the surface. . However, due to the fact that the thickness of the coating was not required, moisture and gas existing on the surface and inside of the graphite diffused to the heat-treated metal Cr during heat treatment, causing surface discoloration, contamination, and internal Cause the invasion of impurities,
It was not possible to obtain a sound Cr part (Comparative Example 2).

【0035】実験 実施例6,7,8;上記した実験
では、熱処理用容器の素材材質としてC
r板や炭素を使用し、その表面を所定の条件を有する金
属クロムや酸化クロムを被覆して使用した(実施例1〜
6)。しかし、本発明では、これらに限ることなくその
目的を達成することができる。即ち、熱処理用容器の素
材材質として、上記したCr板や炭素以外の酸化カルシ
ウム又は酸化イットリウムであっても、表面を所定条件
とした熱処理用容器を使用し、かつ被熱処理金属(原材
料)を加圧せず前記熱処理用容器に載置・導入し、被熱
処理金属(原材料)を前記熱処理用容器と共に加熱、焼
結する本発明方法によれば、効果を達成出来る(実施例
6、実施例7)ことが判った。即ち、酸化カルシウム製
の熱処理用容器の表面に0.1μmのCrを被覆した
後、そのCrを炭化クロム(主としてCr3 2 )とし
たもの(実施例6)、および酸化イットリウム製の熱処
理用容器の表面に0.1μmのCrを被覆した後、その
Crを酸化クロム(主としてCr2 3 )としたもの
(実施例7)である。また、酸化カルシウム製の熱処理
用容器の表面に、0.1μmのCrを被覆した後、その
Crを炭化クロム(主としてCr3 2 )、および酸化
クロム(主としてCr2 3 )とを混在させたもの(実
施例8)である。
Experiments Examples 6, 7 and 8: In the above experiment, C was used as the material of the heat treatment container.
An r plate or carbon was used, and the surface thereof was coated with metallic chromium or chromium oxide having predetermined conditions (Examples 1 to 1).
6). However, the present invention is not limited to these, and the object can be achieved. That is, even if the above-mentioned Cr plate or calcium oxide or yttrium oxide other than carbon is used as the material for the heat treatment container, the heat treatment container whose surface is set to a predetermined condition is used, and the metal to be heat treated (raw material) is added. According to the method of the present invention in which the metal to be heat treated (raw material) is heated and sintered together with the container for heat treatment by placing and introducing into the container for heat treatment without pressing, the effect can be achieved (Examples 6 and 7). ) Was found. That is, after coating the surface of a heat treatment container made of calcium oxide with 0.1 μm of Cr, the Cr was changed to chromium carbide (mainly Cr 3 C 2 ) (Example 6), and yttrium oxide for heat treatment was used. The surface of the container was coated with 0.1 μm of Cr, and then Cr was changed to chromium oxide (mainly Cr 2 O 3 ) (Example 7). In addition, after coating the surface of the heat treatment container made of calcium oxide with 0.1 μm of Cr, the Cr is mixed with chromium carbide (mainly Cr 3 C 2 ) and chromium oxide (mainly Cr 2 O 3 ). (Example 8).

【0036】被熱処理金属(原材料)を熱処理用容器へ
導入・載置した後、熱処理温度、原料粒径の調節、焼結
助材の添加などで、焼結部材の空隙率、即ち理論密度に
対する空隙の割合を、30〜95%程度の広い範囲に調
節することが可能である。また、被熱処理金属(原材
料)として、Crを代表例として述べたが、被熱処理金
属(原材料)がTiの場合には、熱処理用容器表面をT
iとして、その少なくとも一部を酸化チタン又は/及び
炭化チタンとすることによって、同様に高品質の焼結部
材を得ることが出来る。
After the metal to be heat treated (raw material) is introduced and placed in the heat treatment container, the porosity of the sintered member, that is, the theoretical density, is adjusted by adjusting the heat treatment temperature, the grain size of the raw material, the addition of the sintering aid, and the like. It is possible to adjust the ratio of voids to a wide range of about 30 to 95%. Although Cr has been described as a representative example of the metal to be heat-treated (raw material), when the metal to be heat-treated (raw material) is Ti, the surface of the heat-treating container is T
By using at least a part of titanium oxide and / or titanium carbide as i, a similarly high quality sintered member can be obtained.

