JPH08170110A - High melting point metal-based alloy powder and production of high melting point metal-based alloy compact - Google Patents
High melting point metal-based alloy powder and production of high melting point metal-based alloy compactInfo
- Publication number
- JPH08170110A JPH08170110A JP7110649A JP11064995A JPH08170110A JP H08170110 A JPH08170110 A JP H08170110A JP 7110649 A JP7110649 A JP 7110649A JP 11064995 A JP11064995 A JP 11064995A JP H08170110 A JPH08170110 A JP H08170110A
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- Prior art keywords
- based alloy
- powder
- refractory metal
- metal
- producing
- Prior art date
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Links
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 90
- 239000000956 alloy Substances 0.000 title claims abstract description 90
- 239000000843 powder Substances 0.000 title claims abstract description 77
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 27
- 239000002184 metal Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 238000002844 melting Methods 0.000 title description 10
- 230000008018 melting Effects 0.000 title description 10
- 239000002245 particle Substances 0.000 claims description 43
- 239000003870 refractory metal Substances 0.000 claims description 39
- 239000002994 raw material Substances 0.000 claims description 21
- 239000011812 mixed powder Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000005275 alloying Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000001513 hot isostatic pressing Methods 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 7
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 description 22
- 238000000034 method Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 12
- 238000005469 granulation Methods 0.000 description 7
- 230000003179 granulation Effects 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910000881 Cu alloy Inorganic materials 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000009863 impact test Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000009864 tensile test Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000012768 molten material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910017315 Mo—Cu Inorganic materials 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229910003267 Ni-Co Inorganic materials 0.000 description 1
- 229910018054 Ni-Cu Inorganic materials 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 229910003262 Ni‐Co Inorganic materials 0.000 description 1
- 229910018106 Ni—C Inorganic materials 0.000 description 1
- 229910018481 Ni—Cu Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000011361 granulated particle Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高融点金属基合金体の
製造方法と、それに使用する高融点金属基合金粉末の製
造方法とに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a refractory metal-based alloy body and a method for producing a refractory metal-based alloy powder used therein.
【０００２】[0002]
【従来の技術】従来、ＬＳＩのヒートシンク台としてＷ
−Ｃｕ合金が用いられたり、高エネルギー弾体としてＷ
−Ｎｉ−Ｆｅ合金が、さく孔工具用としてＷ−Ｎｉ−Ｃ
ｕ合金が用いられるなど、Ｗ基合金体が各種用途に用い
られている。2. Description of the Related Art Conventionally, W has been used as a heat sink base for LSI.
-Cu alloy is used, or W is used as a high energy bullet
-Ni-Fe alloy is W-Ni-C for drilling tools
W-based alloy bodies are used for various purposes, such as u alloys.
【０００３】こうしたＷ基合金体は、Ｗの粉末と他の金
属又は合金（例えば、Ｃｕ，Ｎｉ，Ｆｅ，Ｃｏ，Ｎｉ−
Ｆｅ，Ｎｉ−Ｃｕ，Ｎｉ−Ｃｏ等）の粉末とを混合し、
プレス成形後、固相焼結又は液相焼結したり、あるいは
前記混合・焼結後にカプセルに封入して熱間静水圧にて
加圧焼結するなどの方法により製造されていた。あるい
は、Ｗ−Ｃｕ合金の場合には、Ｗ粉末を焼結後にＣｕを
含浸させる方法もあった。Such W-based alloy bodies are composed of W powder and other metals or alloys (for example, Cu, Ni, Fe, Co, Ni--).
Fe, Ni-Cu, Ni-Co, etc. powder,
After press molding, solid-phase sintering or liquid-phase sintering was performed, or after the mixing / sintering, the mixture was encapsulated and pressed under hot isostatic pressure for pressure sintering. Alternatively, in the case of W-Cu alloy, there is also a method of impregnating Cu after sintering W powder.
【０００４】また、高融点金属基合金体としては、他
に、ヒートシンクとしてのＭｏ−Ｃｕ合金、ターゲット
材としてのＷ−Ｔｉ合金、接点材料としてのＷ−Ａｇ合
金、電極材料としてのＷ−Ｃｕ合金なども知られてお
り、これらも上記のような製法によっていた。Further, as the refractory metal-based alloy body, in addition, a Mo-Cu alloy as a heat sink, a W-Ti alloy as a target material, a W-Ag alloy as a contact material, and a W-Cu as an electrode material. Alloys and the like are also known, and these were also manufactured by the above-described manufacturing method.
