JPH01301801A - Production of ti-al intermetallic compound powder - Google Patents
Production of ti-al intermetallic compound powderInfo
- Publication number
- JPH01301801A JPH01301801A JP63133124A JP13312488A JPH01301801A JP H01301801 A JPH01301801 A JP H01301801A JP 63133124 A JP63133124 A JP 63133124A JP 13312488 A JP13312488 A JP 13312488A JP H01301801 A JPH01301801 A JP H01301801A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- mixture
- intermetallic compound
- temp
- less
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 82
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 229910021362 Ti-Al intermetallic compound Inorganic materials 0.000 title claims 2
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000010298 pulverizing process Methods 0.000 claims abstract description 14
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 35
- 229910004349 Ti-Al Inorganic materials 0.000 abstract description 14
- 229910004692 Ti—Al Inorganic materials 0.000 abstract description 14
- 229910052748 manganese Inorganic materials 0.000 abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 6
- 229910052796 boron Inorganic materials 0.000 abstract description 5
- 229910052759 nickel Inorganic materials 0.000 abstract description 5
- 229910052758 niobium Inorganic materials 0.000 abstract description 5
- 229910052721 tungsten Inorganic materials 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 229910052720 vanadium Inorganic materials 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract 1
- 229910000765 intermetallic Inorganic materials 0.000 description 24
- 239000010936 titanium Substances 0.000 description 23
- 239000002245 particle Substances 0.000 description 15
- 238000000280 densification Methods 0.000 description 14
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 14
- 239000010931 gold Substances 0.000 description 14
- 229910052737 gold Inorganic materials 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000005266 casting Methods 0.000 description 6
- 238000011109 contamination Methods 0.000 description 6
- 238000007872 degassing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005275 alloying Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009689 gas atomisation Methods 0.000 description 2
- -1 gold metal compound Chemical class 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000979 O alloy Inorganic materials 0.000 description 1
- 102100034742 Rotatin Human genes 0.000 description 1
- 101710200213 Rotatin Proteins 0.000 description 1
- 229910021330 Ti3Al Inorganic materials 0.000 description 1
- 229910010038 TiAl Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940125904 compound 1 Drugs 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、射出成形等による粉末焼結体の製造に供され
るＴｉ−Ａｌ系金金属間化合物粉末製造方法に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing a Ti-Al based gold intermetallic compound powder that is used for producing a powder sintered body by injection molding or the like.
［従来の技術］
従来、Ｔｉ−Ａｌ系金金属間化合物 １’ ｉ Ａ Ｑ
、Ｔ ｌ ３Ａ Ｑ等）は、優れた高温強度及び耐酸化
性を有することが知られている。しかし、この部材は、
常温および高温で展延性に乏しいので、従来の加工技術
では成形することが困難であり、実用材料に供すること
ができないという問題点があった。[Prior art] Conventionally, Ti-Al based gold intermetallic compound 1' i A Q
, T 1 3A Q, etc.) are known to have excellent high temperature strength and oxidation resistance. However, this member
Since it has poor malleability at room temperature and high temperature, it is difficult to mold using conventional processing techniques, and there is a problem in that it cannot be used as a practical material.
これを解決する手段として、たとえば、Ｔｉ −３７％
（以下、％は重量％を示す。）へ〇合金部材を側圧付加
押出法等の特別な押出加工方法により実現しようとする
試みがなされているが、実用化に至っていない。As a means to solve this problem, for example, Ti -37%
(Hereinafter, % indicates weight %.) Attempts have been made to produce alloy members using special extrusion processing methods such as lateral pressure extrusion methods, but they have not been put to practical use.
また、このようなＴｉ−Ａｌ系金金属間化合物部材製造
方法の１つとして、Ｔｉ−Ａ（１！系金金属化合物の粉
末を用いて射出成形から焼成工程を経ることにより焼結
体を製造する方法があり、ＮｅａｒＮｅｔ ５ｈａｐｅ
が可能であることから、とくに注目されている。In addition, as one of the methods for manufacturing such Ti-Al based gold intermetallic compound members, a sintered body is manufactured by using powder of Ti-A (1! based gold metal compound) through injection molding and firing steps. There is a way to do this, NearNet 5hape
It is attracting particular attention because it is possible.