【0037】本発明者らは、炭素製熱処理用容器の上に
金属被膜を生成させた熱処理用容器であっても、表面損
傷および表面汚染および内部への不純物の侵入のない、
健全な状態の製品や半製品が得られること、しかし、炭
素製熱処理用容器の上に金属被膜の厚さが不適切である
と、強固な相互拡散現象が見られ好ましくないことが判
った。
The present inventors have found that even in a heat treatment container in which a metal coating film is formed on a carbon heat treatment container, there is no surface damage, surface contamination, and intrusion of impurities into the interior.
It was found that a product or a semi-finished product in a healthy state can be obtained, but if the thickness of the metal coating on the carbon heat treatment container is inappropriate, a strong mutual diffusion phenomenon is observed, which is not preferable.

【0038】以上述べた様に、上記知見に基づき本発明
者は、前記した焼結前の原料粉体の受ける圧力が、各焼
結部材毎のみならず各焼結部材内部のミクロ的部分につ
いても一定となる技術についての検討及び前記した実験
検討とを相乗し結果、本発明を完成した。
As described above, based on the above findings, the present inventor has found that the pressure applied to the raw material powder before sintering is not only for each sintered member but also for the microscopic portion inside each sintered member. The present invention has been completed as a result of a synergistic effect of the study on the technology that makes constant and the above-mentioned experimental study.

【0039】[0039]

【表1】 条 件 No. 被熱処理金属 熱処理支持部材 熱処理 条件 容器の 容器の 素材 表面 実験:参考 アークメルトした Cr Cr 真空 Crケーキ 810 ℃ (Cr製耐触 フランジ部品) 実験:参考 脱ガス処理した Cr Cr 同上 Cr粉成型体 (Cr粉製耐蝕性 歯車部品) 実験:実施例1 脱ガス処理した 炭素 炭素表面に 同上 Cr粉 0.1 μm 厚さのCrを イオン プレーティング法 で被覆 同上 :比較例1 実験と同じ Cr板 Cr板のまま 同上 (厚さ 3mm) 実験:実施例2 実験と同じ 炭素 炭素表面に 同上 0.1 μm 厚さのCrを スパッタリング法 で被覆 実験:実施例3 実験と同じ 炭素 炭素表面に 同上 0.1 μm 厚さの (Cr2 3 ) 被膜を スパッタリング法 で被覆 実験:実施例4 実験と同じ 同上 炭素表面に 同上 0.1 μm 厚さの (Cr3 2 ) 被膜を スパッタリング法 で被覆 実験:実施例5 実験と同じ 同上 炭素表面に 同上 100 μm 厚さのCrを 真空蒸着法 で被覆 同上 :比較例2 実験と同じ 同上 炭素表面に 同上 0.01μm 厚さのCrを スパッタリング法 で被覆 実験:実施例6 実験と同じ 酸化 酸化カル 同上 カル シウム表面に シウ 0.1 μm ム 厚さのCrを 被覆 その一部を スパッタリング法 でCr3 2 とした 同上 :実施例7 実験と同じ 酸化 酸化イット 同上 イット リウム表面に リウム 0.1 μm 厚さのCrを 被覆 その一部を スパッタリング法 でCr2 3 とした 同上 :実施例8 実験と同じ 酸化 酸化カル 同上 カル シウム表面に シウ 0.1 μm ム 厚さのCrを 被覆 その一部を スパッタリング法 でCr2 3 と Cr3 2 との 混在とした[Table 1] Condition No. Heat treated metal Heat treated support member Heat treatment condition Container material Surface test: Reference Arc melted Cr Cr Vacuum Cr cake 810 ° C (Cr contact resistant flange parts) Experiment: Reference Degassed Cr Cr Same as above Cr powder compact ( Cr powder corrosion resistance gear parts) Experiment: Example 1 Degassed carbon Carbon Same as above Cr powder 0.1 μm thick Cr was coated by ion plating method Same as above: Comparative Example 1 Same Cr plate Cr plate as experiment Same as above (thickness: 3 mm) Experiment: Same as in Example 2 Experiment Carbon: Carbon surface was coated with Cr of 0.1 μm thickness as above by sputtering method Experiment: Same as Example 3 Experiment: Same as above in carbon carbon surface of 0.1 μm thickness ( Cr 2 O 3) coating experiment a film by a sputtering method: the same ditto carbon surface as in example 4 experiments ibid 0.1 [mu] m thickness (Cr 3 C 2) scan the film Coating by Tattering method: Example 5 Same as in experiment Same as above Same as above Carbon coating with 100 μm thickness of Cr as above by vacuum deposition method Same as above: Comparative example 2 Same as in experiment Same as above Same as carbon surface sputtering with 0.01 μm thickness of Cr as above Experiment: Same as in Example 6 Same as experiment: Oxidation of calcium oxide Same as above Oxidation of calcium on surface of Cr with 0.1 μm thickness of Cr 3 C 2 by sputtering method Same as above: Example 7 Same as experiment Oxidation Yt Oxide Same as above Yttrium surface coated with Cr 0.1 μm thick Cr part of which was made Cr 2 O 3 by the same method Same as above: Example 8 Same as experiment Oxidation calcium oxide Same as above Si 0.1 μm on surface of calcium Coated with a thickness of Cr, part of which was mixed with Cr 2 O 3 and Cr 3 C 2 by sputtering