【０００５】[0005]
【発明が解決しようとする課題】しかし、この様な従来
の製造方法による高融点金属基合金体は、機械的性質、
特に靱性が不足し、性能的に十分とはいえなかった。そ
こで、本発明は、機械的性質、特に靱性が十分である高
融点金属基合金体及びその原料となる高融点金属基合金
粉末を提供することを目的とする。However, the refractory metal-based alloy body produced by such a conventional manufacturing method has the following mechanical properties:
In particular, the toughness was insufficient and the performance was not sufficient. Therefore, an object of the present invention is to provide a refractory metal-based alloy powder having sufficient mechanical properties, particularly toughness, and a refractory metal-based alloy powder as a raw material thereof.
【０００６】[0006]
【課題を解決するための手段】本発明の高融点金属基合
金粉末の製造方法は、高融点金属の粉末とその他の金属
又は合金の粉末とを混合し、該混合粉末を所定の粒径に
造粒した後、該造粒粉末粒子を少なくとも当該粒子内で
溶融体又は半溶融体を形成するまで加熱した後に、急速
に凝固せしめ、必要に応じて粉砕工程を経た後に所定の
粒度に分級することを特徴とする。The method for producing a refractory metal-based alloy powder according to the present invention comprises mixing a refractory metal powder with another metal or alloy powder and bringing the mixed powder to a predetermined particle size. After granulating, the granulated powder particles are heated at least until a melt or a semi-molten body is formed in the particles, and then rapidly solidified, and if necessary, subjected to a pulverizing step and then classified to a predetermined particle size. It is characterized by
【０００７】ここで、混合粉末粒子内で溶融体又は半溶
融体を形成するまで加熱し、急速に凝固させる実用的方
法としては、造粒粉末粒子を溶接材料としてアーク加熱
による粉体肉盛溶接でビードを水冷床に形成する方法
や、混合粉末粒子を溶解材料としてアーク溶解又はプラ
ズマアーク溶解をし、これを水冷炉床に堆積させつつ凝
固させる方法や、高周波プラズマにて超高温層を形成し
ておき、ここに造粒粉末粒子を通過させ、パーティクル
・トゥー・パーティクルにて溶融・凝固させる方法（造
粒粒子を粒子の形態のまま一旦溶融させ、そのまま粒子
の状態に凝固させる方法）などを採用するとよい。Here, as a practical method of heating the mixed powder particles until a molten material or a semi-molten material is formed and rapidly solidifying, a powder overlay welding by arc heating using granulated powder particles as a welding material. To form a bead on a water-cooled bed, a method of arc melting or plasma arc melting using mixed powder particles as a melting material, and solidifying this while depositing it on a water-cooled hearth, or forming an ultra-high temperature layer by high-frequency plasma Then, the granulated powder particles are passed through here, and the particles are melted and solidified by particle-to-particle (the granulated particles are once melted in the form of particles and then solidified into the particle state). Should be adopted.
【０００８】また、必要に応じて粉砕すればよいのは、
最終的な粒度に調整された造粒粉末をパーティクル・ト
ゥー・パーティクルで溶融・凝固する場合には粉砕は不
要となるからである。さらに、造粒の方法としては、プ
レス造粒を行うことにすれば、造粒に当たってバインダ
を必要としないので、複合粉末自体の性能に酸素や炭素
等の混入による悪影響を生じさせることがない点でも望
ましい。[0008] Further, it is only necessary to grind if necessary.
This is because crushing is not necessary when the granulated powder adjusted to the final particle size is melted and solidified with particles to particles. Further, as a method of granulation, if press granulation is performed, a binder is not required for granulation, so that the performance of the composite powder itself is not adversely affected by the inclusion of oxygen, carbon, or the like. But desirable.
【０００９】なお、本発明に用いる高融点金属として
は、Ｗ，Ｍｏ，Ｔａ，Ｎｂ，Ｚｒ，Ｔｉ，Ｉｒ，Ｐｔ，
Ｈｆ，Ｃｒ等を挙げることができる。また、前記造粒粉
末は、真空、アルゴンまたは水素雰囲気中で焼結された
後に溶融されることが望ましい。これは、粉末の造粒時
に空気中の酸素や窒素が混入するのを防ぐためである。
酸素が混入することによる耐摩耗性の低下や、窒素が混
入することによる脆化を防止するためである。これはま
た粉砕工程についてもいえ、前記粉砕工程は、真空、ア
ルゴンまたは水素雰囲気中で行われることが望ましい。
混合についても同様である。The refractory metals used in the present invention include W, Mo, Ta, Nb, Zr, Ti, Ir, Pt,
Hf, Cr, etc. can be mentioned. Further, it is preferable that the granulated powder is melted after being sintered in a vacuum, argon or hydrogen atmosphere. This is to prevent oxygen and nitrogen in the air from being mixed during granulation of the powder.
This is to prevent deterioration of wear resistance due to the inclusion of oxygen and embrittlement due to the inclusion of nitrogen. This also applies to the grinding process, which is preferably carried out in a vacuum, argon or hydrogen atmosphere.