この製造方法に使用されるＴｉ−Ａｌ系金金属間化合物
粉末を製造するのに、Ｔｉ−Ａｌの鋳造により鋳塊を製
造し、これを粉砕する方法を採った場合には、Ｔｉを含
有しているために鋳造時の汚染で純粋な組成の粉末を製
造することが困難であり、また汚染を防止するためには
高価な錆造設備を要するという問題がある。In order to produce the Ti-Al based gold intermetallic compound powder used in this production method, if a method is adopted in which an ingot is produced by casting Ti-Al and the ingot is pulverized, Ti-based gold intermetallic compound powder is produced. Because of this, it is difficult to produce powder with a pure composition due to contamination during casting, and expensive rust forming equipment is required to prevent contamination.
また、他の粉末製造方法として、ＲＥＰ法（Ｒ。In addition, as another powder manufacturing method, REP method (R.
ｔａｔｉｎｇ Ｅｌｅｃｔｒｏｄｅ Ｐｒｏｃｅｓｓ）
あるいはＰＲＥＰ？去（Ｐｌａｓｍａ Ｒｏｔａｔｉｎ
ｇ Ｅｌｅｃｔｒｏｄｅ Ｐｒｏｃｅｓｓ）等がある０
この方法は、ＴｉとｋＱ’ｊｉ：？ｉＪ解・鋳造し、切
削加工することにより丸棒の電極部材を製造し、この電
極部材を回転させながらアークにより溶融することによ
り粉末を形成するものである。tating Electrode Process)
Or PREP? Plasma Rotatin
g Electrode Process) etc.0
This method uses Ti and kQ'ji:? A round bar electrode member is manufactured by iJ melting, casting, and cutting, and powder is formed by melting the electrode member with an arc while rotating the electrode member.
しかし、この方法でも電極を製造するのに鋳造を用いて
いるために、汚染をさけることができず、鋳造設備等が
大型化したり、また、ＲＥＰ法等の高価な設備を必要と
するほか工程が長くなるとともに、原料の歩留りが悪く
、得られた粉末が著しく高価になるという問題もあった
。However, since this method also uses casting to manufacture the electrodes, contamination cannot be avoided, the casting equipment becomes larger, and expensive equipment such as the REP method is required. There was also the problem that as the time became longer, the yield of raw materials was poor and the resulting powder became extremely expensive.
［発明が解決しようとする課題］
本発明は、上記従来の技術の問題を解決することを課題
とし、高品質でかつ経済的なＴｉ−Ａｌ系金金属間化合
物粉末製造する方法を提供することを目的とする。[Problems to be Solved by the Invention] An object of the present invention is to solve the above-mentioned problems of the conventional technology, and to provide a high-quality and economical method for producing Ti-Al based gold intermetallic compound powder. With the goal.
［課題を解決するための手段］
上記課題を達成するためになされた本発明のＴｉ−Ａ（
２系金属間化合物粉末の製造方法は５、ｌ！１４重量％
重量％型６３重量％Ｔｉの割合になるように、Ａｌ粗粉
末またはＴｉ粉末、またはこれらの合金粉末を混合し、
この混合物の全部または一部を５５０℃以上で該混合物
の固相線以下の温度で加熱焼成し、この焼成物を粉砕す
ることを特徴とする。[Means for Solving the Problems] The Ti-A (
The manufacturing method of the binary intermetallic compound powder is 5.l! 14% by weight
Coarse Al powder, Ti powder, or alloy powder thereof are mixed so that the proportion of Ti is 63% by weight,
The method is characterized in that all or part of this mixture is heated and calcined at a temperature of 550°C or higher and lower than the solidus line of the mixture, and the calcined product is pulverized.
以下、本発明によるＴｉ−Ａｌ系金金属間化合物粉末製
造するための各工程について第１図に基づいて詳細に説
明し、さらにこれに他の工程を付加することにより一層
優れた粉末を製造できる方法について第２図を用いて説
明する。Hereinafter, each process for producing Ti-Al based gold intermetallic compound powder according to the present invention will be explained in detail based on FIG. 1, and by adding other processes to this, even more excellent powder can be produced. The method will be explained using FIG. 2.