【0040】[0040]

【発明の効果】以上説明したように、この発明によれ
ば、第1に、熱処理用支持部材表面の少なくとも一部分
を被熱処理金属の炭化物又は/及び酸化物としたため、
加熱処理中に、熱処理用支持部材材質と被熱処理金属と
の直接接触を避けることが可能となって、両者間の冶金
的反応が生じることがなく、表面的損傷及び汚染の障害
のない焼結部材を得ることができる。また、被熱処理金
属は加圧せずに熱処理用支持部材上に載置、導入して加
熱処理をするようにしたため、加圧成型に起因する成型
圧力分布の不均一性等による焼結の不均一化を防止する
ことができて組織的偏析のない焼結部材を得ることがで
きる。
As described above, according to the present invention, firstly, since at least a part of the surface of the heat treatment supporting member is made of the carbide or / and the oxide of the metal to be heat treated,
It is possible to avoid direct contact between the heat-treating support member material and the heat-treatable metal during the heat treatment, no metallurgical reaction occurs between the two, and there is no surface damage or contamination damage. The member can be obtained. In addition, since the metal to be heat treated is placed on the support member for heat treatment without being pressed and is introduced and subjected to heat treatment, the non-uniformity of the sintering due to the non-uniformity of the molding pressure distribution caused by the pressure molding, etc. It is possible to prevent homogenization and obtain a sintered member without structural segregation.

【0041】第2に、熱処理用支持部材は、その表面の
少なくとも一部分を被熱処理金属で被覆した後、その被
覆した被熱処理金属の少なくとも一部分を当該被熱処理
金属の炭化物又は/及び酸化物としたため、上記第1の
発明と同様の効果を得ることができる。
Secondly, the heat-treating support member has at least a portion of its surface coated with the metal to be heat-treated, and at least a portion of the coated metal to be heat-treated is a carbide or / and an oxide of the metal to be heat-treated. The same effect as that of the first invention can be obtained.

