JPH073355A - Method for producing Ti / Al-based intermetallic compound - Google Patents
Method for producing Ti / Al-based intermetallic compoundInfo
- Publication number
- JPH073355A JPH073355A JP3174698A JP17469891A JPH073355A JP H073355 A JPH073355 A JP H073355A JP 3174698 A JP3174698 A JP 3174698A JP 17469891 A JP17469891 A JP 17469891A JP H073355 A JPH073355 A JP H073355A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- intermetallic compound
- titanium
- tial
- sintering
- 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
Links
- 229910000765 intermetallic Inorganic materials 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 51
- 239000010936 titanium Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 32
- 229910010038 TiAl Inorganic materials 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 22
- -1 titanium hydride Chemical compound 0.000 claims abstract description 18
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 14
- 239000000956 alloy Substances 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims description 9
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 5
- 230000006835 compression Effects 0.000 abstract description 5
- 238000007906 compression Methods 0.000 abstract description 5
- 150000002736 metal compounds Chemical class 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 22
- 239000011812 mixed powder Substances 0.000 description 16
- 230000000704 physical effect Effects 0.000 description 9
- 229910004349 Ti-Al Inorganic materials 0.000 description 8
- 229910004692 Ti—Al Inorganic materials 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000007796 conventional method Methods 0.000 description 7
- 238000001513 hot isostatic pressing Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000009924 canning Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 229910052735 hafnium Inorganic materials 0.000 description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910021362 Ti-Al intermetallic compound Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
(57)【要約】
【目的】高温圧縮を用いずに、通常の焼結技術により緻
密な焼結材を簡便かつ容易に製造し得る新しいＴｉ−Ａ
ｌ系金属化合物の製造方法を提供する。
【構成】金属間化合物ＴｉＡｌまたはＴｉ3 Ａｌ，ある
いはこれらの２相金属間化合物ＴｉＡｌ／Ｔｉ3 Ａｌの
製造に際し、チタン粉または水素化チタン粉と、チタン
を３０〜７０質量量％含有するアルミニウム母合金粉と
を、各々、所定の金属間化合物組成となるように混合
し、成形した後に焼結する。(57) [Abstract] [Purpose] A new Ti-A that can easily and easily produce a dense sintered material by ordinary sintering technology without using high temperature compression.
A method for producing an 1-based metal compound is provided. [Structure] In producing an intermetallic compound TiAl or Ti 3 Al, or a two-phase intermetallic compound TiAl / Ti 3 Al, an aluminum mother containing titanium powder or titanium hydride powder and 30 to 70 mass% of titanium. The alloy powder and the alloy powder are mixed so as to have a predetermined intermetallic compound composition, molded, and then sintered.
Description
【産業上の利用分野】この発明は、Ｔｉ−Ａｌ系金属間
化合物の製造方法に関するものである。さらに詳しく
は、この発明は、通常の焼結技術で簡便かつ容易に緻密
なＴｉ−Ａｌ系金属間化合物を製造することのできる新
しいＴｉ−Ａｌ系金属間化合物の製造方法に関するもの
である。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a Ti--Al intermetallic compound. More specifically, the present invention relates to a method for producing a new Ti-Al-based intermetallic compound capable of easily and easily producing a dense Ti-Al-based intermetallic compound by an ordinary sintering technique.
【従来の技術とその課題】従来より、Ｔｉ−Ａｌ系金属
間化合物については、一般的に、溶製法により製造して
きているが、金属や合金などに比べて展延性が劣るため
に、複雑形状部品や薄板などの製造には多くの問題があ
ることが指摘されている。そこで、このようなＴｉ−Ａ
ｌ金属間化合物の展延性についての欠点を改善し、その
加工性を向上すべく多くの研究がなされてきているが、
未だ充分な成果が得られていないのが実情である。一般
に、複雑形状部品や薄板などの製造には、焼結法が有利
であることが知られていることから、最近、焼結法によ
りこのＴｉ−Ａｌ系金属間化合物を製造することが試み
られている。この場合の原料粉としては、たとえばチタ
ン粉とアルミニウム粉の混合粉、またはＴｉＡｌ，Ｔｉ
3 Ａｌ等の金属間化合物粉が用いられている。しかしな
がら、これらの原料粉はいずれも難焼結性であるため、
複雑形状部品や薄板などを緻密な焼結材として容易に製
造することはほとんど不可能である。すなわち、混合粉
より金属間化合物ＴｉＡｌを製造する場合には、焼結過
程でアルミニウム粉が溶融すると、自己発熱による強い
燃焼反応が起こり、多量のガス発生とともに焼結材が膨
張して多孔質となる。一旦多孔質となった金属間化合物
を通常の焼結技術により緻密にすることはきわめて困難
である。また、Ｔｉ3Ａｌは燃焼反応を起こさないため
に膨張しないものの、アルミ粉溶融による膨張が避けら
れない。チタン粉自体は優れた焼結性を有し緻密になる
傾向を示すものの、この膨張により相殺され、ＴｉＡｌ
の場合と同様に緻密な焼結材を得ることは難しくなる。
さらに、２相金属間化合物ＴｉＡｌ／Ｔｉ3 Ａｌにおい
ては、ＴｉＡｌ側では燃焼反応による膨張が生じ、かつ
Ｔｉ3 Ａｌ側ではアルミニウム粉溶融による膨張が生じ
るため、上記したようなＴｉＡｌなどの場合と同様に緻
密な焼結材を作ることが困難となる。一方、金属間化合
物粉を用いてＴｉ−Ａｌ系金属間化合物を製造する場合
には、金属間化合物粉自体が難焼結性であるため、通常
の成形−焼結のみの工程により緻密で健全な焼結材を得
ることはきわめて困難である。これを改善し、健全な焼
結材とするためにはサブミクロンの微粉が望まれること
になるが、Ｔｉ−Ａｌ系の化合物粉は活性であり、微粒
化にともない酸素量が顕著に増加するとともに、このよ
うな微粉を直接大気に曝すと自己発熱により燃焼もしく
は爆発が生ずる危険性がある。また、この種の微粉は成
形性が劣ってもいるため、プレス成形する上で問題とな
る。以上のように、焼結法によるＴｉ−Ａｌ系金属化合
物の製造には、原料粉の成形性や焼結性などに問題があ