The same applies to mixing.
【００１０】さらに、前記粉砕工程の前に、焼鈍または
焼鈍と急冷処理を施すことが望ましい。これは、焼鈍を
施すことにより、その後の粉砕工程での工数節減が可能
となるからである。上記の様な本発明方法によって製造
される高融点金属基合金粉末は、高融点金属とその他の
金属とを均一分散状態に合金化させたものとなる。即
ち、高融点金属と他の金属とが、高温加熱状態で液相−
液相又は固相−液相で分散・混合し、そのままの分散・
混合状態で固化した状態となっているのである。Furthermore, it is desirable to perform annealing or annealing and quenching treatment before the crushing step. This is because annealing makes it possible to reduce the number of steps in the subsequent crushing step. The refractory metal-based alloy powder produced by the method of the present invention as described above is obtained by alloying the refractory metal and other metals in a uniformly dispersed state. That is, the refractory metal and the other metal are in liquid phase under high temperature heating.
Disperse and mix in liquid phase or solid-liquid phase, and
It is in a solidified state in the mixed state.
【００１１】一方、本発明の高融点金属基合金体の製造
方法は、高融点金属とその他の金属とを均一分散状態に
合金化させた粉末を原料として、熱間静水圧プレス（以
下、「ＨＩＰ」という）にて加圧焼結することを特徴と
する。この場合、上述した本発明の高融点金属基合金粉
末の製造方法によって製造された粉末を原料として、Ｈ
ＩＰにて加圧焼結するようにするとよい。また、前記Ｈ
ＩＰは、高融点金属基合金の液相線温度以下の所定温度
下で実行するようにするとよい。これは、液相線温度以
上でＨＩＰを行うとすると、高融点金属リッチ相と他相
との間に重力偏析が発生し、分散の均一性が損なわれる
という不具合があるからである。On the other hand, in the method for producing a refractory metal-based alloy body of the present invention, a powder obtained by alloying a refractory metal and another metal in a uniformly dispersed state is used as a raw material, and hot isostatic pressing (hereinafter referred to as " It is characterized by performing pressure sintering with "HIP"). In this case, the powder produced by the above-mentioned method for producing a refractory metal-based alloy powder of the present invention is used as a raw material, and H
It is preferable to perform pressure sintering with IP. Also, the above H
The IP may be performed at a predetermined temperature equal to or lower than the liquidus temperature of the refractory metal-based alloy. This is because if HIP is performed at a liquidus temperature or higher, gravity segregation occurs between the refractory metal-rich phase and the other phase, and the uniformity of dispersion is impaired.
【００１２】[0012]
【作用及び効果】本発明の高融点金属基合金体の製造方
法によれば、予め合金化した粉末をＨＩＰで焼結・固化
するので、粉末の再配列が行われると同時に、メタルの
塑性流動が起こって「ち密化」した合金相が微細に分散
した組織の高融点金属基合金体を容易に得ることができ
る。According to the method for producing a refractory metal-based alloy body of the present invention, the pre-alloyed powder is sintered and solidified by HIP, so that the powder is rearranged and at the same time the plastic flow of the metal is performed. It is possible to easily obtain a refractory metal-based alloy body having a structure in which the "dense" alloy phase is finely dispersed due to the occurrence of the above.
【００１３】ここで、本発明方法と従来方法との違い
を、Ｗ−Ｃｕ合金体の例について模式図を用いて説明す
ると、図１の様になる。本発明方法により製造されるＷ
−Ｃｕ合金体は、各粉末自体がＷ粒子とＣｕ粒子とが均
一分散状態に合金化されたものであり、しかもＨＩＰに
より加圧下で焼結・固化されるので、図１（Ａ）に示す
ように、焼結体全体として「均質でち密化」した組織と
なるのである。これに対し、従来の方法（粉末を混合し
てプレスした後に焼結する方法）では、同図（Ｂ）に示
すように、Ｗ粒子の隙間にＣｕが溶け込むと同時に、Ｗ
とＣｕ間で合金化して焼結が進行するが、両者の融点差
と低溶解度のため、高靱性の焼結体を得るのが困難であ
った。Here, the difference between the method of the present invention and the conventional method will be described with reference to a schematic view of an example of a W--Cu alloy body as shown in FIG. W produced by the method of the present invention
The —Cu alloy body is shown in FIG. 1A because each powder itself is an alloy in which W particles and Cu particles are uniformly dispersed and is sintered and solidified under pressure by HIP. Thus, the entire sintered body has a "homogeneous and densified" structure. On the other hand, in the conventional method (method of mixing powders, pressing and then sintering), as shown in FIG. 6B, Cu melts in the gaps of W particles and, at the same time, W
And Cu are alloyed and sintering proceeds, but it was difficult to obtain a sintered body having high toughness due to the difference in melting point and low solubility between the two.