（Ｔｉ粉末またはＴｉ合金粉末の製造工程Ｉ）これらの
粉末には、常法の粉末冶金法により製造されたものを用
いることができ、例えは、スポンジチタン、（ＮａＣＱ
またはＭ ｇ ＣＱ ２を２０００ｐｐｍ以内含有して
いる。）、ガスアトマイズ法、ＰＲＥＰ法、ＲＥＰ法等
で製造されたもの、錆塊、板、棒等を切削したものを用
いることができ、その粒度を５０００１Ｌｍ以下に調製
する。また、Ｔｉを他の元素との冶金粉末として加える
場合には、Ｔｉを主成分として、必要に応じてＡｌ、Ｂ
、Ｚ「、Ｎ ｉ、 Ｎｂ、 Ｍｎ、 Ｓ ｉ、 ｖ、
Ｗ、 Ｍｏのうち１種以上を後述する割合となるように
添加する。(Manufacturing process I of Ti powder or Ti alloy powder) For these powders, those manufactured by the conventional powder metallurgy method can be used. For example, sponge titanium, (NaCQ
Or it contains M g CQ 2 within 2000 ppm. ), gas atomization method, PREP method, REP method, etc., or cut rust lumps, plates, rods, etc. can be used, and the particle size is adjusted to 50001 Lm or less. In addition, when adding Ti as a metallurgical powder with other elements, Ti is the main component, and if necessary Al, B
, Z ", N i, Nb, Mn, S i, v,
One or more of W and Mo are added in the proportions described below.
（Ａｌ粗粉末たはＡｌＱ金粉末の製造工程■）Ａｌ粗粉
末、常法の粉末製造方法、例えは、ガスアトマイズ法、
ＰＲＥＰ法、ＲＥＰ法等で製造されたものを用いること
ができ、その粒度を５０００μｍ以下に調製する。(Manufacturing process of Al coarse powder or AlQ gold powder ■) Al coarse powder, conventional powder manufacturing method, for example, gas atomization method,
Those manufactured by PREP method, REP method, etc. can be used, and the particle size is adjusted to 5000 μm or less.
また、八〇を他の元素との合金粉末として加える場合に
は゛、八〇を主成分として、必要に応じてＴｉ５Ｂ、
Ｚｒ５Ｎｉ、 Ｎｂ、 Ｍｎ、 Ｓｉ、 Ｖ、
Ｗ、Ｍｏのうち、１種以上を後述する割合となるように
添加する。In addition, when adding 80 as an alloy powder with other elements, use 80 as the main component and optionally add Ti5B,
Zr5Ni, Nb, Mn, Si, V,
One or more of W and Mo are added in the proportions described below.
（混合工程■）
次に、Ａｌ２１４％〜６３％、残部Ｔｉの割合になるよ
うにＴｉｍ末またはＴｉ合金粉末、Ａ Ｑ ｙＪ末また
はＡｌＱ金粉末を適宜選択して、Ｖ型混合機等で均一に
混合する。(Mixing process ■) Next, appropriately select Tim powder or Ti alloy powder, AQ yJ powder or AlQ gold powder so that the proportion of Al2 is 14% to 63% and the balance is Ti, and mix uniformly with a V-type mixer etc. Mix with
上記のような混合割合にするのは、Ａｌが１４％〜６３
％の範囲外では、Ｔｉ３Ａｌ、Ｔ ｉＡｌ、およびＴｉ
ＡＬ系の金属間化合物の単相あるいは２相とならないか
らである。The above mixing ratio is achieved when Al is 14% to 63%.
%, Ti3Al, TiAl, and Ti
This is because the AL-based intermetallic compound does not form a single phase or two phases.
