JPS63223101A - Production of alloy powder - Google Patents
Production of alloy powderInfo
- Publication number
- JPS63223101A JPS63223101A JP62054990A JP5499087A JPS63223101A JP S63223101 A JPS63223101 A JP S63223101A JP 62054990 A JP62054990 A JP 62054990A JP 5499087 A JP5499087 A JP 5499087A JP S63223101 A JPS63223101 A JP S63223101A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- alloy powder
- alloy
- phase
- amorphous
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 154
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 81
- 239000000956 alloy Substances 0.000 title claims abstract description 81
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 150000004767 nitrides Chemical class 0.000 claims abstract description 18
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 9
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 9
- 229910052718 tin Inorganic materials 0.000 claims abstract description 9
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 9
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims description 19
- 238000005551 mechanical alloying Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 13
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000000137 annealing Methods 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 2
- 229910000881 Cu alloy Inorganic materials 0.000 abstract 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 1
- -1 ZrN Chemical class 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 239000002994 raw material Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 238000010791 quenching Methods 0.000 description 6
- 230000000171 quenching effect Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、非晶質相、非晶質相と析出物、結晶質相と析
出物又は非晶質相と酸化物又は窒化物からなる合金粉末
の製造法に関するものである。Detailed Description of the Invention (Field of Industrial Application) The present invention provides an amorphous phase, an amorphous phase and a precipitate, a crystalline phase and a precipitate, or an amorphous phase and an oxide or nitride. This invention relates to a method for producing alloy powder.
（従来の技術）
従来より、非晶質合金、金属粒子分散型合金を作製する
最も一般的な方法として、液体急冷法があげられる（「
アモルファス合金その物性と応用」■アグネ、第６〜１
１頁参照）、この方法では。(Prior art) Liquid quenching has traditionally been the most common method for producing amorphous alloys and metal particle dispersed alloys ("
"Amorphous alloys, their physical properties and applications" ■Agne, Volumes 6-1
(see page 1), in this method.
金属を溶融状態から１０４〜ｂ
冷却速度で金属ロール又は水中に噴出することにより、
薄帯、細線、粉末状材料を容易に作製できる。中でも、
この方法により作製された粉末は。By ejecting the metal from a molten state into a metal roll or water at a cooling rate of 104~b,
Thin strips, thin wires, and powder materials can be easily produced. Among them,
The powder made by this method is.
その後の成型により所望の形状にできるという点で、広
い分野での応用が考えられている。Since it can be formed into a desired shape by subsequent molding, it is considered to have applications in a wide range of fields.
一方、最近、非晶質合金粉末を作製する新しい方法とし
て、特開昭６１−２５０１２２号公報記載の拡散反応に
よる製造法がある。On the other hand, recently, as a new method for producing amorphous alloy powder, there is a production method using a diffusion reaction described in JP-A-61-250122.
（発明が解決しようとする問題点）
前記した液体急冷法で非晶質合金粉末を得るには、状態
図において共晶組成近傍や化合物組成近傍に限られてい
ることから、その合金成分には自ずと制約がある。(Problems to be Solved by the Invention) In order to obtain an amorphous alloy powder by the liquid quenching method described above, since the phase diagram is limited to the vicinity of the eutectic composition or the vicinity of the compound composition, the alloy composition must be Naturally, there are restrictions.
一方、拡散反応による製造法も、液体急冷法と同じ組成
範囲のものしか得られず、新しい合金組成での非晶質化
は見い出されていない。On the other hand, the production method using diffusion reaction can only produce products in the same composition range as the liquid quenching method, and amorphousization with a new alloy composition has not been found.
したがって、この液体急冷法や拡散反応で得ることので
きない合金組成で非晶質相が得られれば。Therefore, if an amorphous phase can be obtained with an alloy composition that cannot be obtained by this liquid quenching method or diffusion reaction.
ユニークな性質を発揮し、用途拡大に結びつくものと考
えられ、今まで得ることができなかった合金組成で、し
かも簡単な方法で得ることができる非晶質合金粉末が強
く望まれている。There is a strong desire for an amorphous alloy powder that exhibits unique properties and is thought to lead to expanded applications, has an alloy composition that has not been available until now, and can be obtained by a simple method.
