JPH0860270A - Production of ti sintered compact and supporting material at the time of sintering therefor - Google Patents
Production of ti sintered compact and supporting material at the time of sintering thereforInfo
- Publication number
- JPH0860270A JPH0860270A JP19324994A JP19324994A JPH0860270A JP H0860270 A JPH0860270 A JP H0860270A JP 19324994 A JP19324994 A JP 19324994A JP 19324994 A JP19324994 A JP 19324994A JP H0860270 A JPH0860270 A JP H0860270A
- Authority
- JP
- Japan
- Prior art keywords
- sintering
- sintered body
- tray
- support material
- sintered compact
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- Powder Metallurgy (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、Ｔｉ焼結体の製造方法
及びそのための焼結時支持材に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a Ti sintered body and a supporting material for sintering thereof.
【０００２】[0002]
【従来の技術】近年、金属粉末射出成形法（Ｍｅｔａｌ
Ｉｎｊｅｃｔｉｏｎ Ｍｏｌｄｉｎｇ；以下、ＭＩＭ
という。）や圧粉焼結などにより、エレクトロニクス、
精密機械、医療、自動車など幅広い分野の部品が焼結品
とし提供されるようになっている。2. Description of the Related Art In recent years, metal powder injection molding (Metal)
Injection Molding; Below, MIM
Say. ) And compaction sintering,
Parts in a wide range of fields such as precision machinery, medical care, and automobiles are now available as sintered products.
【０００３】こうした焼結品の原料としては、ステンレ
ス鋼（ＳＵＳ），Ｆｅ−Ｎｉ，低合金鋼，ハイス，耐熱
鋼などが使用されており、焼結時には、Ａｌ2 Ｏ3 ，Ｚ
ｒＯ 2 ，ＳｉＯ2 ，ＳｉＣ，Ｓｉ3 Ｎ4 などのセラミッ
クス製のトレイなどに成形品を載置していた。A raw material for such a sintered product is a stainless steel.
Steel (SUS), Fe-Ni, low alloy steel, high speed steel, heat resistant
Steel, etc. is used, and during sintering, Al2 O3 , Z
rO 2 , SiO2 , SiC, Si3 NFour Such as ceramic
The molded product was placed on a tray made of cous.
【０００４】[0004]
【発明が解決しようとする課題】ところで、最近では、
特に軽量・高強度で人体とも馴染みがよいＴｉ粉末を用
いた焼結品が望まれるようになってきた。しかし、Ｔｉ
は活性が高いため、Ａｌ2 Ｏ3 などと反応してしまい、
焼結中にトレイとくっついてしまったり、割れたりする
という問題があった。また、仮に割れなどが起こらない
としても、焼結品の延性が不十分となり、最終製品が脆
く割れ易いという問題があった。By the way, recently,
In particular, a sintered product using Ti powder, which is lightweight, has high strength, and is familiar to the human body, has been desired. However, Ti
Has high activity, it reacts with Al 2 O 3 etc.,
There was a problem of sticking to the tray or cracking during sintering. Even if cracks do not occur, the ductility of the sintered product is insufficient, and the final product is brittle and easily cracked.
【０００５】そこで、本発明は、十分なる延性を有する
Ｔｉ焼結体を割れなどを生じることなく製造する方法及
びそのための焼結時支持材を提供することを目的とす
る。Therefore, an object of the present invention is to provide a method for producing a Ti sintered body having sufficient ductility without causing cracks and the like, and a supporting material during sintering for the method.