り、通常の焼結技術によっては緻密な焼結材を作ること
が不可能であるために、ＨＩＰ法、ホットプレス法、パ
ック鍛造法などの高温圧縮技術の応用が検討されてい
る。しかしながら、これらの方法では、工程が複雑とな
り、製品が高価になるのみならず、複雑形状部品や薄板
などの製品の量産が困難で、焼結法の特徴を充分に生か
すことができないという欠点がある。この発明は、以上
の通りの事情に鑑みてなされたものであり、従来法の欠
点を解消し、高温圧縮法を用いずに、通常の焼結技術に
より緻密な焼結材を簡便かつ容易に製造することのでき
る新しいＴｉ−Ａｌ系金属化合物の製造方法を提供する
ことを目的としている。2. Description of the Related Art Conventionally, Ti--Al based intermetallic compounds have generally been produced by a melting method. However, since they are inferior in ductility to metals and alloys, they have complicated shapes. It has been pointed out that there are many problems in the production of parts and thin plates. Therefore, such Ti-A
Although a lot of researches have been made to improve the workability of the intermetallic compound by improving the defects of the ductility of the intermetallic compound,
The reality is that sufficient results have not yet been obtained. Generally, it is known that the sintering method is advantageous for the production of complicated shaped parts, thin plates and the like. Therefore, recently, it has been attempted to produce this Ti—Al-based intermetallic compound by the sintering method. ing. As the raw material powder in this case, for example, a mixed powder of titanium powder and aluminum powder, or TiAl, Ti
3 Intermetallic compound powder such as Al is used. However, since all of these raw material powders are difficult to sinter,
It is almost impossible to easily manufacture complicated shaped parts or thin plates as dense sintered materials. That is, when the intermetallic compound TiAl is produced from the mixed powder, when the aluminum powder is melted during the sintering process, a strong combustion reaction occurs due to self-heating, and a large amount of gas is generated, the sintered material expands and becomes porous. Become. It is extremely difficult to make an intermetallic compound, which has been once porous, dense by a normal sintering technique. Further, Ti 3 Al does not expand because it does not cause a combustion reaction, but expansion due to melting of aluminum powder is unavoidable. Titanium powder itself has excellent sinterability and tends to become dense, but this expansion cancels out TiAl.
It becomes difficult to obtain a dense sintered material as in the case of.
Further, in the two-phase intermetallic compound TiAl / Ti 3 Al, expansion due to combustion reaction occurs on the TiAl side, and expansion due to aluminum powder melting occurs on the Ti 3 Al side, so that it is similar to the case of TiAl as described above. It becomes difficult to make a dense sintered material. On the other hand, when the Ti-Al-based intermetallic compound is produced using the intermetallic compound powder, the intermetallic compound powder itself is difficult to sinter, so that it is dense and sound only by the ordinary molding-sintering process. It is extremely difficult to obtain a good sintered material. Submicron fine powder is desired in order to improve this and make a healthy sintered material, but the Ti-Al-based compound powder is active, and the amount of oxygen increases remarkably with atomization. At the same time, if such fine powder is directly exposed to the atmosphere, there is a risk of combustion or explosion due to self-heating. In addition, since this type of fine powder has poor moldability, it causes a problem in press molding. As described above, in the production of the Ti-Al-based metal compound by the sintering method, there are problems in the formability and sinterability of the raw material powder, and it is necessary to make a dense sintered material by the usual sintering technique. Since it is impossible, application of high temperature compression technology such as HIP method, hot pressing method, pack forging method and the like is being studied. However, in these methods, not only the process becomes complicated and the product becomes expensive, but it is difficult to mass-produce products such as parts with complicated shapes and thin plates, and the characteristics of the sintering method cannot be fully utilized. is there. The present invention has been made in view of the above circumstances, eliminates the drawbacks of the conventional method, and easily and easily produces a dense sintered material by a normal sintering technique without using a high-temperature compression method. It is an object of the present invention to provide a new method for producing a Ti-Al-based metal compound that can be produced.
