JP3279346B2 - Method for producing amorphous TiAl-based powder - Google Patents
Method for producing amorphous TiAl-based powderInfo
- Publication number
- JP3279346B2 JP3279346B2 JP19145892A JP19145892A JP3279346B2 JP 3279346 B2 JP3279346 B2 JP 3279346B2 JP 19145892 A JP19145892 A JP 19145892A JP 19145892 A JP19145892 A JP 19145892A JP 3279346 B2 JP3279346 B2 JP 3279346B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- amorphous
- reactor
- tial
- stirring
- 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.)
- Expired - Fee Related
Links
- 239000000843 powder Substances 0.000 title claims description 51
- 229910010038 TiAl Inorganic materials 0.000 title claims description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- 238000005551 mechanical alloying Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 239000007790 solid phase Substances 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 4
- 230000009466 transformation Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 2
- 238000005275 alloying Methods 0.000 claims 1
- 239000010936 titanium Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000005280 amorphization Methods 0.000 description 5
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910000765 intermetallic Inorganic materials 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002076 thermal analysis method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 241000287462 Phalacrocorax carbo Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ＴｉＡｌ3 、ＴｉＡ
ｌ、Ｔｉ3 Ａｌ等のアモルファスＴｉＡｌ系粉末を効率
よく製造するための方法に関する。The present invention relates to TiAl 3 , TiA
1 and a method for efficiently producing an amorphous TiAl-based powder such as Ti 3 Al.
【０００２】[0002]
【従来の技術】従来、アモルファス（非晶質）構造の合
金粉末を得るためには融液や気相からの超急冷凝固法が
用いられてきたが、最近、メカニカルアロイング法によ
る固相アモルファス化のプロセスが開発されている。こ
の方法を用いると超急冷凝固法より広い組成範囲でアモ
ルファス合金を得ることができ、溶解や凝固等の工程も
不要となることから、アモルファス合金の工業的な製造
技術として注目されている。2. Description of the Related Art Conventionally, an ultra-rapid solidification method from a melt or a gas phase has been used to obtain an alloy powder having an amorphous structure. Process is being developed. By using this method, an amorphous alloy can be obtained in a wider composition range than in the rapid quenching solidification method, and steps such as melting and solidification are not required.
【０００３】アモルファス合金をメカニカルアロイング
手段を用いて製造する方法に関しては、例えばＣｏ、Ｎ
ｉまたはＦｅとＴｉ、ＮｂまたはＺｒからなる合金組成
をもつ非晶質微小粒子の製造方法（特開昭63−118002号
公報）、ＣｏリッチＣｏ合金系の高飽和磁束密度または
磁歪零特性をもつ軟質磁性アモルファス合金の製造方法
（特開昭63−241102号公報、特開昭63−243203号公報)
等の提案がある。このほか、ＴｉＡｌ系などの金属間化
合物粉末を製造する際にメカニカルアロイングを用いる
方法（特開平１−215903号公報）も提案されているが、
この方法ではアモルファス合金粉末を得ることについて
は意図されていない。[0003] Regarding a method of producing an amorphous alloy using mechanical alloying means, for example, Co, N
Method for producing amorphous fine particles having an alloy composition of i or Fe and Ti, Nb or Zr (JP-A-63-118002), which has a high saturation magnetic flux density or zero magnetostriction characteristic of a Co-rich Co alloy system Production method of soft magnetic amorphous alloy (JP-A-63-241102, JP-A-63-243203)
There are proposals such as. In addition, a method using mechanical alloying when producing an intermetallic compound powder such as a TiAl-based powder (JP-A-1-215903) has been proposed.
This method is not intended to obtain an amorphous alloy powder.