【０００６】[0006]
【課題を解決するための手段、作用及び効果】かかる目
的を達成するためになされた本発明のＴｉ焼結体の製造
方法は、希土類酸化物を９０％以上含有する支持材上に
載置して焼結することを特徴とする。本発明のＴｉ焼結
体の製造方法によれば、希土類酸化物を主成分（９０％
〜１００％）とした支持材を用いるので、支持材とＴｉ
との反応が抑えられ、焼結時の支持材へのくっつきや割
れの発生を防止することができる。希土類酸化物として
は、Ｙ2 Ｏ3 をあげることができるが、その他、Ｌａ2
Ｏ3 ，Ｃｅ2 Ｏ3 ，んｄ2 Ｏ3 ，Ｓｍ2 Ｏ3 などであっ
てもよい。いずれもＴｉとの活性が小さいことから同様
の作用効果が得られる。[Means for Solving the Problems, Actions and Effects] The method for producing a Ti sintered body of the present invention, which has been made in order to achieve such an object, comprises placing it on a support material containing 90% or more of a rare earth oxide. It is characterized by being sintered. According to the method for producing a Ti sintered body of the present invention, the rare earth oxide is the main component (90%).
~ 100%), the support material and Ti
The reaction with the can be suppressed, and the occurrence of sticking or cracking to the support material during sintering can be prevented. Examples of the rare earth oxide, may be mentioned Y 2 O 3, other, La 2
It may be O 3 , Ce 2 O 3 , d 2 O 3 , Sm 2 O 3 or the like. Since both of them have a small activity with Ti, the same effect can be obtained.
【０００７】ここで、希土類酸化物以外の成分として
は、ＺｒＯ2 、ＣａＯ、ＭｇＯといったＴｉとの反応が
比較的起こりにくいものに限ることが望ましい。また、
これらは合計で１０％未満に抑える必要がある。ＺｒＯ
2 、ＣａＯ、ＭｇＯに限るのは、それ以外のＡｌ2 Ｏ3
やＳｉＯ2 などでは、Ｔｉとの活性が高く、少し混ざっ
ているだけでも焼結時に反応が起こるおそれが高いから
である。[0007] As the components other than rare earth oxide, ZrO 2, CaO, it is desirable that the reaction between Ti such MgO is limited to those relatively unlikely. Also,
These must be suppressed to less than 10% in total. ZrO
2 , CaO and MgO are limited to other Al 2 O 3
This is because, for example, SiO 2 and SiO 2 have a high activity with Ti, and even if they are mixed in a small amount, a reaction is likely to occur during sintering.
【０００８】また、前記支持材としては粉末層を用いる
ことができるが、トレイを用いるときには、その気孔率
が１０％以上あることが望ましい。これは、気孔率が少
ないと、脱脂中にバインダーの分解ガスが放出されず、
製品に割れや膨れが生ずることや、あるいはトレイとの
接触面のＣが高くなり製品の靱性を損なうからである。
粉末の場合には、そもそも粉末間に隙間があるのでこう
した問題はない。Although a powder layer can be used as the support material, it is desirable that the porosity is 10% or more when using a tray. This is because if the porosity is low, the decomposition gas of the binder is not released during degreasing,
This is because the product is cracked or swelled, or the C of the contact surface with the tray is increased and the toughness of the product is impaired.
In the case of powder, since there is a gap between powders in the first place, there is no such problem.
【０００９】一方、本発明のＴｉ焼結体製造用の焼結時
支持材は、希土類酸化物が９０％以上であり、ＺｒＯ
2 、ＣａＯ、ＭｇＯの中から選ばれた１種又は２種以上
の酸化物が合計で１０％未満とされたものである。この
焼結時支持材は、トレイ又は粉末層として使用される。
トレイとして使用されるときには気孔率が１０％以上必
要である。この焼結時支持材によれば、その主成分がＴ
ｉとの活性の低い元素であるので、焼結の際にＴｉと支
持材とが反応してしまうことがなく、支持材へのくっつ
きや焼結体の割れが発生するのを防止できる。On the other hand, the sintering supporting material for producing the Ti sintered body of the present invention contains 90% or more of rare earth oxides and ZrO 2.
2 , one or two or more kinds of oxides selected from CaO and MgO are contained in less than 10% in total. During this sintering, the support material is used as a tray or powder layer.
When used as a tray, the porosity must be 10% or more. According to this supporting material at the time of sintering, the main component is T
Since it is an element having low activity with i, Ti and the support material do not react with each other during sintering, and it is possible to prevent sticking to the support material and cracking of the sintered body.