【0042】第3に、Cr製耐食焼結部材の製造に際
し、支持部材表面の少なくとも一部分を炭化クロム又は
/及び酸化クロムとしたため、前記第1の発明と同様の
効果を得ることができる。
Thirdly, at the time of producing the Cr corrosion resistant sintered member, at least a part of the surface of the supporting member is made of chromium carbide and / or chromium oxide, so that the same effect as the first invention can be obtained.

【0043】第4、第5に、Cr製耐食焼結部材の製造
に際し、支持部材表面の少なくとも一部分をCr膜で被
覆するか、又は支持部材表面の少なくとも一部分をCr
膜で被覆した後、そのCr膜の少なくとも一部分を炭化
クロム又は/及び酸化クロムとしたため、上記第3の発
明と同様の効果を得ることができる。
Fourthly and fifthly, in the production of the Cr corrosion resistant sintered member, at least a part of the surface of the supporting member is coated with a Cr film, or at least a part of the surface of the supporting member is made of Cr.
After coating with the film, since at least a part of the Cr film is made of chromium carbide and / or chromium oxide, the same effect as the third invention can be obtained.

【0044】第6に、支持部材の材質を炭素としたた
め、その高温下での優れた還元力と多くの金属との低い
濡れ性により、上記第1乃至第5の発明における焼結部
材の表面的損傷及び汚染の防止効果をより良く達成する
ことができる。
Sixth, since the material of the supporting member is carbon, the surface of the sintered member in the first to fifth inventions is excellent due to its excellent reducing power at high temperature and low wettability with many metals. The effect of preventing physical damage and pollution can be better achieved.

【0045】第7、第8に、支持部材の材質を酸化カル
シウム又は酸化イットリウムとしたため、その高温下で
の多くの金属との低い濡れ性により、上記第6の発明と
ほぼ同様の効果が得られる。
Seventh and eighth, since the material of the supporting member is calcium oxide or yttrium oxide, its low wettability with many metals at high temperature provides substantially the same effect as the sixth invention. To be

───────────────────────────────────────────────────── フロントページの続き (72)発明者 奥冨 功 東京都府中市東芝町1番地 株式会社東芝 府中工場内 (72)発明者 関口 薫旦 神奈川県横浜市磯子区新杉田町8番地 株 式会社東芝横浜事業所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Isao Okutomi No. 1 Toshiba-cho, Fuchu-shi, Tokyo Inside the Fuchu factory, Toshiba Corp. (72) Inventor Kadan Sekiguchi, 8 Shinsita-cho, Isogo-ku, Yokohama, Kanagawa Inside the Yokohama office

Claims (8)