【０００４】[0004]
【発明が解決しようとする課題】攪拌型ボールミルを利
用したメカニカルアロイングは、高エネルギー下での衝
撃、剪断、冷間圧接が繰り返されるため、他の方法に比
較して短時間内にアモルファス化を完了させることがで
きる利点がある。ところが、ＴｉとＡｌの反応をこの高
エネルギー過程を経て進行させると、一時的または局所
的に反応温度が数百℃にも達し、このため結晶性の金属
間化合物などの好ましくない不均一相の生成を促して均
一なアモルファス粉末を得ることができなくなる。ま
た、処理時に鋼製ボールなどを高速で攪拌する関係で、
ボールミル内部の反応器材から主にＦｅ分が不純物とし
てアモルファス粉末中に混入するうえ、安定な反応の進
行を阻害する問題点があった。In mechanical alloying using a stirring type ball mill, impact, shearing and cold welding under high energy are repeated, so that the amorphous alloy becomes amorphous in a shorter time than other methods. There is an advantage that can be completed. However, when the reaction between Ti and Al proceeds through this high-energy process, the reaction temperature temporarily or locally reaches several hundred degrees Celsius, and therefore, undesirable heterogeneous phases such as crystalline intermetallic compounds are formed. Generation is promoted and uniform amorphous powder cannot be obtained. In addition, due to the high speed stirring of steel balls during processing,
There has been a problem that Fe is mainly mixed as impurities from the reactor material inside the ball mill into the amorphous powder and that the progress of the stable reaction is hindered.
【０００５】本発明は上記の問題点を解消するために開
発されたもので、メカニカルアロイング法を用いて高品
位のＴｉＡｌ系組成からなる固相アモルファス粉末を安
定かつ効率的に製造する方法を提供することを目的とし
ている。SUMMARY OF THE INVENTION The present invention has been developed to solve the above-mentioned problems, and a method for stably and efficiently producing a solid-phase amorphous powder having a high-quality TiAl-based composition by using a mechanical alloying method has been developed. It is intended to provide.
【０００６】[0006]
【課題を解決するための手段】上記の目的を達成するた
めの本発明によるアモルファスＴｉＡｌ系粉末の製造方
法は、ＴｉとＡｌの混合粉末を不活性雰囲気に保たれた
攪拌型ボールミルの反応器によりメカニカルアロイング
するにあたり、メカニカルアロイングの処理前に、前記
反応器となる攪拌型ボールミルの内部を、予めＴｉ粉、
Ａｌ粉またはＴｉＡｌ系粉末の単独または混合物により
コーティングし、温度６０〜８０℃の範囲においてＴｉ
とＡｌの多層構造化を行わせる多層構造化の過程と、該
多層構造化の過程後に行われる、反応温度の急激な上昇
を経て、温度８０℃を越え、１５０℃以下の範囲におい
て固相アモルファス変態を行わせる固相アモルファス変
態の過程との２段階の過程を、攪拌型ボールミルの攪拌
回転数を３００ｒｐｍ以下に設定するとともに、反応器
に供給する冷却水を用いて反応器を強制冷却して、該２
段階の過程における反応温度を制御することにより、行
うことを構成上の特徴とする。In order to achieve the above object, a method for producing an amorphous TiAl-based powder according to the present invention is provided by using a stirred ball mill reactor in which a mixed powder of Ti and Al is kept in an inert atmosphere. In mechanical alloying , before the mechanical alloying treatment,
The inside of a stirring type ball mill serving as a reactor is previously filled with Ti powder,
Al powder or TiAl powder alone or as a mixture
Coated, and at a temperature in the range of
Comprising the steps of a multilayer structuring Ru to perform the multi-layer structure of Al and, the
It is performed after the process of multi-layer structured, through a rapid increase in the reaction temperature, exceeding the temperature 80 ° C., 0.99 ° C. varying solid amorphous to perform solid phase amorphous transformation in the following ranges
The two-stage process with the agitating type ball mill
Set the rotation speed to 300 rpm or less, and
The reactor was forcibly cooled using cooling water supplied to
By controlling the reaction temperature in the course of the step,
Cormorant it is a feature of the configuration a.