【００１０】[0010]
【実施例】次に、本発明を一層明らかにするために、好
適な実施例を比較例と比べながら説明する。実施例とし
ては、不可避的不純物を含有し、特に、Ｏ含有量が０．
１５ｗｔ％で残部がＴｉの純Ｔｉ粉末（平均粒径３１．
９μｍ、以下大径粉という）と、同じく、不可避的不純
物を含有し、特に、Ｏ含有量が０．３１ｗｔ％で残部が
Ｔｉの純Ｔｉ粉末（平均粒径１５．２μｍ、以下小径粉
という）とを、７０：３０の重量比で混合し、バインダ
ーを加えて混練し、ＭＩＭ用射出成形機にて引張試験片
を成形し、脱脂後、焼結をした。詳細については以下の
通りである。 （１）最初の混合には、Ｖブレンダーを使用した。 （２）バインダーとしては、ポリオレフィンにワックス
を４０：６０の重量比で混合したものを用いた。なお、
バインダー量は、Ｔｉ粉末に対して１１．５ｗｔ％とし
た。 （３）射出成形は、１５０〜１７０℃に加熱した状態で
実行した。 （４）引張試験片は、図１に示すように、全長１１０mm
×厚さ４mmで、チャック部の幅が１２mm、本体部の幅が
７．５mmの板状のものとした。 （５）脱脂としては、まず有機溶剤にてＭＩＭ成形体中
のバインダーの一部を除去した後、下記表１に示すよう
な支持材上に成形体を載置し、４３０℃に加熱して１時
間保持を行った。 （６）焼結についても、下記表１に示すような支持材上
に成形体を載置し、まず、真空中で室温から１２００℃
まで昇温し、その後Ａｒ雰囲気中（圧力５Torr）で１３
００℃に１時間保持して最終焼結をした。EXAMPLES In order to further clarify the present invention, preferred examples will be described in comparison with comparative examples. Examples include unavoidable impurities, and particularly, the O content is 0.
Pure Ti powder (average particle size 31.
9 μm, hereinafter referred to as large-diameter powder) as well as unavoidable impurities, in particular, pure Ti powder having an O content of 0.31 wt% and the balance of Ti (average particle size 15.2 μm, hereinafter referred to as small-diameter powder) Were mixed at a weight ratio of 70:30, a binder was added and kneaded, and a tensile test piece was molded by an injection molding machine for MIM, degreased, and then sintered. Details are as follows. (1) A V blender was used for the initial mixing. (2) As the binder, a mixture of polyolefin and wax in a weight ratio of 40:60 was used. In addition,
The binder amount was 11.5 wt% with respect to the Ti powder. (3) The injection molding was performed in a state of being heated to 150 to 170 ° C. (4) As shown in Fig. 1, the tensile test piece has a total length of 110 mm.
The plate-shaped product had a thickness of 4 mm, a chuck width of 12 mm, and a main body width of 7.5 mm. (5) For degreasing, first, a part of the binder in the MIM molded product was removed with an organic solvent, and then the molded product was placed on a support material as shown in Table 1 below and heated to 430 ° C. Hold for 1 hour. (6) Also for sintering, the molded body is placed on a supporting material as shown in Table 1 below, and first, in vacuum, from room temperature to 1200 ° C.
Up to 13 and then in Ar atmosphere (pressure 5 Torr) for 13
The final sintering was performed by holding at 00 ° C for 1 hour.
【００１１】以上の処理の結果得られた引張試験片の、
外観及び伸びを調べた結果を表１に併せて記載する。The tensile test piece obtained as a result of the above treatment,
The results of examining the appearance and elongation are also shown in Table 1.