【００１４】こうした差により、本発明方法により製造
した高融点金属基合金体は、従来のプレス焼結法により
製造した合金体に比べて、その機械的性質の内、特に、
靱性が高いものとなる。そして、本発明の高融点金属基
合金粉末の製造方法によれば、このような高靱性の高融
点金属基合金体を容易に製造せしめることができる。Due to such a difference, the refractory metal-based alloy body produced by the method of the present invention has a mechanical property, in particular, of the mechanical properties as compared with the alloy body produced by the conventional press sintering method.
High toughness. Further, according to the method for producing a refractory metal-based alloy powder of the present invention, such a toughness refractory metal-based alloy body can be easily produced.
【００１５】即ち、本発明方法としての高融点金属基合
金体の製造方法では、高融点金属と他の金属とが均一分
散状態に合金化されていればよいのであるから、例え
ば、メカニカル・アロイイングによって原料粉末を製造
することも可能である。しかし、メカニカル・アロイイ
ングではその処理に時間がかかる。従って、本発明によ
る高融点金属基合金粉末の製造方法を用いるなら、高融
点金属基合金体の原料粉末を容易に製造できるという効
果があるのである。That is, in the method for producing a refractory metal-based alloy body as the method of the present invention, it is sufficient that the refractory metal and the other metal are alloyed in a uniformly dispersed state. Therefore, for example, mechanical alloying is used. It is also possible to manufacture the raw material powder by. However, in mechanical alloying, the processing takes time. Therefore, if the method for producing a refractory metal-based alloy powder according to the present invention is used, the raw material powder for a refractory metal-based alloy body can be easily produced.
【００１６】[0016]
【実施例】次に、本発明を一層明らかにするために、好
適な実施例を説明する。 ［第１実施例］まず、Ｗ基合金体について説明する。Next, preferred examples will be described in order to further clarify the present invention. [First Embodiment] First, a W-based alloy body will be described.
【００１７】Ｗ基合金体の原料となるＷ及び他の金属と
を均一分散状態に合金化させた原料粉末は、以下の工程
により製造される。まず最初に、用途に応じてＷ粉末及
びその他の金属の粉末を選定する。他の金属としては、
通常は、Ｗに対して低融点金属が選択されることにな
る。次に、Ｗ粉末（粒径０．１〜３μｍ）とその他の金
属の粉末（粒径１〜１０μｍ）とを混合して原料の配合
・調整をする（：原料配合）。A raw material powder obtained by alloying W as a raw material of a W-based alloy body and another metal in a uniformly dispersed state is manufactured by the following steps. First, W powder and other metal powders are selected according to the application. Other metals include
Normally, a low melting point metal will be selected for W. Next, W powder (particle size 0.1 to 3 μm) and other metal powder (particle size 1 to 10 μm) are mixed to mix and adjust the raw materials (: raw material mixing).
【００１８】そして、この原料混合物を混合撹拌機にお
いて均質な混合状態になる様に混合する（：混合撹
拌）。この混合撹拌は、Ａｒ雰囲気中で行う。混合物が
混合撹拌機にて均質な混合状態となったら、これをプレ
ス造粒機にかけて造粒し、さらに焼結・粉砕・分級し、
所定粒度（粒径３〜８ｍｍ）の粉末に調整する（：プ
レス造粒・焼結）。この焼結は、真空雰囲気中で行う。Then, the raw material mixture is mixed in a mixing stirrer so as to be in a homogeneous mixed state (: mixing and stirring). This mixing and stirring is performed in an Ar atmosphere. When the mixture becomes a homogeneous mixed state with a mixing stirrer, it is granulated by a press granulator, and further sintered, crushed and classified,
The powder is adjusted to a predetermined particle size (particle size 3 to 8 mm) (: press granulation / sintering). This sintering is performed in a vacuum atmosphere.
【００１９】こうして所定粒度に調整された混合粉末粒
子を得たら、これを用いてプラズマ積層凝固炉（ＰＰＣ
炉）にて溶融・凝固させる（：溶融・凝固）。ここ
で、溶融・凝固の工程についてもう少し詳しく説明する
と、上記混合粉末粒子をプラズマアークによる超高温で
急速溶解をした後、冷却炉床上に堆積させつつ急速に凝
固させることにより、Ｗとその他の金属とを溶体化し、
互いに均一に分散した状態のＷ基合金粉末の溶融化堆積
物を製造するのである。具体的には、約１００００℃の
プラズマアークに対して、混合粉末粒子を２００ｇ／分
の速度で給送する。When mixed powder particles adjusted to a predetermined particle size are obtained in this manner, the mixed powder particles are used to form a plasma layered solidification furnace (PPC).