【０００７】原料となるＴｉとＡｌの混合粉末は、微粉
砕されたＴｉ粉末とＡｌ粉末を目的とするアルモファス
ＴｉＡｌ系粉末の組成に応じて所定の原子比に配合し、
均一に混合したものが用いられる。メカニカルアロイン
グの反応器となる撹拌型ボールミルには、複数の撹拌棒
を軸着した撹拌器を装着した密閉反応槽の内部に鋼球や
セラミックス球などの撹拌球を入れた構造のものが用い
られるが、本発明の目的には反応器に水冷ジャケットお
よび温度計測装置を設置し、反応温度を制御し得る構造
に設計された装置が効果的に適用される。The mixed powder of Ti and Al as raw materials is prepared by mixing the finely pulverized Ti powder and Al powder in a predetermined atomic ratio according to the composition of the target Almoface TiAl-based powder.
What is uniformly mixed is used. The stirring type ball mill used as a mechanical alloying reactor has a structure in which stirring balls such as steel balls and ceramic balls are put inside a sealed reaction tank equipped with a stirrer with a plurality of stirring rods. However, for the purpose of the present invention, an apparatus designed to have a structure capable of controlling a reaction temperature by installing a water cooling jacket and a temperature measuring device in a reactor is effectively applied.
【０００８】撹拌型ボールミルは、メカニカルアロイン
グの処理前に原料混合粉末と接触する内壁、撹拌器材等
に対し、予めＴｉ粉、Ａｌ粉またはＴｉＡｌ系粉末の単
独または混合物をコーティングしておくことが好まし
い。このコーティングにより、不純物の混入量が著しく
低下するうえ反応時間が大幅に短縮化でき、しかも品質
性状が向上する効果がもたらされる。[0008] In the stirring type ball mill, before the mechanical alloying treatment, the inner wall, the stirrer, etc., which come into contact with the raw material mixed powder, are coated with Ti powder, Al powder or TiAl-based powder alone or in advance. preferable. By this coating, the amount of impurities is significantly reduced, the reaction time can be significantly reduced, and the effect of improving the quality properties is brought about.
【０００９】メカニカルアロイングの条件は、反応器の
内部をアルゴンガス等で不活性雰囲気に保ち、反応器を
強制冷却して反応過程の温度水準を安定的に１５０℃以
下、好ましくは１００℃以下の温度域に保持することが
第１の要件となる。メカニカルアロイングの過程では外
的、内的要因により温度が急激に上昇するが、反応過程
でこの温度を１５０℃以下に制御することにより、Ｔｉ
とＡｌが結晶性の金属間化合物に転化することを防止す
る。また、反応系内を不活性雰囲気に保つ理由は原料や
反応生成物の酸化などの現象を防止するためで、真空で
あっても差し支えない。The conditions for mechanical alloying are as follows: the inside of the reactor is maintained in an inert atmosphere with argon gas or the like, and the reactor is forcibly cooled to stably maintain the temperature level in the reaction process at 150 ° C. or lower, preferably 100 ° C. or lower. Is the first requirement. In the process of mechanical alloying, the temperature rises rapidly due to external and internal factors, but by controlling this temperature to 150 ° C. or less in the reaction process, Ti
And Al are prevented from being converted into a crystalline intermetallic compound. The reason why the inside of the reaction system is kept in an inert atmosphere is to prevent phenomena such as oxidation of raw materials and reaction products, and a vacuum may be used.