【００１２】[0012]
【表１】 [Table 1]
【００１３】表１から分かる様に、Ｎｏ．１〜６は、い
ずれも伸びが１５％以上あり、焼結体に十分な延性が備
わっていることが分かる。また、Ｎｏ．１〜３は外観も
全く問題がなく、Ｎｏ．４〜６も若干の変色があるもの
の外観上の問題はないといえる。As can be seen from Table 1, No. It is understood that all of Nos. 1 to 6 have an elongation of 15% or more, and the sintered body has sufficient ductility. In addition, No. Nos. 1 to 3 have no problem in appearance and No. Nos. 4 to 6 also have some discoloration, but it can be said that there is no problem in appearance.
【００１４】一方、Ｎｏ．７を見ると、支持材の材質は
Ｙ2 Ｏ3 であるものの、気孔率が３．１％しかないトレ
イであるので、焼結中のバインダーの逃げが不十分とな
り、外観的には膨れが生じた。また、伸びも２．１％し
かなかった。また、Ｎｏ．８〜１９は、いずれも伸びが
１０％未満であり、Ｎｏ．１２，１３は特にトレイと焼
結体が反応してくっついてしまった。また、Ｎｏ．８，
１８，１９では焼結体にクラックが生じた。なお、クラ
ックが生じるということは、トレイとＴｉとが反応をす
ることにより抵抗が生じ、焼結時の熱歪によって割れが
生じたと考えることができる。また、粉付着も反応の一
つである。On the other hand, No. Looking at No. 7, although the support material is Y 2 O 3, it is a tray with a porosity of only 3.1%, so the escape of the binder during sintering becomes insufficient and swelling in appearance. occured. In addition, the growth was only 2.1%. In addition, No. Nos. 8 to 19 are all less than 10% in elongation, and No. Particularly in Nos. 12 and 13, the tray and the sintered body reacted with each other and stuck to each other. In addition, No. 8,
In Nos. 18 and 19, cracks occurred in the sintered body. The occurrence of cracks can be considered to be that resistance occurs due to the reaction between the tray and Ti, and cracks occur due to thermal strain during sintering. Further, powder adhesion is one of the reactions.
【００１５】これらのことから、支持材としてはＹ2 Ｏ
3 を９０％以上含有するものを用いなければ十分な延性
を有するＴｉ焼結体が得られないということが分かる。
また、支持材がトレイである場合にはＹ2 Ｏ3 を９０％
以上含有するという条件だけでなく、気孔率についても
１０％以上とする必要があるということが分かる。From the above, Y 2 O is used as the support material.
It can be seen that a Ti sintered body having sufficient ductility cannot be obtained unless a material containing 90% or more of 3 is used.
If the supporting material is a tray, 90% of Y 2 O 3 is added.
It can be seen that not only the condition of containing the above, but also the porosity needs to be 10% or more.
【００１６】以上本発明の実施例を説明したが、本発明
はこれら実施例に限定されるものではなく、その要旨を
逸脱しない範囲内で種々なる態様にて実現することがで
きることはいうまでもない。例えば、射出成形前に混練
するバインダーとしては、ポリプロピレンの他に、ポリ
オレフィン、ポリエチレン、ポリスチレンなどの各種熱
可塑性樹脂を用いることができるし、ワックスの他に、
パラフィン、カルナバなどを用いることもできる。Although the embodiments of the present invention have been described above, it is needless to say that the present invention is not limited to these embodiments and can be implemented in various modes without departing from the scope of the invention. Absent. For example, as the binder to be kneaded before injection molding, in addition to polypropylene, various thermoplastic resins such as polyolefin, polyethylene and polystyrene can be used, and in addition to wax,
Paraffin, carnauba, etc. can also be used.
【００１７】また、ＭＩＭに限らず、Ｔｉ粉末を圧粉成
形した成形体を焼結する場合に本発明を適用できること
はもちろんである。Of course, the present invention can be applied not only to MIM but also to the sintering of a compact obtained by compacting Ti powder.