Melt and solidify in a furnace (: Melt and solidify). Here, the melting and solidifying process will be described in a little more detail. After the mixed powder particles are rapidly melted at an ultrahigh temperature by a plasma arc, they are rapidly solidified while being deposited on the cooling hearth, so that W and other metals are And are solidified,
A molten deposit of W-based alloy powder in a state of being uniformly dispersed in each other is produced. Specifically, the mixed powder particles are fed at a rate of 200 g / min with respect to a plasma arc of about 10,000 ° C.
【００２０】こうしてできた合金粉末の溶融化堆積物を
Ａｒ雰囲気下においてボールミルで粉砕し（：粉
砕）、振動分級機又は気流分級機にかけてＨＩＰ原料と
して使用するのに適した粒度（７５μｍ以下）の合金粉
末に分級する（：分級）。こうしてＷとその他の金属
とが均一分散状態で溶体化した所定粒度のＷ基合金粉末
が製造できたら、これを原料としてＨＩＰ（１４００
℃，１２００ｋｇｆ／ｃｍ2 ，１８０分）にかけ、方向
性のない「ち密」な組織のＷ基合金体を製造する。この
とき、ＨＩＰ温度は、原料粉末としてのＷ基合金の液相
線温度以下の温度としている。The molten deposit of the alloy powder thus obtained is crushed (: crushed) with a ball mill in an Ar atmosphere and subjected to a vibration classifier or an airflow classifier to have a particle size (75 μm or less) suitable for use as a HIP raw material. Classify into alloy powder (: classification). In this way, when W-based alloy powder having a predetermined particle size in which W and other metals are solution-dissolved in a uniformly dispersed state can be produced, HIP (1400
C., 1200 kgf / cm 2 , 180 minutes) to produce a W-based alloy body having a “dense” structure with no orientation. At this time, the HIP temperature is set to a temperature not higher than the liquidus temperature of the W-based alloy as the raw material powder.
【００２１】一方、比較例として、次の様な方法により
Ｗ基合金体を製造する。まず、Ｗ粉末及びその他の金属
の粉末を選定し、これらをＶブレンダーにて均質な混合
状態になる様に混合し、プレス成形機にかけて所定形状
に成形する。プレス成形圧は、５トン／ｃｍ2 とした。
こうして得られた成形体を、焼結炉にて１５００℃×６
０分間、水素気流中で焼結を行い、５０℃／分の速度で
炉冷した。On the other hand, as a comparative example, a W-based alloy body is manufactured by the following method. First, W powder and other metal powders are selected, mixed with a V blender so as to be in a homogeneous mixed state, and molded into a predetermined shape by a press molding machine. The press molding pressure was 5 ton / cm 2 .
The molded body thus obtained is 1500 ° C. × 6 in a sintering furnace.
Sintering was performed in a hydrogen stream for 0 minutes, and furnace cooling was performed at a rate of 50 ° C./minute.
【００２２】こうして製造した実施例及び比較例のＷ基
合金体を硬さ試験、引っ張り試験、衝撃試験のそれぞれ
様に加工し、特性を調べた。この結果を、表に示す。The W-based alloy bodies of Examples and Comparative Examples thus manufactured were processed by a hardness test, a tensile test and an impact test, respectively, and their properties were examined. The results are shown in the table.
【００２３】[0023]
【表１】 [Table 1]
【００２４】表から明かな様に、実施例により製造した
Ｗ基合金体と比較例により製造したＷ基合金体は、硬さ
及び引張強さに関してはほぼ同じ特性となったが、伸び
及び衝撃値において著しい差異が認められることが分か
る。即ち、実施例により製造されたＷ基合金体は、比較
例に比べて著しく靱性が向上することが分かる。As is apparent from the table, the W-based alloy bodies produced in the examples and the W-based alloy bodies produced in the comparative examples have almost the same characteristics in hardness and tensile strength, but elongation and impact It can be seen that there are significant differences in the values. That is, it can be seen that the W-based alloy bodies produced in the examples have significantly improved toughness as compared with the comparative examples.
【００２５】なお、上記のＷ基合金体は、例えば、熱間
加工具の台金などの用途に適している。 ［第２実施例］次に、Ｍｏ基合金体について説明する。The W-based alloy body described above is suitable for use as a base metal of a hot working tool, for example. [Second Embodiment] Next, a Mo-based alloy body will be described.