【００１０】第２の要件は、ＴｉとＡｌの多層構造化の
段階を介して固相アモルファスに変態させることであ
る。すなわち、メカニカルアロイングによるアモルファ
ス化は、Ｔｉ粉とＡｌ粉がメカニカルアロイング処理に
よる粉砕−再圧接の繰り返しで多層構造化する段階と反
応温度が急激に上昇してほぼ一定温度で固相アモルファ
ス化が進行する段階との２段階の過程を経ることが重要
で、前段階の層状構造を十分に形成せずに直接高温での
アモルファス化を進行させた場合には正常なアモルファ
ス変態を得ることができなくなる。均一な多層構造化を
経て固相アモルファス化を進行させるためには、撹拌型
ボールミルの撹拌回転数を３００rpm 以下に設定し、反
応器に供給する冷却水の温度を可及的に低く、かつ設定
流量に対するバラツキをなくす等の条件設定を与えるこ
とが好ましい対応操作となる。The second requirement is to transform into a solid phase amorphous through a multi-layered structure of Ti and Al. Amorphization by mechanical alloying is a process in which Ti powder and Al powder are multi-layered by repetition of pulverization and re-welding by mechanical alloying, and the reaction temperature rises sharply, and the solid phase becomes amorphous at almost constant temperature. It is important to go through a two-stage process with the stage in which the phase progresses. If the amorphization directly proceeds at high temperature without sufficiently forming the layer structure in the previous stage, a normal amorphous transformation can be obtained. become unable. In order to progress the solid-phase amorphization through uniform multilayer structure, the stirring rotation speed of the stirring ball mill is set to 300 rpm or less, and the temperature of the cooling water supplied to the reactor is set as low and as possible. It is a preferable corresponding operation to provide a condition setting such as eliminating variations in the flow rate.
【００１１】[0011]
【作用】本発明によるメカニカルアロイングは、次のよ
うな機構を経ておこなわれる。まず、撹拌型ボールミル
の反応器にＴｉとＡｌの混合粉末を入れて撹拌を開始す
ると、その直後に一時的に反応温度が急激に上昇し、つ
いで一定の温度水準で推移する。この段階で、撹拌によ
るミリング作用で粉砕、再圧接が安定に反復されながら
原料混合粉末の多層構造化が進む。多層構造化が臨界に
達すると、一旦反応温度が急上昇したのち安定した温度
で反応が進行する。この段階で原料粉末はアモルファス
ＴｉＡｌ系粉末に転化する。アモルファス化が完結する
と温度が急激に低下して反応が終了する。The mechanical alloying according to the present invention is performed through the following mechanism. First, when a mixed powder of Ti and Al is put into a reactor of a stirring type ball mill and stirring is started, immediately after that, the reaction temperature rises temporarily temporarily and then changes at a constant temperature level. At this stage, the multi-layer structure of the raw material mixed powder proceeds while the pulverization and re-pressing are stably repeated by the milling action by stirring. When the multilayer structure reaches the criticality, the reaction proceeds at a stable temperature once the reaction temperature rises rapidly. At this stage, the raw material powder is converted into an amorphous TiAl-based powder. When the amorphization is completed, the temperature drops sharply and the reaction ends.
【００１２】上記の２段階の過程は、反応器を強制冷却
して反応過程の温度水準を安定的に１５０℃以下に保持
することにより、結晶性の金属間化合物の生成を伴わず
に正常なアモルファス化を進行させることができる。さ
らに、処理前に攪拌型ボールミルの内部を予めＴｉ粉、
Ａｌ粉またはＴｉＡｌ系粉末などでコーティングしてお
くと、前記の２段階反応が一層円滑に進行し、同時に不
純物の混入汚染が防止されて短時間内に高品位のアモル
ファスＴｉＡｌ系粉末を効率的に製造することが可能と
なる。In the above two-stage process, the reactor is forcedly cooled to stably maintain the temperature level of the reaction process at 150 ° C. or less, so that the normal level can be obtained without the formation of crystalline intermetallic compounds. Amorphization can proceed. Further, before the treatment, the inside of the stirring type ball mill is
By coating with Al powder or TiAl-based powder or the like, the two-step reaction proceeds more smoothly, and at the same time, contamination of impurities is prevented, and high-quality amorphous TiAl-based powder can be efficiently produced within a short time. It can be manufactured.
【００１３】[0013]
【実施例】以下、本発明を実施例に基づいて説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to embodiments.