また、ＴｉおよびＡｌ以外の添加元素の割合は、０．０
０５％≦Ｂ≦３％、 １％≦Ｚｒ≦５％０．１％≦Ｎ
１≦５％、 １％≦Ｎｂ≦３０％０．１％≦Ｍｎ≦
５％、
０．０５％≦Ｓｉ≦５％ １％≦Ｖ≦５％０．１％≦
Ｗ≦１０％ １％≦Ｍｏ≦５％となるように調整す
る。Furthermore, the proportion of additive elements other than Ti and Al is 0.0
05%≦B≦3%, 1%≦Zr≦5%0.1%≦N
1≦5%, 1%≦Nb≦30% 0.1%≦Mn≦
5%, 0.05%≦Si≦5% 1%≦V≦5%0.1%≦
Adjust so that W≦10% and 1%≦Mo≦5%.
ここで、Ｂ、 Ｚｒ、 Ｎ ｉ、 Ｎｂ、 Ｍｎ
、 Ｖ、Ｍｏの元素を上記範囲とするのは、該範囲内
において常温あるいは高温における延性の改良効果が得
られ、すなわち、下限値未満では、延性の改良の効果が
得られず、また、上限値を超えると延性の改良が飽和す
るからである。Here, B, Zr, Ni, Nb, Mn
The reason why the elements of , V, and Mo are set in the above range is that the effect of improving ductility at room temperature or high temperature is obtained within the range, that is, the effect of improving ductility cannot be obtained below the lower limit, and This is because if the value is exceeded, the improvement in ductility will be saturated.
また、Ｗ、 Ｓ ｉ、 Ｎ ｂ、 Ｍｏの成分範囲
を上記の範囲とするのは、該範囲内において耐酸化性を
向上させることができ、すなわち、下限値未満では耐酸
化性の向上がみられず、また、上限値を超えると、耐酸
化性が飽和するからである。Furthermore, the reason why the component ranges of W, Si, Nb, and Mo are set to the above ranges is that the oxidation resistance can be improved within the ranges, that is, the oxidation resistance cannot be improved below the lower limit. Moreover, if the upper limit is exceeded, the oxidation resistance will be saturated.
（Ｄ処理■）
次に、混合工程■により所定の割合で調整された混合物
の全体または一部を５５０℃以上で固相線以下の温度で
加熱することにより、Ｔｉと八〇の合金化反応を生じさ
せ、Ｔｉ−Ａｌ系金金属間化合物形成する。この反応は
、発熱反応であるために、その温度が１５００℃近くま
でなることがある。この反応は数分間で終了し、その後
、処理物の温度は雰囲気温度まで低下する。このときの
雰囲気は、真空中または不活性ガス（Ｈｅ、Ａｒ等）中
とする。なお、Ｍｇ、 Ｎ ａ、 ＣＱ等を含んだスポ
ンジＴｉを使用した場合、真空においては、反応開始と
同時にこれらの物質が気化し、雰囲気の圧力が上昇する
が、反応終了とともにすみやかに元の真空に戻り、焼結
体への汚染を低減できる。(D treatment ■) Next, by heating the whole or part of the mixture adjusted at a predetermined ratio in the mixing step ■ at a temperature of 550°C or more and below the solidus line, an alloying reaction of Ti and 80 is carried out. to form a Ti-Al based gold intermetallic compound. Since this reaction is exothermic, the temperature may reach nearly 1500°C. This reaction is completed in a few minutes, after which the temperature of the treated material is lowered to ambient temperature. The atmosphere at this time is a vacuum or an inert gas (He, Ar, etc.). Note that when Ti sponge containing Mg, Na, CQ, etc. is used in a vacuum, these substances vaporize as soon as the reaction starts, and the pressure of the atmosphere rises, but as soon as the reaction ends, it returns to the original vacuum. The contamination of the sintered body can be reduced.
さらに、熱処理■により、焼結体が多孔質になることが
あり、この場合、次工程Ｖでの粉砕が容易となる。Furthermore, the heat treatment (1) may cause the sintered body to become porous, and in this case, pulverization in the next step (V) becomes easier.
（粉砕工程Ｖ） 続く工程では、焼成体を所定の粒径に粉砕する。(Crushing process V) In the subsequent step, the fired body is pulverized to a predetermined particle size.
粉砕の手法としては、通常の粉砕法、例えは、ボールミ
ル等の機械的な粉砕機を用いたり、気流粉砕法を適用す
ることができる。As the pulverization method, a conventional pulverization method, for example, a mechanical pulverizer such as a ball mill, or a pneumatic pulverization method can be applied.