【課題を解決するための手段】この発明は、上記の課題
を解決するものとして、金属間化合物ＴｉＡｌまたはＴ
ｉ3 Ａｌ，あるいはこれらの２相金属間化合物ＴｉＡｌ
／Ｔｉ3 Ａｌの製造に際し、チタン粉または水素化チタ
ン粉と、チタンを３０〜７０質量％含有するアルミニウ
ム母合金粉とを、各々、所定の金属間化合物組成となる
ように混合し、成形した後に焼結することを特徴とする
Ｔｉ−Ａｌ系金属間化合物の製造方法を提供する。この
発明の方法において、チタンを３０〜７０質量％含有す
るアルミニウム母合金粉を用いるのは、混合により緻密
な焼結材が得られることと、この組成のものは脆く粉末
を作りやすいなどの利点があるためである。チタンが３
０％の場合には、金属間化合物ＴｉＡｌ3 とアルミニウ
ムの２相組織となるが、これより少ないと延性に富むア
ルミニウムの増加により急激に粉末を作りにくくなり、
しかもこのような組成のものを粉末にしようとすると酸
素量が急増し、原料粉末として不適当なものとなる。ま
た、３０％より少ないと、アルミニウムが原子比で８０
％を超えるために、ＴｉＡｌやＴｉＡｌ／Ｔｉ3 Ａｌの
焼結においては、強い燃焼反応が生じて密度が低下す
る。したがって、チタン量は３０質量％以上とする。一
方、チタンが７０％より多い組成では、延性に富むＴｉ
3 Ａｌの増加により粉末を作りにくくなる。しかもこの
場合には、混合するチタン粉または水素化チタン粉の量
が少なくなり、混合粉の成形性が低下してしまう。した
がって、アルミニウム母合金粉中のチタン量は７０質量
％以下であることが望ましい。また、この発明の方法に
おいては、原料粉の一つとして水素化チタンを用いるこ
とができることも特徴の一つである。焼結材の密度を真
密度の９５％以上とするには、使用するチタン粉の粒度
調整が必要となる場合が多い。このような粒度調整は、
チタン粉のミリング等によって行うこともできるが、チ
タン粉より脆い水素化チタンまたは水素化チタン粉のミ
リングの方が有利であり、チタン粉の粒度調整が容易と
なる。一方、水素化チタン粉を混合した原料混合粉につ
いては、脱水素処理が必要となる。この処理は成形前の
混合粉または成形後の成形体について行うことができ
る。より優れた成形性が要求される場合には、成形前の
混合粉について処理することが望ましい。またこの発明
の方法においては、原料粉末を混合する際に、必要に応
じてワックス、樹脂等の潤滑剤あるいは結合剤を添加・
混合することができる。この場合、焼結に先立ちこれら
を除去することが好ましい。また、機械的性質、耐酸化
性および耐食性を改善するために、アルミニウム母合金
粉にはその３０質量％以内でたとえばマンガン、リン、
炭素、クロム、モリブデン、タングステン、バナジウ
ム、ジルコニウム、ハフニウム、イットリウム、希土類
元素を添加することも有効である。これらの、添加元素
の内、マンガン、リン、バナジウム、ニオブ、クロムお
よびモリブデンは金属間化合物の延性を向上させる作用
がある。また、炭素、ジルコニウム、バナジウム、ニオ
ブ、クロム、モリブデン、タングステン、ハフニウム、
イットリウムおよび希土類元素には、強度を向上させる
作用がある。リン、イットリウムおよび希土類元素は、
耐酸化性の向上に有効である。焼結は、真空または不活
性ガス雰囲気中で行うことができる。焼結温度は金属間
化合物によっても異なるが、たとえば1200〜1500℃程度
が緻密な焼結材を得るのに適した温度として例示され
る。さらにこの発明の方法においては、焼結した後の焼
結材を常温または高温で圧縮処理することを好ましい態
様として包含してもいる。この焼結後の圧縮処理により
焼結後にも残留する空隙が除去され、より緻密で強靭な
焼結材の製造が可能となる。たとえば複雑形状部品を製
造する場合には、その密度が真密度の９５％以上のもの
については、キャンニングすることなくたとえばＨＩ
Ｐ，擬ＨＩＰ法などで圧縮処理することができ、薄板の
場合には圧延、鍛造などで行うことができる。In order to solve the above problems, the present invention provides an intermetallic compound TiAl or T.