（問題点を解決するための手段）
本発明者らは、これらの事情に鑑み、今まで液体急冷法
や拡散反応で得ることのできない合金組成で、しかも簡
単な方法で合金粉末を得ることのできる製造法を提供す
ることを目的として鋭意研究した結果、特定金属又は合
金粉末を特定の混合比で混合して機械的合金法により製
造すると、非晶質相の合金粉末が得られ、この非晶質相
の合金粉末を焼なまし処理することによって、非晶質相
と均一に分散した析出物又は結晶質Ｃｕ相と均一に分散
した析出物を有する合金粉末が、また、この非晶質相の
合金粉末と酸化物又は窒化物粉末とを混合して機械的合
金法により製造することによって、非晶質相と酸化物又
は窒化物を有する合金粉末が得られることを見い出し、
さらに、これらの粉末が超伝導性１機械的特性、耐食性
、磁気的特性等のユニークな特性を有していることを見
い出して本発明を完成した。(Means for Solving the Problems) In view of these circumstances, the present inventors have devised a method to obtain an alloy powder with an alloy composition that could not be obtained by the liquid quenching method or diffusion reaction by a simple method. As a result of intensive research aimed at providing a manufacturing method that can produce By annealing the crystalline phase alloy powder, an alloy powder having an amorphous phase and uniformly dispersed precipitates or a crystalline Cu phase and uniformly dispersed precipitates can be produced. It has been discovered that an alloy powder having an amorphous phase and an oxide or nitride can be obtained by mixing phase alloy powder and oxide or nitride powder and producing it by a mechanical alloying method,
Furthermore, the present invention was completed by discovering that these powders have unique properties such as superconductivity, mechanical properties, corrosion resistance, and magnetic properties.
すなわち９本発明は２機械的合金法により合金粉末を製
造するに際し、Ｃｕ粉末、Ｃｕ−Ｎ（ＮはＡｊ！、Ｓｉ
、Ｓｎ、Ｇｏ、Ｂ、Ｐ、Ｃからなる群より選ばれる一種
又は二種以上の元素）粉末。In other words, 9 the present invention produces alloy powder by 2 mechanical alloying method, Cu powder, Cu-N (N is Aj!, Si
, Sn, Go, B, P, and C) powder.
Ｍ （ＭはＮｂ、 Ｖ、 Ｔａ、 Ｗ、 Ｃｒ、 Ｍｏ
、 Ｃｏ。M (M is Nb, V, Ta, W, Cr, Mo
, Co.
Ｆｅからなる群より選ばれる一種又は二種以上の元素）
粉末、Ｍ−Ｎ粉末及びＮ粉末からなる群より選ばれる少
なくとも二種の粉末を下記式Ｃｕｒ＊ｏ−＜トｖ＞
ＭＸ −ＮＹ（Ｘは２０〜６０原子％、Ｙは１０〜３
０原子％である。）で示される割合で混合して９組織が
非晶質相である合金粉末を得ることを特徴とする合金粉
末の製造法１機械的合金法により合金粉末を製造するに
際し、Ｃｕ粉末、Ｃｕ−Ｎ（ＮはＡｌ。one or more elements selected from the group consisting of Fe)
At least two types of powder selected from the group consisting of powder, M-N powder, and N powder are represented by the following formula Cur*o-<tv>
MX -NY (X is 20 to 60 atom%, Y is 10 to 3
It is 0 atom%. ) A manufacturing method of alloy powder characterized by obtaining an alloy powder in which nine microstructures are amorphous phases 1 When manufacturing an alloy powder by the mechanical alloying method, Cu powder, Cu- N (N is Al.
Ｓｔ、Ｓｎ、Ｇｅ、Ｂ、Ｐ、Ｃからなる群より選ばれる
一種又は二種以上の元素）粉末、 Ｍ （ＭはＮｂ、
Ｖ、 Ｔａ、 Ｗ、 Ｃｒ、 Ｍｏ、 Ｇｏ、 Ｆｅか
らなる群より選ばれる一種又は二種以上の元素）粉末、
Ｍ−Ｎ粉末及びＮ粉末からなる群より選ばれる少なくと
も二種の粉末を下記式
Ｃｕ １１１０− （Ｘ＊ＶＩ Ｍｘ −ＮＹ（
Ｘは２０〜６０原子％、Ｙは１０〜３０原子％である。one or more elements selected from the group consisting of St, Sn, Ge, B, P, and C) powder, M (M is Nb,
one or more elements selected from the group consisting of V, Ta, W, Cr, Mo, Go, Fe) powder;
At least two types of powder selected from the group consisting of M-N powder and N powder are expressed by the following formula Cu 1110- (X*VI Mx -NY(
X is 20 to 60 atomic %, and Y is 10 to 30 atomic %.