ここで、好適な粉砕法としては、例えは、ボールミル等
を使用して粒径を１００μｍ程度に粗粉砕し、その後、
気流粉砕法を用いて粉砕し数μｍの粉末を得るものが適
用できる。このように気流粉砕法では、粉末が球状とな
り、さらに不活性ガス中で粉砕することにより、他の粉
砕法に比べて、粉末への汚染が少なく、例えば、射出焼
結用微粉末の製造に適している。Here, as a suitable pulverization method, for example, use a ball mill etc. to coarsely pulverize the particle size to about 100 μm, and then
It is possible to use a method that obtains a powder of several micrometers by pulverization using an air flow pulverization method. In this way, in the air flow pulverization method, the powder becomes spherical, and by pulverizing it in an inert gas, there is less contamination of the powder compared to other pulverization methods, and it is suitable for producing fine powder for injection sintering, for example. Are suitable.
本発明の主たる工程は以上であるが、必要に応じて、第
２図に示す処理を加えてもよい。The main steps of the present invention have been described above, but the processing shown in FIG. 2 may be added if necessary.
（他の金属、合金の粉末製造工程■）
Ｔｉ−Ａｌ系金金属間化合物部材有効な添加元素、たと
えば、延性改良に効果のあるＢ、Ｚｒ、Ｎ ｉ、 Ｎ
ｂ、 Ｍｎ、 Ｖ、 Ｍｏ、または耐酸化性に効果が
あるＷ、Ｓｉは、上述した工程Ｉ、■ではＴｉ合金また
はへ〇合金として所定の混合割合になるように添加した
が、これに限らず、これらの単体金属粉、合金粉または
Ｔｉ５０％以下またはＡｌ５０％以下を含む合金粉とし
て上記Ａ（２粉末およびＴｉ粉末等と混合してもよい。(Powder production process for other metals and alloys ■) Effective additive elements for Ti-Al based gold intermetallic compound members, such as B, Zr, Ni, N, which are effective in improving ductility
b, Mn, V, Mo, or W and Si, which are effective in oxidation resistance, were added at a predetermined mixing ratio as a Ti alloy or a 〇 alloy in the above-mentioned steps I and ①, but they are not limited to this. First, these single metal powders, alloy powders, or alloy powders containing 50% or less of Ti or 50% or less of Al may be mixed with the above A(2 powder, Ti powder, etc.).
（脱気工程■）
上記混合工程■に続いて脱気工程■および後述する緻密
化処理■を行うことにより、Ｔｉ粉末やへ〇粉末等め原
料粉末として粗粒（２００ｕｍ以上）のものを用いるこ
とができる。(Degassing process ■) Following the above mixing process ■, a degassing process ■ and a densification process ■ described below are performed to use coarse grains (200 um or more) as the raw material powder such as Ti powder or He〇 powder. be able to.
まず、脱気工程■では、混合物を容器に収納して真空ポ
ンプ等により脱気処理を行う。これは、粉末表面の吸着
ガス、吸着水を除去するとともに、後の厳密化処理■等
における酸化を防止するためである。この脱気処理■は
、粉末の酸化を防止するために真空度１０Ｔｏｒｒ以下
で行うことが好ましい。また、脱気処理は、常温〜５５
０℃、さらに望ましくは、４００℃〜５００℃で行うと
、吸着ガス・吸着水の除去が容易となり好ましい。なお
、５５０℃を越える場合には、ＴｉとＡｌとの合金化反
応が生じるので好ましくない。First, in the degassing step (2), the mixture is placed in a container and degassed using a vacuum pump or the like. This is to remove adsorbed gas and adsorbed water on the powder surface, as well as to prevent oxidation in subsequent strict processing (2), etc. This degassing treatment (1) is preferably carried out at a vacuum level of 10 Torr or less in order to prevent oxidation of the powder. In addition, deaeration treatment is performed at room temperature to 55%
It is preferable to carry out the reaction at 0° C., more preferably at 400° C. to 500° C., because it facilitates the removal of adsorbed gas and water. Note that if the temperature exceeds 550°C, an alloying reaction between Ti and Al will occur, which is not preferable.