i 3 Al, or these two-phase intermetallic compounds TiAl
In the production of / Ti 3 Al, titanium powder or titanium hydride powder and aluminum mother alloy powder containing 30 to 70% by mass of titanium were mixed and molded so as to have a predetermined intermetallic compound composition. Provided is a method for producing a Ti-Al-based intermetallic compound, which is characterized by being sintered later. In the method of the present invention, the use of the aluminum master alloy powder containing 30 to 70% by mass of titanium is advantageous in that a dense sintered material can be obtained by mixing, and that this composition is brittle and powder can be easily formed. Because there is. 3 titanium
In the case of 0%, the intermetallic compound TiAl 3 and aluminum have a two-phase structure, but if it is less than this, it becomes difficult to make powder rapidly due to the increase of aluminum which is rich in ductility,
In addition, when powder having a composition as described above is used, the amount of oxygen increases rapidly, which makes the powder unsuitable. Also, if it is less than 30%, the atomic ratio of aluminum is 80
%, A strong combustion reaction occurs in the sintering of TiAl or TiAl / Ti 3 Al and the density decreases. Therefore, the amount of titanium is 30% by mass or more. On the other hand, in a composition containing more than 70% titanium, Ti with high ductility
3 Increase of Al makes it difficult to make powder. Moreover, in this case, the amount of titanium powder or titanium hydride powder to be mixed becomes small, and the moldability of the mixed powder is deteriorated. Therefore, the amount of titanium in the aluminum mother alloy powder is preferably 70% by mass or less. In addition, one of the features of the method of the present invention is that titanium hydride can be used as one of the raw material powders. In order to make the density of the sintered material 95% or more of the true density, it is often necessary to adjust the particle size of the titanium powder used. Such particle size adjustment is
It can be performed by milling titanium powder, but milling titanium hydride or titanium hydride powder, which is more brittle than titanium powder, is more advantageous, and the particle size of titanium powder can be easily adjusted. On the other hand, the raw material mixed powder obtained by mixing the titanium hydride powder needs to be dehydrogenated. This treatment can be performed on the mixed powder before molding or the molded body after molding. When higher moldability is required, it is desirable to treat the mixed powder before molding. Further, in the method of the present invention, when the raw material powders are mixed, if necessary, a lubricant such as wax or resin or a binder is added.
Can be mixed. In this case, it is preferable to remove them prior to sintering. Further, in order to improve the mechanical properties, the oxidation resistance and the corrosion resistance, the aluminum master alloy powder may contain manganese, phosphorus,
It is also effective to add carbon, chromium, molybdenum, tungsten, vanadium, zirconium, hafnium, yttrium and rare earth elements. Among these additive elements, manganese, phosphorus, vanadium, niobium, chromium and molybdenum have an effect of improving the ductility of the intermetallic compound. In addition, carbon, zirconium, vanadium, niobium, chromium, molybdenum, tungsten, hafnium,
Yttrium and rare earth elements have a function of improving strength. Phosphorus, yttrium and rare earth elements are
It is effective for improving the oxidation resistance. Sintering can be done in vacuum or in an inert gas atmosphere. Although the sintering temperature differs depending on the intermetallic compound, for example, about 1200 to 1500 ° C. is exemplified as a temperature suitable for obtaining a dense sintered material. Further, in the method of the present invention, it is preferable to compress the sintered material after sintering at room temperature or high temperature. By the compression treatment after the sintering, voids remaining after the sintering are removed, and it becomes possible to manufacture a denser and stronger sintered material. For example, in the case of manufacturing a complex shaped part, if the density is 95% or more of the true density, for example, HI is used without canning.
P and pseudo HIP methods can be used for compression treatment, and in the case of a thin plate, rolling and forging can be performed.
【実施例】以下、実施例を示し、この発明のＴｉ−Ａｌ
系金属間化合物の製造方法についてさらに詳しく説明す
る。実施例１〜２ 表１に示した試料No.1チタン粉41.2％に、表２に示した
試料No.1のアルミニウム母合金粉を58.8％添加したもの
（実施例１）と、表１に示した試料No.2の水素化チタン
粉42.8％に、表２に示した試料No.1のアルミニウム母合
金粉を58.8％添加したもの（実施例２）を、各々、ボー
ルミルで１時間混合し、チタンを63.3質量％含有するＴ
ｉＡｌ組成の混合粉を調製した。この混合粉を３トン／
cm2 で成形し、実施例１では真空中で脱水素後、真空中
1370℃で１時間焼結した。焼結材の組織はいずれも金属
間化合物ＴｉＡｌの単相であった。EXAMPLES Examples are shown below to illustrate the Ti--Al of the present invention.