【図１】 実施例で製造した試験片の平面図である。FIG. 1 is a plan view of a test piece manufactured in an example.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成６年８月２３日[Submission date] August 23, 1994
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００６[Correction target item name] 0006
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【０００６】[0006]
【課題を解決するための手段、作用及び効果】かかる目
的を達成するためになされた本発明のＴｉ焼結体の製造
方法は、希土類酸化物を９０％以上含有する支持材上に
載置して焼結することを特徴とする。本発明のＴｉ焼結
体の製造方法によれば、希土類酸化物を主成分（９０％
〜１００％）とした支持材を用いるので、支持材とＴｉ
との反応が抑えられ、焼結時の支持材へのくっつきや割
れの発生を防止することができる。希土類酸化物として
は、Ｙ2 Ｏ3 をあげることができるが、その他、Ｌａ2
Ｏ3 ，Ｃｅ2 Ｏ3 ，Ｎｄ2 Ｏ3 ，Ｓｍ2 Ｏ3 などであっ
てもよい。いずれもＴｉとの活性が小さいことから同様
の作用効果が得られる。[Means for Solving the Problems, Actions and Effects] The method for producing a Ti sintered body of the present invention, which has been made in order to achieve such an object, comprises placing it on a support material containing 90% or more of a rare earth oxide. It is characterized by being sintered. According to the method for producing a Ti sintered body of the present invention, the rare earth oxide is the main component (90%).
~ 100%), the support material and Ti
The reaction with the can be suppressed, and the occurrence of sticking or cracking to the support material during sintering can be prevented. Examples of the rare earth oxide, may be mentioned Y 2 O 3, other, La 2
It may be O 3 , Ce 2 O 3 , Nd 2 O 3 , Sm 2 O 3 or the like. Since both of them have a small activity with Ti, the same effect can be obtained.
Claims (5)
材上に載置して焼結することを特徴とするＴｉ焼結体の
製造方法。1. A method for producing a Ti sintered body, which comprises placing it on a support material containing 90% or more of a rare earth oxide and sintering it.
ａＯ、ＭｇＯの中から選ばれた１種又は２種以上の酸化
物であることを特徴とする請求項１記載のＴｉ焼結体の
製造方法。2. A component other than the rare earth oxide is ZrO 2 , C.
The method for producing a Ti sintered body according to claim 1, wherein the oxide is one or more oxides selected from aO and MgO.
であることを特徴とする請求項１又は請求項２記載のＴ
ｉ焼結体の製造方法。3. The T according to claim 1, wherein the support material is a tray having a porosity of 10% or more.
i A method for manufacturing a sintered body.
する請求項１又は請求項２記載のＴｉ焼結体の製造方
法。4. The method for producing a Ti sintered body according to claim 1, wherein the support material is a powder layer.
Ｏ2 、ＣａＯ、ＭｇＯの中から選ばれた１種又は２種以
上の酸化物が合計で１０％未満とされたＴｉ焼結体製造
用の焼結時支持材。5. The rare earth oxide is 90% or more, Zr
A supporting material at the time of sintering for producing a Ti sintered body in which the total amount of one or more oxides selected from O 2 , CaO and MgO is less than 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19324994A JPH0860270A (en) | 1994-08-17 | 1994-08-17 | Production of ti sintered compact and supporting material at the time of sintering therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19324994A JPH0860270A (en) | 1994-08-17 | 1994-08-17 | Production of ti sintered compact and supporting material at the time of sintering therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0860270A true JPH0860270A (en) | 1996-03-05 |
Family
ID=16304818
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19324994A Pending JPH0860270A (en) | 1994-08-17 | 1994-08-17 | Production of ti sintered compact and supporting material at the time of sintering therefor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0860270A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004332012A (en) * | 2003-05-01 | 2004-11-25 | Shin Etsu Chem Co Ltd | Heat-resistant holder and heat-treating/sintering method |
-
1994
- 1994-08-17 JP JP19324994A patent/JPH0860270A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004332012A (en) * | 2003-05-01 | 2004-11-25 | Shin Etsu Chem Co Ltd | Heat-resistant holder and heat-treating/sintering method |
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