【００１４】参考例１ 水冷ジャケットと温度計測装置を備える攪拌型ボールミ
ルの反応器に水を充填し、鋼球とともに２５０rpm の回
転攪拌を１時間おこなって清浄化したのち、十分に乾燥
して内部の水分を完全に除去した。反応器の内部をＡｒ
ガス雰囲気で置換保持し、これに粒径４５μm 以下のＴ
ｉ粉とＡｌ粉を原子比１：１の割合で混合した原料粉末
５００g を素早く投入した。ついで、５℃に温度調整さ
れた冷却水を水冷ジャケットに一定流量で供給し、反応
温度が１００℃を越えないように制御しながら攪拌回転
数２５０rpm でメカニカルアロイングをおこなった。反
応器内の温度は図１のように経時変動しており、反応が
多層構造化を経て固相アモルファス化していることが認
められたが、反応の完結までには約５２時間を要した。
なお、この参考例１は図１〜図３においては、「実施例
１」で表記した。 REFERENCE EXAMPLE 1 Water was charged into a reactor of a stirring-type ball mill equipped with a water-cooling jacket and a temperature measuring device, and was rotated and stirred with steel balls at 250 rpm for 1 hour. Water was completely removed. Ar inside the reactor
Substitution is maintained in a gas atmosphere.
500 g of raw material powder obtained by mixing i powder and Al powder at an atomic ratio of 1: 1 was quickly charged. Next, cooling water whose temperature was adjusted to 5 ° C. was supplied to the water cooling jacket at a constant flow rate, and mechanical alloying was performed at a stirring rotation speed of 250 rpm while controlling the reaction temperature so as not to exceed 100 ° C. The temperature in the reactor fluctuated with time as shown in FIG. 1, and it was confirmed that the reaction had become a solid-phase amorphous through a multi-layer structure, but it took about 52 hours to complete the reaction.
Note that this reference example 1 is shown in FIGS.
1 ".
【００１５】得られた粉末は、Ｔｉ６４．０重量％、Ａ
ｌ３３．７重量％の組成をもつアモルファスＴｉＡｌ粉
末であったが、不純物としてＦｅが１．２３重量％含有
されていた。図２にこのアモルファスＴｉＡｌ粉末を示
差走査型熱量計(DSC) で測定した熱分析曲線を示した。
この曲線からアモルファス相に若干の濃度勾配がみられ
るものの、全体としてアモルファス構造を呈しているこ
とが認められる。図３はこのアモルファスＴｉＡｌ粉末
のＸ線回折パターンを示したものであるが、アモルファ
ス特有のハーロパターンを呈していることが判る。The obtained powder was composed of 64.0% by weight of Ti,
The amorphous TiAl powder had a composition of 133.7% by weight, but contained 1.23% by weight of Fe as an impurity. FIG. 2 shows a thermal analysis curve of the amorphous TiAl powder measured by a differential scanning calorimeter (DSC).
From this curve, although a slight concentration gradient is observed in the amorphous phase, it is recognized that the amorphous phase as a whole exhibits an amorphous structure. FIG. 3 shows the X-ray diffraction pattern of the amorphous TiAl powder, and it can be seen that the amorphous TiAl powder has a halo pattern unique to amorphous.