The method for producing the intermetallic compound will be described in more detail. Examples 1 and 2 The sample No. 1 titanium powder 41.2% shown in Table 1 was added with the aluminum master alloy powder No. 1 sample 58.8% shown in Table 2 (Example 1) and Table 1 58.8% of the aluminum master alloy powder of sample No. 1 shown in Table 2 (Example 2) was added to 42.8% of the titanium hydride powder of sample No. 2 shown in the above, and each was mixed in a ball mill for 1 hour. , T containing 63.3% by mass of titanium
A mixed powder having an iAl composition was prepared. 3 tons of this mixed powder
cm 2 and, in Example 1, after dehydrogenation in vacuum, in vacuum
Sintered at 1370 ° C for 1 hour. The structure of each of the sintered materials was a single phase of intermetallic compound TiAl.
【表１】 [Table 1]
【表２】 焼結前後の密度物性は、各々、図１の値（１）（実施例
１）および値（１′）（実施例２）に示した通りであっ
た。後述する比較例１〜２との対比からも明らかなよう
に、この発明の方法により緻密なＴｉＡｌ金属間化合物
を製造することが可能であることが確認された。焼結材
の密度物性は、図１に示したように、この発明の方法に
よる焼結密度は真密度の９６％以上にも達するのに対
し、従来法では高々８７％であった。比較例１〜２ 表１の試料No.2の水素化チタン粉65.7％に表１の試料N
o.3のアルミニウム粉を36.7％添加し、実施例２とほぼ
同様な組成と粒度を有する混合粉を調製した後、実施例
２と同様に、順次、成形、脱水素および焼結を行った。
得られた焼結材の組織は実施例１および２と同様であっ
た（比較例１）。また、次の表３に示した試料No.1の実
施例１とほぼ同様な組成のＴｉＡｌ金属間化合物粉を同
様にして成形、焼結した。この焼結材の組織も実施例１
および２と同様であった（比較例２）。[Table 2] The density physical properties before and after sintering were as shown in the value (1) (Example 1) and the value (1 ′) (Example 2) in FIG. 1, respectively. As is clear from comparison with Comparative Examples 1 and 2 described later, it was confirmed that it is possible to produce a dense TiAl intermetallic compound by the method of the present invention. As shown in FIG. 1, the density property of the sintered material was as high as 87% by the conventional method, whereas the sintered density by the method of the present invention reached 96% or more of the true density. Comparative Examples 1 and 2 65.7% of titanium hydride powder of Sample No. 2 in Table 1 was added to Sample N of Table 1
36.7% of o.3 aluminum powder was added to prepare a mixed powder having substantially the same composition and particle size as in Example 2, and thereafter, molding, dehydrogenation and sintering were sequentially performed in the same manner as in Example 2. .
The structure of the obtained sintered material was the same as in Examples 1 and 2 (Comparative Example 1). In addition, TiAl intermetallic compound powder having substantially the same composition as in Example 1 of Sample No. 1 shown in Table 3 below was shaped and sintered in the same manner. The structure of this sintered material is also Example 1
And 2 (Comparative Example 2).
【表３】 これらの焼結材の焼結前後の密度物性は、各々、図１の
値（２）（比較例１）および値（３）（比較例２）の通
りであった。緻密なＴｉＡｌ金属間化合物は得られず、
この図１からも明らかなようにこれらの焼結材の密度は
低かった。実施例３〜４ 前記表１の試料No.2の水素化チタン粉75.4％に表２の試
料No.1のアルミニウム母合金粉を27.4％添加したもの
（実施例３）と、表１の試料No.2の水素化チタン粉55.2
％に表２の試料No.2のアルミニウム母合金粉を46.8％添
加したもの（実施例４）を、各々、ボールミルで１時間
混合し、チタンを82.9質量％含有するＴｉ3 Ａｌ組成の
混合粉を調製した。この混合粉を３トン／cm2 で成形
し、真空中で脱水素後、真空中1370℃で１時間焼結し
た。焼結材の組織はいずれも金属間化合物Ｔｉ3 Ａｌと
少量のＴｉ相との混合組織であった。焼結前後の密度物
性は、各々、図２の値（１）と値（１′）に示した通り
であった。後述する比較例３〜４との対比からも明らか