）で示される割合で混合して２組織が非晶質相である合
金粉末を得９次いで、この粉末を焼なまし処理して２組
織が非晶質相と析出物又は結晶質Ｃｕ相と析出物である
合金粉末を得ることを特徴とする合金粉末の製造法及び
機械的合金法により合金粉末を製造するに際し、Ｃｕ粉
末。) to obtain an alloy powder in which the two structures are an amorphous phase.9 Then, this powder is annealed to form an amorphous phase and a precipitate or a crystalline Cu phase in the two structures. Cu powder when producing alloy powder by a mechanical alloying method and a method for producing alloy powder characterized by obtaining alloy powder as a precipitate.
Ｃｕ−Ｎ（ＮはＡｌ、 ｓ ｉ、 Ｓｎ、 Ｇ ｅ、
Ｂ、 ｐ。Cu-N (N is Al, si, Sn, Ge,
B, p.
Ｃからなる群より選ばれる一種又は二種以上の元素）粉
末、 Ｍ （ＭはＮｂ、Ｖ、Ｔａ、Ｗ、Ｃｒ。one or more elements selected from the group consisting of C) powder, M (M is Nb, V, Ta, W, Cr.
Ｍｏ、Ｃｏ、Ｆｅからなる群より選ばれる一種又は二種
以上の元素）粉末、Ｍ−Ｎ粉末及びＮ粉末からなる群よ
り選ばれる少なくとも二種の粉末を下記式
％式％
（Ｘは２０〜６０原子％、Ｙは１０〜３０原子％である
。）で示される割合で混合して１組織が非晶質相である
合金粉末を得２次いで、この粉末と酸化物又は窒化物粉
末とを混合して２組織が非晶質相と酸化物又は窒化物で
ある合金粉末を得ることを特徴とする合金粉末の製造法
を要旨とするものである。One or more elements selected from the group consisting of Mo, Co, and Fe) powder, at least two types of powder selected from the group consisting of M-N powder and N powder in the following formula % formula % (X is 20 to 60 atomic % and Y is 10 to 30 atomic %) to obtain an alloy powder in which one structure is an amorphous phase.2 Next, this powder and an oxide or nitride powder are mixed. The gist of this invention is a method for producing an alloy powder, which is characterized by mixing to obtain an alloy powder whose two structures are an amorphous phase and an oxide or nitride.
まず１本発明の第１発明について説明すると。First, the first aspect of the present invention will be explained.
原料としてＣｕ粉末、Ｃｕ−Ｎ（ＮはＡｌ、Ｓｉ。Raw materials include Cu powder and Cu-N (N is Al and Si.
Ｓｎ、Ｇｅ、Ｂ、Ｐ、Ｃからなる群より選ばれる一種又
は二種以上の元素）粉末、 Ｍ （ＭはＮｂ。one or more elements selected from the group consisting of Sn, Ge, B, P, and C) powder, M (M is Nb).
Ｖ＊ Ｔ ａ ＊ Ｗ＊ Ｃ’ ｒ １Ｍ ｏ 、Ｃ
ｏ 、Ｆ ｅからなる群より選ばれる一種又は二種以上
の元素）粉末。V* T a * W* C' r 1M o ,C
one or more elements selected from the group consisting of o, Fe, e) powder.
Ｍ−Ｎ粉末及びＮ粉末からなる群より選ばれる少なくと
も二種の粉末を用い２式（Ｃｕ、。。−（Ｘ＊ＩＭＸ
Ｎ？）（Ｘは２０〜６０原子％、Ｙは１０〜３０原子
％である。）で示される割合で混合して１機械的合金法
で製造することが必要である。Using at least two types of powder selected from the group consisting of M-N powder and N powder, 2 formulas (Cu,...-(X*IMX
N? ) (X is 20 to 60 atomic %, Y is 10 to 30 atomic %.) It is necessary to manufacture them by a mechanical alloying method by mixing them in the proportions shown.
この機械的合金法は９例えば、「軽金属Ｊ ＶＯＬ。This mechanical alloying method is used in 9, for example, "Light Metals J VOL.
３２、磁１２．Ｐ６８８〜６９５ （１９８２）の文献
に記載されているごとく、上記粉末を高硬度の金属製あ
るいはセラミック製のボールとともに、ボールの材質と
同じ円筒の容器に入れて粉砕混練するもので、このとき
の粉砕混練する時間としては。32, magnetic 12. As described in the document P688-695 (1982), the above powder is crushed and kneaded together with high-hardness metal or ceramic balls in a cylindrical container made of the same material as the balls. As for the time for crushing and kneading.
１０〜４０時間であることが好ましく、特に１５〜３０
時間が好ましい、また、原料として用いる粉末の大きさ
としては、２００μｍ以下が適当であり、１００μｍ以
下が好ましい。The time period is preferably 10 to 40 hours, particularly 15 to 30 hours.