【００２６】Ｍｏ基合金体の原料となる原料粉末も、Ｗ
基合金体について説明したの第１実施例と同様の工程に
より製造される。このとき、：原料配合の工程におい
ては、Ｍｏ粉末としては粒径１〜３μｍのものを、その
他の金属の粉末としては粒径１〜３μｍのものを使用す
る。：プレス造粒・焼結では、粒径３〜８ｍｍの粉末
に造粒・焼結・分級する。：溶融・凝固においては、
約１００００℃のプラズマアークに対して、混合粉末粒
子を２００ｇ／分の速度で給送する。そして、：粉砕
及び：分級により、最終的に、粒径７５μｍ以下の合
金粉末とする。The raw material powder used as the raw material for the Mo-based alloy is also W
It is manufactured by the same process as the first embodiment described for the base alloy body. At this time, in the step of blending the raw materials, Mo powder having a particle size of 1 to 3 μm and other metal powder having a particle size of 1 to 3 μm are used. : In the press granulation / sintering, the powder having a particle size of 3 to 8 mm is granulated / sintered / classified. : In melting and solidification,
The mixed powder particles are fed at a rate of 200 g / min for a plasma arc of about 10000C. Then, by: crushing and: classification, an alloy powder having a particle diameter of 75 μm or less is finally obtained.
【００２７】こうして所定粒度のＭｏ基合金粉末が製造
できたら、これを原料としてＨＩＰ（１４００℃，１２
００ｋｇｆ／ｃｍ2 ，１８０分）にかけ、方向性のない
「ち密」な組織のＭｏ基合金体を製造する。このとき、
ＨＩＰ温度は、原料粉末としてのＭｏ基合金の液相線温
度以下の温度としている。When the Mo-based alloy powder having a predetermined grain size is manufactured in this manner, HIP (1400 ° C., 12
(100 kgf / cm 2 , 180 minutes) to produce a Mo-based alloy body having a “dense” structure with no orientation. At this time,
The HIP temperature is set to a temperature equal to or lower than the liquidus temperature of the Mo-based alloy as the raw material powder.
【００２８】一方、比較例は、第１実施例と同様に、プ
レス成形・焼結により製造する。このときのプレス成形
圧は、５トン／ｃｍ2 、焼結の条件は、１４５０℃×６
０分間、真空雰囲気中で焼結し、３０℃／分の速度で炉
冷している。こうして製造した実施例及び比較例のＭｏ
基合金体を硬さ試験、引っ張り試験、衝撃試験のそれぞ
れ様に加工し、特性を調べた。この結果を、表に示す。On the other hand, the comparative example is manufactured by press molding and sintering as in the first embodiment. The press molding pressure at this time is 5 ton / cm 2 , and the sintering condition is 1450 ° C. × 6.
Sintering is performed in a vacuum atmosphere for 0 minutes, and furnace cooling is performed at a rate of 30 ° C./minute. Mo produced in the above-described examples and comparative examples
The base alloy body was processed by a hardness test, a tensile test, and an impact test, and the characteristics were examined. The results are shown in the table.
【００２９】[0029]
【表２】 [Table 2]
【００３０】表から明かな様に、実施例により製造した
Ｍｏ基合金体と比較例により製造したＭｏ基合金体は、
硬さ及び引張強さに関してはほぼ同じ特性となったが、
伸び及び衝撃値において著しい差異が認められることが
分かる。即ち、実施例により製造されたＭｏ基合金体
は、比較例に比べて著しく靱性が向上することが分か
る。As is apparent from the table, the Mo-based alloy bodies produced according to the examples and the Mo-based alloy bodies produced according to the comparative examples are
The hardness and tensile strength were almost the same, but
It can be seen that there are significant differences in elongation and impact values. That is, it can be seen that the Mo-based alloy bodies produced in the examples have significantly improved toughness as compared with the comparative examples.
【００３１】なお、上記のＭｏ基合金体は、例えば、ヒ
ートシンクなどの用途に適している。 ［第３実施例］次に、Ｔｉ基合金体について説明する。The above Mo-based alloy body is suitable for applications such as heat sinks. [Third Embodiment] Next, a Ti-based alloy body will be described.
【００３２】Ｔｉ基合金体の原料となる原料粉末も、Ｗ
基合金体について説明したの第１実施例と同様の工程に
より製造される。このとき、：原料配合の工程におい
ては、Ｔｉ粉末としては粒径１〜１０μｍのものを、Ｍ
ｏ粉末としては粒径１〜３μｍのものを使用する。：
プレス造粒・焼結では、粒径３〜８ｍｍの粉末に造粒・
焼結・分級する。：溶融・凝固においては、約１００
００℃のプラズマアークに対して、混合粉末粒子を２０
０ｇ／分の速度で給送する。そして、：粉砕及び：
分級により、最終的に、粒径７５μｍ以下の合金粉末と
する。The raw material powder used as the raw material for the Ti-based alloy is also W
It is manufactured by the same process as the first embodiment described for the base alloy body. At this time: In the step of mixing the raw materials, the Ti powder having a particle size of 1 to 10 μm is
o Powder having a particle size of 1 to 3 μm is used. :
In press granulation / sintering, granulate into powder with a particle size of 3-8 mm.