なように、この発明の方法により緻密なＴｉＡｌ金属間
化合物を製造することが可能であることが図２より確認
される。比較例３〜４ 表１の試料No.2の水素化チタン粉86.1％に表１の試料N
o.3のアルミニウム粉を17.1％添加し、実施例３とほぼ
同様な組成と同様な粒度を有する混合粉を調製した後、
実施例３と同様に、順次、成形、脱水素および焼結を行
った。焼結材の組織は実施例３と同様であった（比較例
３）。一方、表３に示した試料No.2の実施例３とほぼ同
様な組成のＴｉ3 Ａｌ金属間化合物粉を同様な手順で成
形、焼結した。この焼結材の組織も実施例３と同様であ
った（比較例４）。これらの焼結前後の密度物性は、各
々、図２の値（２）（比較例３）および値（３）（比較
例４）の通りであった。しかしながら、緻密なＴｉ3 Ａ
ｌ金属間化合物は得られなかった。実施例５ 表１の試料No.2の水素化チタン粉54.4％に表２の試料N
o.1のアルミニウム母合金粉47.6％を添加し、ボールミ
ルで１時間混合した後、チタンを70.3質量％含有するＴ
ｉＡｌ／Ｔｉ3 Ａｌ組成の混合粉を調製した。この混合
粉を３トン／cm2成形し、真空中で脱水素後、真空中137
0℃で１時間焼結した。焼結材の組織はＴｉＡｌとＴｉ
3 Ａｌの混合組織であった。焼結前後密度の物性は図３
の値（１）に示した通りであった。後述する比較例５〜
６との対比からも明らかなように、この発明の方法によ
り緻密なＴｉＡｌ金属間化合物を製造することが可能で
あることが図３より確認される。比較例５〜６ 表１の試料No.2の水素化チタン粉73.0％に表１の試料N
o.3のアルミニウム粉29.7％添加し、実施例５とほぼ同
様な組成と粒度を有する混合粉を調製した後、実施例５
と同様に、順次、成形、脱水素および焼結を行った。焼
結材の組織は実施例５と同様であった（比較例５）。一
方、表３に示した試料No.3の実施例５とほぼ同様な組成
のＴｉＡｌ／Ｔｉ3Ａｌ金属間化合物粉を同様な手順で
成形、焼結した。焼結材の組織は実施例５と同様であっ
た（比較例６）。これらの密度物性は、各々、図３の値
（２）（比較例５）および値（３）（比較例６）の通り
であった。緻密なＴｉＡｌ／Ｔｉ3 Ａｌ金属間化合物は
得られなかった。実施例６ 実施例１で焼結した図１の値（１）および値（１′）に
示される焼結材について、キャンニングすることなくア
ルゴン雰囲気中、1350℃，100ＭＰａ，１時間の条件で
熱間静水圧プレス（ＨＩＰ）処理を行った。ＨＩＰ処理
後の密度物性は、各々、図４の値（１）および値
（１′）に示した通りであった。後述する比較例７〜８
との対比からも明らかなように、焼結−圧縮材の密度物
性は、この発明の方法による金属間化合物の場合にはほ
ぼ100％になるのに対し、従来法では９２％以下となっ
た。緻密な焼結材を製造するのには、この発明の方法が
格段に優れていることが確認される。比較例７〜８ 実施例１で焼結した図１の値（２）および値（３）に示
される焼結材について、実施例６と同様のＨＩＰ処理を
行った。ＨＩＰ処理後の密度物性は、各々、図４の値
（２）（比較例７）および値（３）（比較例８）に示し
た通りであった。これらの密度は、この発明の方法によ
り製造された金属間化合物より著しく低かった。 もち
ろんこの発明は、以上の例によって限定されるものでは
ない。組成比や、潤滑剤、結合剤および添加元素の種類
や添加量等の細部については様々な態様が可能であるこ
とはいうまでもない。[Table 3] The density physical properties of these sintered materials before and after sintering were as shown by the value (2) (Comparative Example 1) and the value (3) (Comparative Example 2) in FIG. 1, respectively. A dense TiAl intermetallic compound cannot be obtained,
As is apparent from FIG. 1, the density of these sintered materials was low. Examples 3 to 4 77.4% of the titanium hydride powder of sample No. 2 in Table 1 above, to which 27.4% of the aluminum mother alloy powder of sample No. 1 in Table 2 was added (Example 3), and the sample of Table 1 No.2 titanium hydride powder 55.2
%, To which 46.8% of the aluminum mother alloy powder of sample No. 2 in Table 2 was added (Example 4) was mixed in a ball mill for 1 hour, respectively, and a mixed powder of Ti 3 Al composition containing 82.9% by mass of titanium was mixed. Was prepared. The mixed powder was molded at 3 ton / cm 2 , dehydrogenated in vacuum, and then sintered in vacuum at 1370 ° C. for 1 hour. The structure of each of the sintered materials was a mixed structure of the intermetallic compound Ti 3 Al and a small amount of Ti phase. The density physical properties before and after sintering were as shown in the values (1) and (1 ′) in FIG. 2, respectively. As is clear from comparison with Comparative Examples 3 to 4 described later, it is confirmed from FIG. 2 that a dense TiAl intermetallic compound can be produced by the method of the present invention. Comparative Examples 3 to 4 86.1% of titanium hydride powder of sample No. 2 in Table 1 was added to sample N of Table 1.