【００１６】実施例１ 参考 例１と同一構造の攪拌型ボールミルの反応器を用
い、参考例１と同様に水洗乾燥し、内部をＡｒガスで置
換したのちアモルファスＴｉＡｌ粉末（ＴｉとＡｌの原
子比１：１）１００g を投入して鋼球とともに攪拌回転
数２５０rpm 、攪拌時間１時間の条件で攪拌処理を施
し、予め反応器の内部にアモルファスＴｉＡｌのコーテ
ィング層を形成した。次に反応器から、コーティングに
用いた残りのアモルファスＴｉＡｌ粉末を抜き出したの
ちに、この反応器に参考例１と同一のＴｉ粉とＡｌ粉の
混合粉末５００g を入れ、同一の条件によりメカニカル
アロイング処理をおこなった。この場合の反応器内温度
は図１のように経時変動しており、均一な多層構造化の
段階を介して固相アモルファス化に変態していることが
認められた。とくに反応が約２８時間で完了しており、
参考例１と比べて著しく短時間内に反応が終了した。[0016] Using the reactor stirring ball mill in Example 1 Reference Example 1 and the same structure, and washed with water and dried in the same manner as in Reference Example 1, the atomic ratio of the amorphous TiAl powder (Ti and Al after the internal was replaced with Ar gas 1: 1) 100 g was added thereto, and a stirring treatment was performed together with a steel ball under the conditions of a stirring rotation speed of 250 rpm and a stirring time of 1 hour, and an amorphous TiAl coating layer was previously formed inside the reactor. Next, after extracting the remaining amorphous TiAl powder used for coating from the reactor, 500 g of the same mixed powder of Ti powder and Al powder as in Reference Example 1 was put into this reactor, and mechanical alloying was performed under the same conditions. Processed. In this case, the temperature in the reactor fluctuated with time as shown in FIG. 1, and it was confirmed that the reactor was transformed into a solid-phase amorphous state through a uniform multilayer structure stage. In particular, the reaction was completed in about 28 hours,
The reaction was completed within a very short time as compared with Reference Example 1.
【００１７】得られた粉末は、Ｔｉ６３．４重量％、Ａ
ｌ３５．７重量％の組成もつアモルファスＴｉＡｌ粉末
であり、Ｆｅ含有量は０．１５重量％と参考例１のアモ
ルファス粉末に比べて高純度であった。また、図２の熱
分析曲線により極めて均一性に優れていることも確認さ
れた。図３はこのアモルファスＴｉＡｌ粉末のＸ線回折
パターンを示したものであるが、参考例１よりも更に好
ましい滑らかなパターンを呈していることが判る。The obtained powder was composed of 63.4% by weight of Ti,
The amorphous TiAl powder had a composition of 135.7% by weight, and the Fe content was 0.15% by weight, which was higher than that of the amorphous powder of Reference Example 1. Further, it was confirmed from the thermal analysis curve of FIG. 2 that the uniformity was extremely excellent. FIG. 3 shows the X-ray diffraction pattern of this amorphous TiAl powder. It can be seen that the amorphous TiAl powder has a smoother pattern than that of Reference Example 1.
【００１８】[0018]
【発明の効果】以上のとおり、本発明に従えばメカニカ
ルアロイング処理により高品質のアモルファスＴｉＡｌ
系粉末を効率よく製造することができる。したがって、
応用範囲の広いＴｉＡｌ系のアモルファス粉末を工業的
に製造する手段として有用性が期待できる。As described above, according to the present invention, high quality amorphous TiAl can be obtained by mechanical alloying.
The system powder can be manufactured efficiently. Therefore,
It is expected to be useful as a means for industrially producing TiAl-based amorphous powder having a wide range of applications.
【図１】実施例における反応時間と反応器内の温度との
関係を示したグラフである。FIG. 1 is a graph showing a relationship between a reaction time and a temperature in a reactor in Examples.
【図２】実施例で得られたアモルファスＴｉＡ粉末の示
差走査熱量計(DSC) による熱分析曲線を示したグラフで
ある。FIG. 2 is a graph showing a thermal analysis curve by a differential scanning calorimeter (DSC) of the amorphous TiO powder obtained in the example.