Sinter and classify. : About 100 for melting and solidification
20 powder mixture particles against a plasma arc at 00 ° C
Feed at a rate of 0 g / min. And: crushing and:
Finally, an alloy powder having a particle size of 75 μm or less is obtained by classification.
【００３３】こうして所定粒度のＴｉ基合金粉末が製造
できたら、これを原料としてＨＩＰ（１４００℃，１２
００ｋｇｆ／ｃｍ2 ，１８０分）にかけ、方向性のない
「ち密」な組織のＴｉ基合金体を製造する。このとき、
ＨＩＰ温度は、原料粉末としてのＴｉ基合金の液相線温
度以下の温度としている。When a Ti-based alloy powder having a predetermined grain size can be manufactured in this manner, HIP (1400 ° C., 12
(100 kgf / cm 2 , 180 minutes) to produce a Ti-based alloy body having a “dense” structure with no orientation. At this time,
The HIP temperature is set to a temperature equal to or lower than the liquidus temperature of the Ti-based alloy as the raw material powder.
【００３４】一方、比較例は、第１実施例と同様に、プ
レス成形・焼結により製造する。このときのプレス成形
圧は、５トン／ｃｍ2 、焼結の条件は、１３５０℃×６
０分間、水素気流中で焼結とし、２０℃／分の速度で炉
冷している。こうして製造した実施例及び比較例のＴｉ
基合金体を硬さ試験、引っ張り試験、衝撃試験のそれぞ
れ様に加工し、特性を調べた。この結果を、表に示す。On the other hand, the comparative example is manufactured by press molding and sintering as in the first embodiment. The press molding pressure at this time is 5 ton / cm 2 , and the sintering condition is 1350 ° C. × 6.
Sintering is performed in a hydrogen stream for 0 minutes, and the furnace is cooled at a rate of 20 ° C./minute. Ti of Examples and Comparative Examples thus manufactured
The base alloy body was processed by a hardness test, a tensile test, and an impact test, and the characteristics were examined. The results are shown in the table.
【００３５】[0035]
【表３】 [Table 3]
【００３６】表から明かな様に、実施例により製造した
Ｔｉ基合金体と比較例により製造したＴｉ基合金体は、
硬さ及び引張強さに関してはほぼ同じ特性となったが、
特に衝撃値において差異が認められることが分かる。即
ち、実施例により製造されたＴｉ基合金体は、比較例に
比べて著しく靱性が向上することが分かる。As is apparent from the table, the Ti-based alloy bodies produced in the examples and the Ti-based alloy bodies produced in the comparative examples are
The hardness and tensile strength were almost the same, but
In particular, it can be seen that a difference is recognized in the impact value. That is, it can be seen that the Ti-based alloy bodies manufactured according to the examples have significantly improved toughness as compared with the comparative examples.
【００３７】なお、上記のＴｉ基合金体は、例えば、耐
食材料などの用途に適している。以上いくつかの実施例
を説明してきたが、本発明は、上記の実施例にのみ限ら
れるものではなく、実施例以外のＷ基合金体，Ｍｏ基合
金体，Ｔｉ基合金体はもちろん、Ｔａ基合金体，Ｎｂ基
合金体，Ｚｒ基合金体，Ｃｒ基合金体の製造に適用して
もよいし、さらにその他の高融点金属基合金体の製造に
適用してもよく、最初の合金化した粉末を得る方法も、
ＰＰＣ炉を用いる方法に限らない。The Ti-based alloy body described above is suitable for use as, for example, a corrosion resistant material. Although some embodiments have been described above, the present invention is not limited to the above-mentioned embodiments, and not only the W-based alloy body, the Mo-based alloy body and the Ti-based alloy body other than the embodiments but also the Ta-based alloy body can be used. It may be applied to the production of a base alloy body, an Nb base alloy body, a Zr base alloy body, a Cr base alloy body, or may be applied to the production of other refractory metal base alloy bodies, and the first alloying The method of obtaining powder
The method is not limited to using a PPC furnace.
【００３８】また、粉末自体も、溶射材料などとして使
用して構わず、その場合も高融点金属に対して他の金属
が均一分散状態となっているので、Also, the powder itself may be used as a thermal spraying material, etc., and in that case, since the other metal is uniformly dispersed in the refractory metal,
【図１】 本発明の作用を説明する模式図である。FIG. 1 is a schematic diagram illustrating an operation of the present invention.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成７年５月１０日[Submission date] May 10, 1995
【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】００３８[Correction target item name] 0038
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００３８】また、粉末自体も、溶射材料などとして使
用して構わず、その場合も高融点金属に対して他の金属
が均一分散状態となっている。 Further, the powder itself, without regard to use as such as the spray material, the case that have been other metals and uniformly dispersed state with respect to the refractory metal.