After adding 17.1% of o.3 aluminum powder to prepare a mixed powder having a composition substantially similar to that of Example 3 and a similar particle size,
As in Example 3, molding, dehydrogenation and sintering were sequentially performed. The structure of the sintered material was the same as in Example 3 (Comparative Example 3). On the other hand, Ti 3 Al intermetallic compound powder having substantially the same composition as in Example 3 of Sample No. 2 shown in Table 3 was molded and sintered by the same procedure. The structure of this sintered material was similar to that of Example 3 (Comparative Example 4). The density physical properties before and after sintering were as shown by the value (2) (Comparative Example 3) and the value (3) (Comparative Example 4) in FIG. 2, respectively. However, fine Ti 3 A
No intermetallic compound was obtained. Example 5 Titanium hydride powder of sample No. 2 in Table 1 was 54.4% and sample N in Table 2 was
47.6% of aluminum mother alloy powder of o.1 was added and mixed in a ball mill for 1 hour, then T containing 70.3% by mass of titanium
A mixed powder having an iAl / Ti 3 Al composition was prepared. This mixed powder is molded to 3 ton / cm 2 and dehydrogenated in vacuum, then 137 in vacuum
Sintered at 0 ° C for 1 hour. The structure of the sintered material is TiAl and Ti
It had a mixed structure of 3 Al. Figure 3 shows the physical properties of the density before and after sintering.
Was as shown in the value (1). Comparative examples 5 to be described later
As is clear from the comparison with Example 6, it is confirmed from FIG. 3 that it is possible to produce a dense TiAl intermetallic compound by the method of the present invention. Comparative Examples 5 and 6 73.0% of titanium hydride powder of sample No. 2 in Table 1 and sample N in Table 1
After adding 29.7% of o.3 aluminum powder to prepare a mixed powder having substantially the same composition and particle size as in Example 5, Example 5
In the same manner as above, molding, dehydrogenation and sintering were sequentially performed. The structure of the sintered material was the same as in Example 5 (Comparative Example 5). On the other hand, TiAl / Ti 3 Al intermetallic compound powder having substantially the same composition as in Example 5 of sample No. 3 shown in Table 3 was molded and sintered by the same procedure. The structure of the sintered material was the same as in Example 5 (Comparative Example 6). These density physical properties were as shown by the value (2) (Comparative Example 5) and the value (3) (Comparative Example 6) in FIG. 3, respectively. No dense TiAl / Ti 3 Al intermetallic compound was obtained. Example 6 The sintered materials shown in the values (1) and (1 ′) of FIG. 1 sintered in Example 1 were subjected to 1350 ° C., 100 MPa, 1 hour in an argon atmosphere without canning. Hot isostatic pressing (HIP) treatment was performed. The density physical properties after the HIP treatment were as shown in the values (1) and (1 ′) in FIG. 4, respectively. Comparative Examples 7 to 8 described later
As is clear from the comparison with, the density physical property of the sintered-compressed material was almost 100% in the case of the intermetallic compound according to the method of the present invention, whereas it was 92% or less in the conventional method. . It is confirmed that the method of the present invention is remarkably excellent in producing a dense sintered material. Comparative Examples 7 to 8 HIP treatment similar to that in Example 6 was performed on the sintered materials shown in values (2) and (3) in FIG. 1 which were sintered in Example 1. The density physical properties after the HIP treatment were as shown in the values (2) (Comparative Example 7) and the value (3) (Comparative Example 8) in FIG. 4, respectively. Their densities were significantly lower than the intermetallic compounds produced by the method of this invention. Of course, the present invention is not limited to the above examples. It goes without saying that various aspects are possible in terms of details such as composition ratios, types and amounts of lubricants, binders and additional elements.
【発明の効果】以上詳しく説明した通り、この発明によ
って、通常の焼結技術により密度が真密度の９５％以上
の焼結材を簡便かつ容易に製造することができる。高性
能な複雑形状部品や薄板などの製品の量産も可能とな
る。また、たとえばチタンを３５〜４０質量％有するア
ルミ母合金粉を原料粉として用いた場合には、1340℃よ
りも高温で液相焼結することができ、短時間焼結での緻
密な焼結材の製造が可能となる。さらには、チタン粉ま
たは水素化チタン粉の混合により、混合粉の成形性など
が改善される。水素化チタン粉はチタン粉に比べて安価
であるため、水素化チタン粉の使用により原料粉を安価
とすることも可能となる。As described in detail above, according to the present invention, a sintered material having a density of 95% or more of the true density can be simply and easily manufactured by a normal sintering technique. Mass production of high-performance complex shaped parts and products such as thin plates will also be possible. Further, for example, when an aluminum mother alloy powder containing 35 to 40 mass% of titanium is used as a raw material powder, liquid phase sintering can be performed at a temperature higher than 1340 ° C, and dense sintering in a short time sintering is possible. It becomes possible to manufacture wood. Furthermore, the mixing of titanium powder or titanium hydride powder improves the moldability of the mixed powder. Since titanium hydride powder is cheaper than titanium powder, the raw material powder can be made inexpensive by using titanium hydride powder.