（ｍ密化処理■）
次に、脱気後の混合物をホットプレス、押出、ＣＩ Ｐ
（Ｃｏｌｄ １ｓｏｓｔａｔｉｃ Ｐｒｅｓｓ）また
はＨＩＰ（Ｈｏｔ １ｓｏｓｔａｔｉｃ Ｐｒｅｓｓ）
等で相対密度で９５％以上になるように圧縮し、粉末圧
縮体とする。ここで、相対密度とは、混合物の密度を完
全に緻密化した場合の密度に対する割合を％として表示
したものである。(m-densification treatment■) Next, the degassed mixture is subjected to hot pressing, extrusion, and CI P.
(Cold 1sostatic Press) or HIP (Hot 1sostatic Press)
etc. to obtain a powder compact with a relative density of 95% or more. Here, the relative density is expressed as a percentage of the density of the mixture when it is completely densified.
この緻密化処理■は、後に行われる上述した熱処理■に
おいて合金化反応をより容易にするために行われるもの
である。本緻密化処理■は、この段階でのＴｉとＡｌと
の合金化反応を防止するために５５０℃以下で行う必要
がある。よって、水撒密化処理■後の緻密体には、未だ
Ｔｉ−Ａｌ系金金属間化合物形成されていない。This densification treatment (2) is carried out in order to facilitate the alloying reaction in the above-mentioned heat treatment (2) which will be carried out later. This densification treatment (3) needs to be carried out at 550° C. or lower in order to prevent an alloying reaction between Ti and Al at this stage. Therefore, the Ti-Al based gold intermetallic compound has not yet been formed in the dense body after the water densification treatment (1).
なお、脱気工程■、および緻密化処理■は、真空ホット
プレスを用いて同時に行ってもよい。Note that the degassing step (1) and the densification treatment (2) may be performed simultaneously using a vacuum hot press.
緻密化処理■を加えることにより、粒径の太きい２００
μｍ以上の粉末を使用できるようになり、このため、粉
末の単位質量あたりの表面積が小さく、酸化物が少なく
なるので、その結果低酸素のＴｉ−Ａｌ２系金属間化合
物粉末を製造することができる。By adding densification treatment■, the particle size is increased to 200%.
It is now possible to use powder with a particle diameter of μm or more, which means that the surface area per unit mass of the powder is small and the amount of oxides is reduced, making it possible to produce a low-oxygen Ti-Al2 intermetallic compound powder. .
［実施例コ 以下、本発明の一実施例について説明する。[Example code] An embodiment of the present invention will be described below.
まず、第１表および第２表に示すような組成および処理
を経て焼結体を形成し、その焼結体を粉砕して粉末を製
造し、そしてこの粉末にＴｉ−Ａｌ系金金属間化合物形
成されているか否かについて判定を行った。First, a sintered body is formed through the composition and treatment shown in Tables 1 and 2, the sintered body is crushed to produce a powder, and a Ti-Al based gold intermetallic compound is added to this powder. A determination was made as to whether or not it was formed.
すなわち、Ｔｉ粉末、Ａｌ粗粉末たはそれらの合金粉末
の粒径を２００ａｍ以下、２９７μｍ以下、５００ａｍ
以下、１０００１１ｍ以下、５０００ｕｍ以下に調整し
たものを適宜選択し、混合し、ざらに緻密化処理■（ホ
ットプレス）の有無を絹み合わせ、５７０℃、１０””
Ｔｏｒｒ以下またはＡｒの雰囲気中にて熱処理を行い、
その後、機械的な粉砕等により粉末の製造を行った（試
料１〜試料９）。That is, the particle size of Ti powder, Al coarse powder, or their alloy powder is 200 am or less, 297 μm or less, or 500 am or less.
Below, those adjusted to 100,011 m or less and 5,000 um or less were appropriately selected, mixed, roughly densified (hot press) or not, and heated at 570°C for 10"
Heat treatment is performed in an atmosphere of less than Torr or Ar,
Thereafter, powders were manufactured by mechanical pulverization or the like (Samples 1 to 9).