Claims (7)
金の粉末とを混合し、該混合粉末を所定の粒径に造粒し
た後、該造粒粉末粒子を少なくとも当該粒子内で溶融体
又は半溶融体を形成するまで加熱した後に、急速に凝固
せしめ、必要に応じて粉砕工程を経た後に所定の粒度に
分級することを特徴とする高融点金属基合金粉末の製造
方法。1. A powder of a refractory metal and a powder of another metal or alloy are mixed, the mixed powder is granulated to a predetermined particle size, and the granulated powder particles are melted at least in the particles. Alternatively, a method for producing a high-melting-point metal-based alloy powder, which comprises heating until a semi-molten body is formed, rapidly solidifying, and optionally performing a pulverizing step and then classifying to a predetermined particle size.
水素雰囲気中で焼結された後に溶融されることを特徴と
する請求項１記載の高融点金属基合金粉末の製造方法。2. The method for producing a refractory metal-based alloy powder according to claim 1, wherein the granulated powder is melted after being sintered in a vacuum, argon or hydrogen atmosphere.
水素雰囲気中で行われることを特徴とする請求項１又は
請求項２記載の高融点金属基合金粉末の製造方法。3. The method for producing a refractory metal-based alloy powder according to claim 1, wherein the crushing step is performed in a vacuum, argon or hydrogen atmosphere.
急冷処理を施すことを特徴とする請求項１〜請求項３の
いずれか記載の高融点金属基合金粉末の製造方法。4. The method for producing a refractory metal-based alloy powder according to claim 1, wherein annealing or annealing and quenching treatment are performed before the pulverizing step.
状態に合金化させた粉末を原料として、熱間静水圧プレ
スにて加圧焼結することを特徴とする高融点金属基合金
体の製造方法。5. A refractory metal-based alloy body, characterized in that a powder obtained by alloying a refractory metal and another metal in a uniformly dispersed state is pressure-sintered by a hot isostatic press. Manufacturing method.
融点金属基合金粉末の製造方法によって製造された粉末
を原料として、熱間静水圧プレスにて加圧焼結すること
を特徴とする高融点金属基合金体の製造方法。6. A powder produced by the method for producing a refractory metal-based alloy powder according to claim 1 is used as a raw material and pressure-sintered by a hot isostatic press. And a method for producing a refractory metal-based alloy body.
合金の液相線温度以下の所定温度下で実行することを特
徴とする請求項４又は請求項５記載の高融点金属基合金
体の製造方法。7. The refractory metal-based alloy according to claim 4, wherein the hot isostatic pressing is performed at a predetermined temperature equal to or lower than the liquidus temperature of the refractory metal-based alloy. Body manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7110649A JPH08170110A (en) | 1994-10-18 | 1995-05-09 | High melting point metal-based alloy powder and production of high melting point metal-based alloy compact |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25236294 | 1994-10-18 | ||
| JP6-252362 | 1994-10-18 | ||
| JP7110649A JPH08170110A (en) | 1994-10-18 | 1995-05-09 | High melting point metal-based alloy powder and production of high melting point metal-based alloy compact |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08170110A true JPH08170110A (en) | 1996-07-02 |
Family
ID=26450235
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7110649A Pending JPH08170110A (en) | 1994-10-18 | 1995-05-09 | High melting point metal-based alloy powder and production of high melting point metal-based alloy compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08170110A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011129565A2 (en) * | 2010-04-12 | 2011-10-20 | 희성금속 주식회사 | Method for producing tantalum (ta) powder using eutectic alloys |
| KR101527655B1 (en) * | 2013-12-12 | 2015-06-09 | 희성금속 주식회사 | Recovery method of platinum group metals |
| JP2023126111A (en) * | 2022-02-28 | 2023-09-07 | 山陽特殊製鋼株式会社 | Method for producing mixed powder for 3D modeling |
-
1995
- 1995-05-09 JP JP7110649A patent/JPH08170110A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011129565A2 (en) * | 2010-04-12 | 2011-10-20 | 희성금속 주식회사 | Method for producing tantalum (ta) powder using eutectic alloys |
| WO2011129565A3 (en) * | 2010-04-12 | 2011-12-22 | 희성금속 주식회사 | Method for producing tantalum (ta) powder using eutectic alloys |
| JP2013528700A (en) * | 2010-04-12 | 2013-07-11 | ヒ スング メタル リミテッド | Method for producing tantalum (Ta) powder using eutectic alloy |
| KR101527655B1 (en) * | 2013-12-12 | 2015-06-09 | 희성금속 주식회사 | Recovery method of platinum group metals |
| JP2023126111A (en) * | 2022-02-28 | 2023-09-07 | 山陽特殊製鋼株式会社 | Method for producing mixed powder for 3D modeling |
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