【図１】金属間化合物ＴｉＡｌについての焼結前後の密
度をこの発明の方法と従来法とで比較した密度表示図で
ある。FIG. 1 is a density display diagram comparing the densities of an intermetallic compound TiAl before and after sintering by a method of the present invention and a conventional method.
【図２】金属間化合物Ｔｉ3 Ａｌについての焼結前後の
密度をこの発明の方法と従来法とで比較した密度表示図
である。FIG. 2 is a density display diagram comparing the densities of the intermetallic compound Ti 3 Al before and after sintering by the method of the present invention and the conventional method.
【図３】２相間化合物ＴｉＡｌ／Ｔｉ3 Ａｌについての
焼結前後の密度をこの発明の方法と従来法とで比較した
密度表示図である。FIG. 3 is a density display diagram comparing the densities of a two-phase compound TiAl / Ti 3 Al before and after sintering by the method of the present invention and the conventional method.
【図４】金属間化合物ＴｉＡｌについて、熱間静水圧プ
レス（ＨＩＰ）処理前後の密度をこの発明の方法と従来
法とで比較した密度表示図である。FIG. 4 is a density display diagram comparing the density of the intermetallic compound TiAl before and after the hot isostatic pressing (HIP) treatment between the method of the present invention and the conventional method.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成５年８月５日[Submission date] August 5, 1993
【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】発明の名称[Name of item to be amended] Title of invention
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【発明の名称】 Ｔｉ／Ａｌ系金属間化合物の製
造方法 ─────────────────────────────────────────────────────
Title of the Invention Method for producing Ti / Al intermetallic compound ──────────────────────────────────── ──────────────────
【手続補正書】[Procedure amendment]
【提出日】平成５年８月５日[Submission date] August 5, 1993
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】全図[Correction target item name] All drawings
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図１】 [Figure 1]
【図２】 [Fig. 2]
【図３】 [Figure 3]
【図４】 [Figure 4]
Claims (3)
ｌ，あるいはこれらの２相金属間化合物ＴｉＡｌ／Ｔｉ
3 Ａｌの製造に際し、チタン粉または水素化チタン粉
と、チタンを３０〜７０質量％含有するアルミニウム母
合金粉とを、各々、所定の金属間化合物組成となるよう
に混合し、成形した後に焼結することを特徴とするＴｉ
−Ａｌ系金属間化合物の製造方法。1. Intermetallic compound TiAl or Ti 3 A
l, or these two-phase intermetallic compounds TiAl / Ti
3 At the time of producing Al, titanium powder or titanium hydride powder and aluminum mother alloy powder containing titanium in an amount of 30 to 70% by mass are mixed so that each has a predetermined intermetallic compound composition, and the mixture is baked after molding. Ti characterized by binding
-Method for producing Al-based intermetallic compound.
素処理する請求項１の製造方法。2. The manufacturing method according to claim 1, wherein dehydrogenation treatment is carried out before or after molding, if necessary.
する請求項１または２の製造方法。3. The manufacturing method according to claim 1, wherein the sintered material is compressed at room temperature or at a high temperature after sintering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3174698A JP2716886B2 (en) | 1991-06-20 | 1991-06-20 | Method for producing Ti-Al intermetallic compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3174698A JP2716886B2 (en) | 1991-06-20 | 1991-06-20 | Method for producing Ti-Al intermetallic compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH073355A true JPH073355A (en) | 1995-01-06 |
| JP2716886B2 JP2716886B2 (en) | 1998-02-18 |
Family
ID=15983107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3174698A Expired - Lifetime JP2716886B2 (en) | 1991-06-20 | 1991-06-20 | Method for producing Ti-Al intermetallic compound |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2716886B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012036489A (en) * | 2010-08-11 | 2012-02-23 | Toda Kogyo Corp | Method for manufacturing metal nanoparticle powder, and metal nanoparticle powder |
| CN114990371A (en) * | 2022-05-06 | 2022-09-02 | 北京科技大学 | Fine-grained titanium-aluminum alloy and method for preparing same by adopting powder metallurgy rapid hydrogenation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01301801A (en) * | 1988-05-31 | 1989-12-06 | Sumitomo Light Metal Ind Ltd | Production of ti-al intermetallic compound powder |
-
1991
- 1991-06-20 JP JP3174698A patent/JP2716886B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01301801A (en) * | 1988-05-31 | 1989-12-06 | Sumitomo Light Metal Ind Ltd | Production of ti-al intermetallic compound powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012036489A (en) * | 2010-08-11 | 2012-02-23 | Toda Kogyo Corp | Method for manufacturing metal nanoparticle powder, and metal nanoparticle powder |
| CN114990371A (en) * | 2022-05-06 | 2022-09-02 | 北京科技大学 | Fine-grained titanium-aluminum alloy and method for preparing same by adopting powder metallurgy rapid hydrogenation |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2716886B2 (en) | 1998-02-18 |
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