その結果、第１表の試料１から試料３までは、Ｔｉ−Ａ
ｌ２系金属間化合物が形成され、試料４から試料５まで
は該化合物が形成されなかった。As a result, samples 1 to 3 in Table 1 are Ti-A
A 12-based intermetallic compound was formed, but this compound was not formed in samples 4 to 5.
このことから、２００ｕｍ以下の粒径のＴｉ粉末および
Ａ（２粉末を用いた場合には、緻密化処理■を行ねなく
ても、Ｔｉ−Ａ２系金属間化合物が形成されることが分
かる。なお、第３図に本粉末のＸ線回折結果を示す。From this, it can be seen that when Ti powder and A(2 powder) having a particle size of 200 um or less are used, a Ti-A2 intermetallic compound is formed even if the densification treatment (1) is not performed. Note that FIG. 3 shows the results of X-ray diffraction of this powder.
また、Ａｌ粗粉末粒径を１０００μｍ以下まで大きくし
た場合も、ホットプレスにより緻密化処理■を行った場
合には化合物が形成されたが（試料２）、緻密化処理を
行わなかったときには金属間化合物が形成されなかった
（試料４）。In addition, even when the Al coarse powder particle size was increased to 1000 μm or less, a compound was formed when densification treatment ■ was performed by hot pressing (sample 2), but when no densification treatment was performed, a compound was formed between metals. No compound was formed (Sample 4).
さらに、Ｔｉ粉末およびＡｌ扮粉末粒径を５０００μｍ
まで大きくした場合には、試料３と試料５から明らかな
ように、ホットプレスにより￥！！！密化処理■を行っ
た場合のみ金属間化合物が形成された。Furthermore, the particle size of Ti powder and Al powder was 5000 μm.
As is clear from Samples 3 and 5, when the size is increased to ¥! ! ! Intermetallic compounds were formed only when densification treatment (■) was performed.
したがって、緻密化処理■を加えることにより、粒径の
大きい（２００μｍ以上）粉末を原料としても金属間化
合物が一形成できる。粒径の大きい試料３を使用できる
ことにより、以下の効果がある。Therefore, by adding the densification treatment (1), an intermetallic compound can be formed even if a powder with a large particle size (200 μm or more) is used as a raw material. By being able to use the sample 3 with a large particle size, the following effects can be obtained.
すなわち、第３表において、試料１（ＴＩの粒径２００
μｍ以下）、試料３（同５０００μｍ以下）について熱
処理の前後の成分分析値を示す。同表から分かるように
、粒径の大きいもの（試料３）を使用すると、低酸素濃
度のＴｉ−ＡＣ系金属間化合物粉末が製造できることか
ら、この粉末を用いて焼成体を形成した場合には、展延
性の高いものを製造することができ、さらに、他の元素
（ＣＱ、Ｎａ等）も減らすことができるから強度も高め
ることができる。That is, in Table 3, sample 1 (TI particle size 200
(μm or less) and sample 3 (5000 μm or less) before and after heat treatment. As can be seen from the table, when a large particle size (sample 3) is used, a Ti-AC intermetallic compound powder with a low oxygen concentration can be produced, so when a fired body is formed using this powder, , it is possible to manufacture products with high malleability, and furthermore, since other elements (CQ, Na, etc.) can be reduced, strength can also be increased.
また、第３表から分かるように、熱処理■を真空雰囲気
で行うことにより不純物の低減効果もある。Furthermore, as can be seen from Table 3, performing heat treatment (1) in a vacuum atmosphere also has the effect of reducing impurities.