【特許請求の範囲】[Claims] 【請求項1】 所定形状を有する支持部材表面の少なく
とも一部分を、被熱処理金属の炭化物又は/及び酸化物
とした熱処理用支持部材を得る第1の工程と、該熱処理
用支持部材に被熱処理金属を加圧せず載置、導入して加
熱処理する第2の工程とを有することを特徴とする焼結
部材の製造方法。
1. A first step of obtaining a support member for heat treatment in which at least a part of a surface of the support member having a predetermined shape is a carbide or / and an oxide of a metal to be heat treated, and a metal to be heat treated on the support member for heat treatment. A second step of placing, introducing and heat-treating, without applying pressure.
【請求項2】 所定形状を有する支持部材表面の少なく
とも一部分を、被熱処理金属で被覆した後、該被覆した
被熱処理金属の少なくとも一部分を、当該被熱処理金属
の炭化物又は/及び酸化物とした熱処理用支持部材を得
る第1の工程と、該熱処理用支持部材に被熱処理金属を
加圧せず載置、導入して加熱処理する第2の工程とを有
することを特徴とする焼結部材の製造方法。
2. A heat treatment in which at least a part of the surface of a supporting member having a predetermined shape is coated with a heat-treatable metal, and at least a portion of the coated heat-treatable metal is a carbide or / and an oxide of the heat-treatable metal. Of the sintered member, comprising: a first step of obtaining a supporting member for heat treatment; and a second step of placing a metal to be heat-treated on the supporting member for heat treatment without applying pressure, introducing the metal to be heat-treated, and performing heat treatment. Production method.
【請求項3】 所定形状を有する支持部材表面の少なく
とも一部分を、炭化クロム又は/及び酸化クロムとした
熱処理用支持部材を得る第1の工程と、該熱処理用支持
部材に原材料Crを加圧せず載置、導入して加熱処理す
る第2の工程とを有することを特徴とする焼結部材の製
造方法。
3. A first step of obtaining a heat treatment support member in which at least a part of the surface of the support member having a predetermined shape is made of chromium carbide and / or chromium oxide, and a raw material Cr is pressed against the heat treatment support member. A second step in which the sintered member is placed, introduced and heated.
【請求項4】 所定形状を有する支持部材表面の少なく
とも一部分を、Crで被覆した熱処理用支持部材を得る
第1の工程と、該熱処理用支持部材に原材料Crを加圧
せず載置、導入して加熱処理する第2の工程とを有する
ことを特徴とする焼結部材の製造方法。
4. A first step of obtaining a heat treatment support member in which at least a part of the surface of the support member having a predetermined shape is coated with Cr, and a raw material Cr is placed and introduced on the heat treatment support member without applying pressure. And a second step of performing heat treatment.
【請求項5】 所定形状を有する支持部材表面の少なく
とも一部分を、Crで被覆し、該被覆したCrの少なく
とも一部分を、炭化クロム又は/及び酸化クロムとした
熱処理用支持部材を得る第1の工程と、該熱処理用支持
部材に原材料Crを加圧せず載置、導入して加熱処理す
る第2の工程とを有することを特徴とする焼結部材の製
造方法。
5. A first step of obtaining a support member for heat treatment, in which at least a part of the surface of the support member having a predetermined shape is coated with Cr, and at least a part of the coated Cr is chromium carbide or / and chromium oxide. And a second step of placing the raw material Cr on the support member for heat treatment without applying pressure, introducing the raw material Cr, and performing heat treatment.
【請求項6】 前記所定形状を有する支持部材の材質
は、炭素であることを特徴とする請求項1乃至5の何れ
かに記載の焼結部材の製造方法。
6. The method for manufacturing a sintered member according to claim 1, wherein the material of the support member having the predetermined shape is carbon.
【請求項7】 前記所定形状を有する支持部材の材質
は、酸化カルシウムであることを特徴とする請求項1乃
至5の何れかに記載の焼結部材の製造方法。
7. The method for manufacturing a sintered member according to claim 1, wherein the material of the supporting member having the predetermined shape is calcium oxide.
【請求項8】 前記所定形状を有する支持部材の材質
は、酸化イットリウムであることを特徴とする請求項1
乃至5の何れかに記載の焼結部材の製造方法。
8. The material of the supporting member having the predetermined shape is yttrium oxide.
6. The method for manufacturing a sintered member according to any one of 5 to 5.
JP14090993A 1993-06-11 1993-06-11 Manufacturing method of sintered member Expired - Lifetime JP3442427B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP14090993A JP3442427B2 (en) 1993-06-11 1993-06-11 Manufacturing method of sintered member

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP14090993A JP3442427B2 (en) 1993-06-11 1993-06-11 Manufacturing method of sintered member

Publications (2)

Publication Number Publication Date
JPH06346106A true JPH06346106A (en) 1994-12-20
JP3442427B2 JP3442427B2 (en) 2003-09-02

Family

ID=15279641

Family Applications (1)

Application Number Title Priority Date Filing Date
JP14090993A Expired - Lifetime JP3442427B2 (en) 1993-06-11 1993-06-11 Manufacturing method of sintered member

Country Status (1)

Country Link
JP (1) JP3442427B2 (en)

Also Published As

Publication number Publication date
JP3442427B2 (en) 2003-09-02

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