【図３】実施例で得られたアモルファスＴｉＡｌ粉末に
ついて測定されたＸ線回折パターンである。FIG. 3 is an X-ray diffraction pattern measured for an amorphous TiAl powder obtained in an example.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 籠橋 亘 神奈川県茅ヶ崎市茅ヶ崎３−３−５ 東 邦チタニウム株式会社茅ヶ崎工場内 (56)参考文献 特開 平２−263902（ＪＰ，Ａ) 特開 平４−83883（ＪＰ，Ａ) 特開 平４−331（ＪＰ，Ａ) 特開 平１−215903（ＪＰ，Ａ) 社団法人粉末冶金技術協会 編，粉末 冶金技術講座３ 金属粉の生成，日本, 日刊工業新聞社，1964年９月25日，Ｐ. 32−33 (58)調査した分野(Int.Cl.7，ＤＢ名) C22C 1/00 - 1/04 ──────────────────────────────────────────────────続 き Continuation of front page (72) Wataru Kagohashi 3-3-5 Chigasaki, Chigasaki-shi, Kanagawa Prefecture Inside the Chigasaki Plant of Toho Titanium Co., Ltd. (56) References JP-A-2-263902 (JP, A) JP-A-4-83883 (JP, A) JP-A-4-331 (JP, A) JP-A-1-215903 (JP, A) Powder metallurgy technology association 3 Japan, Nikkan Kogyo Shimbun, September 25, 1964, pp. 32-33 (58) Fields investigated (Int. Cl. 7 , DB name) C22C 1/00-1/04
Claims (1)
保たれた攪拌型ボールミルの反応器によりメカニカルア
ロイングするにあたり、メカニカルアロイングの処理前
に、前記反応器となる攪拌型ボールミルの内部を、予め
Ｔｉ粉、Ａｌ粉またはＴｉＡｌ系粉末の単独または混合
物によりコーティングし、温度６０〜８０℃の範囲にお
いてＴｉとＡｌの多層構造化を行わせる多層構造化の過
程と、該多層構造化の過程後に行われる、反応温度の急
激な上昇を経て、温度８０℃を越え、１５０℃以下の範
囲において固相アモルファス変態を行わせる固相アモル
ファス変態の過程との２段階の過程を、攪拌型ボールミ
ルの攪拌回転数を３００ｒｐｍ以下に設定するととも
に、反応器に供給する冷却水を用いて反応器を強制冷却
して、該２段階の過程における反応温度を制御すること
により、行うことを特徴とするアモルファスＴｉＡｌ系
粉末の製造方法。1. When mechanically alloying a mixed powder of Ti and Al by a reactor of a stirring type ball mill maintained in an inert atmosphere, before mechanical alloying treatment is performed.
In advance, the interior of the stirring ball mill serving as the reactor,
Ti powder, Al powder or TiAl powder alone or mixed
Coated with an object, over the multi-layer structured to Ru to perform the multi-layer structure of Ti and Al in a range of temperatures 60-80 ° C.
Degree and, performed after the process of the multilayer structured, through a rapid increase in the reaction temperature, exceeding the temperature 80 ° C., solid Cupid to perform solid phase amorphous transformation in the range of 0.99 ° C. or less
The two-step process, which is the process of fass transformation,
And set the stirring speed of the
The reactor is forcibly cooled using cooling water supplied to the reactor
Controlling the reaction temperature in the two-step process
A method for producing an amorphous TiAl-based powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19145892A JP3279346B2 (en) | 1992-06-25 | 1992-06-25 | Method for producing amorphous TiAl-based powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19145892A JP3279346B2 (en) | 1992-06-25 | 1992-06-25 | Method for producing amorphous TiAl-based powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0610076A JPH0610076A (en) | 1994-01-18 |
| JP3279346B2 true JP3279346B2 (en) | 2002-04-30 |
Family
ID=16274978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19145892A Expired - Fee Related JP3279346B2 (en) | 1992-06-25 | 1992-06-25 | Method for producing amorphous TiAl-based powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3279346B2 (en) |
-
1992
- 1992-06-25 JP JP19145892A patent/JP3279346B2/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 社団法人粉末冶金技術協会 編，粉末冶金技術講座３ 金属粉の生成，日本，日刊工業新聞社，１９６４年９月２５日，Ｐ．３２−３３ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0610076A (en) | 1994-01-18 |
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