また、第２表に示す例は、ＴＩとＡｌの他にＭｎ、
Ｎ ｉ、 ＢをＡｌ合金粉末として添加し、さらに緻
密化処理の方法、熱処理条件や雰囲気を変えたものであ
る。同表から明らかなように、５００μｍ以下の粒径の
Ｔｉ粉末およびＡ Ｑ −Ｎ ｉ −８合金粉末を用い
た場合には、ｍ密化処理■による相対密度を９５％にし
た場合には、金属間化合物が形成されたが、ＣＩＰによ
り８５％程度の相対密度では金属間化合物が形成されな
かった。したがって、Ｍｎ、Ｎｉ等を添加した場合でも
同様に金属間化合物粉末製造が可能であり、しかも相対
密度を高めることにより粗粒の粉末を用いることができ
る。In addition, in the example shown in Table 2, in addition to TI and Al, Mn,
Ni and B were added as Al alloy powder, and the densification treatment method, heat treatment conditions, and atmosphere were changed. As is clear from the same table, when Ti powder and A Q -N i -8 alloy powder with a particle size of 500 μm or less are used, when the relative density is set to 95% by m-densification treatment (■), Although an intermetallic compound was formed, no intermetallic compound was formed at a relative density of about 85% by CIP. Therefore, even when Mn, Ni, etc. are added, it is possible to produce intermetallic compound powder in the same way, and by increasing the relative density, coarse-grained powder can be used.
［発明の効果コ
以上説明したように、本発明によれは、引出成形等を用
いた粉末冶金に適するＴｉ−Ａ（１！系金金属化合物粉
末を経済的に製造できる。[Effects of the Invention] As explained above, according to the present invention, it is possible to economically produce Ti-A (1! system gold metal compound powder) suitable for powder metallurgy using pultrusion molding or the like.
しかも、鋳造等を行わないので汚染が少なく、原料粉末
の純度と同等以上の純度のＴｉ−Ａｌ系金金属間化合物
粉末製造することができる。Moreover, since no casting or the like is performed, there is little contamination, and Ti-Al based gold intermetallic compound powder can be produced with a purity equal to or higher than that of the raw material powder.
第１図は本発明によるｌ’１−Ａｌ１！系金属間化合物
粉末を製造する過程を示す工程図、第２図は第１図の変
形例を示す工程図、第３図はＴ ｉ −Ａ Ｑ系金属間
化合物粉末のＸ線回折図である。
代理人 弁理士 定立 勉（ばか２名）第１図FIG. 1 shows l'1-Al1! according to the present invention. FIG. 2 is a process diagram showing a modification of FIG. 1, and FIG. 3 is an X-ray diffraction diagram of the Ti-AQ intermetallic compound powder. . Agent Patent Attorney Tsutomu Setate (2 idiots) Figure 1
Claims (1)
うに、Ａｌ粉末、またはＴｉ粉末、またはこれらの合金
粉末を混合し、この混合物の全部または一部を５５０℃
以上で該混合物の固相線以下の温度で加熱焼成し、この
焼成物を粉砕することを特徴とするＴｉ−Ａｌ系金属間
化合物粉末の製造方法。Al powder, Ti powder, or an alloy powder thereof is mixed so that the proportion of Al is 14% by weight to 63% by weight and the balance is Ti, and all or part of this mixture is heated at 550°C.
A method for producing a Ti-Al intermetallic compound powder, which comprises heating and firing the above mixture at a temperature below the solidus line, and pulverizing the fired product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63133124A JPH01301801A (en) | 1988-05-31 | 1988-05-31 | Production of ti-al intermetallic compound powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63133124A JPH01301801A (en) | 1988-05-31 | 1988-05-31 | Production of ti-al intermetallic compound powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01301801A true JPH01301801A (en) | 1989-12-06 |
Family
ID=15097350
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63133124A Pending JPH01301801A (en) | 1988-05-31 | 1988-05-31 | Production of ti-al intermetallic compound powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01301801A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH073355A (en) * | 1991-06-20 | 1995-01-06 | Natl Res Inst For Metals | Production of ti/al intermetallic compound |
| CN104439261A (en) * | 2014-12-25 | 2015-03-25 | 哈尔滨工程大学 | Preparation method for ultrapure Al3Ti intermetallic compound powder |
-
1988
- 1988-05-31 JP JP63133124A patent/JPH01301801A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH073355A (en) * | 1991-06-20 | 1995-01-06 | Natl Res Inst For Metals | Production of ti/al intermetallic compound |
| CN104439261A (en) * | 2014-12-25 | 2015-03-25 | 哈尔滨工程大学 | Preparation method for ultrapure Al3Ti intermetallic compound powder |
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