The time is preferable, and the size of the powder used as a raw material is suitably 200 μm or less, preferably 100 μm or less.
本発明において、上記した原料として用いる粉末を、上
記の式を満足させるように混合することが必要で、Ｘが
２０原子％未満又は６０原子％を超えると、まったく非
晶質化しないか、あるいは一部結晶化して、非晶質相の
合金粉末を得ることができない。また、Ｙが１０原子％
未満又は３０原子％を超えると、これもまったく非晶質
化しないか、あるいは一部結晶化して、非晶質相の合金
粉末を得ることができない。In the present invention, it is necessary to mix the powders used as the raw materials described above so as to satisfy the above formula. Partial crystallization occurs, making it impossible to obtain an amorphous phase alloy powder. In addition, Y is 10 atomic%
If the amount is less than 30 atomic %, it will not become amorphous at all or will be partially crystallized, making it impossible to obtain an alloy powder in an amorphous phase.
このとき、上記原料に酸化物又は窒化物の合金粉末を混
合することもできる。これを混合すると。At this time, an oxide or nitride alloy powder can also be mixed with the above raw material. When you mix this.
組織が非晶質相と酸化物又は窒化物である合金粉末を得
ることができる。この酸化物としては１例えば、ＭｇＯ
，ＺｒＯ，Ａｌｚｏｉ、Ｙ２Ｏ２ＺｎＯ等があげられ、
窒化物としては１例えば、ＺｒＮ。An alloy powder whose structure is an amorphous phase and an oxide or nitride can be obtained. This oxide is 1, for example, MgO
, ZrO, Alzoi, Y2O2ZnO, etc.
Examples of nitrides include ZrN.
ＴｔＮ、Ａｊ！Ｎ等があげられ、これらを体積率で７％
以下になるように混合することが好ましい。TtN, Aj! N, etc. are mentioned, and the volume percentage of these is 7%.
It is preferable to mix as follows.
次に、第２発明について説明すると、第１発明で得られ
た非晶質相の合金粉末を焼なまし処理すると、非晶質相
に分散した析出物又は結晶質Ｃｕ相に分散した析出物の
合金粉末が得られ、この非晶質相に分散した析出物を得
るためには、結晶化温度以下、特に７００℃未満で焼な
ましすることが望まれ、そのときの時間としては、２〜
１０時間が好ましく、特に３〜７時間が好ましい。また
。Next, to explain the second invention, when the alloy powder of the amorphous phase obtained in the first invention is annealed, precipitates dispersed in the amorphous phase or precipitates dispersed in the crystalline Cu phase are formed. In order to obtain alloy powder of ~
Preferably 10 hours, particularly preferably 3 to 7 hours. Also.
結晶質Ｃｕ相に分散した析出物を得るためには。In order to obtain precipitates dispersed in the crystalline Cu phase.
７００〜９００℃の温度で焼なましすることが望まれ、
そのときの時間としては、５〜２０時間が好ましい。It is desirable to anneal at a temperature of 700 to 900°C,
The time at that time is preferably 5 to 20 hours.
さらに、第３発明について説明すると、第１発明で得ら
れた合金粉末と、上記の酸化物又は窒化物とを混合して
機械的合金法により粉砕混練すると、非晶質相と酸化物
又は窒化物の合金粉末が得られ、これらを前記した体積
率が７％以下になるように混合することが好ましい。Furthermore, to explain the third invention, when the alloy powder obtained in the first invention and the above oxide or nitride are mixed and pulverized and kneaded by a mechanical alloying method, an amorphous phase and an oxide or nitride are formed. It is preferable that alloy powders of the above-mentioned materials are obtained, and these are mixed so that the above-mentioned volume fraction becomes 7% or less.
本発明の第１発明では９通常の凝固法は勿論のこと、液
体急冷法でさえも均一な合金にできなかったものを、非
晶質相という極めて均一な組成の合金粉末が得られ１例
えば、Ｃｕ−（Ｎｂ、Ｖ。In the first aspect of the present invention, an alloy powder with an extremely uniform composition called an amorphous phase can be obtained from an alloy that could not be made into a uniform alloy by ordinary solidification methods or even liquid quenching methods. , Cu-(Nb, V.
Ｔａ） （Ｓｎ、ＡＩ！、Ｓ ｉ、Ｇｅ）合金組成か
らなる非晶質単相の粉末は超伝導材料の原料として。Ta) (Sn, AI!, Si, Ge) Amorphous single-phase powder consisting of an alloy composition is used as a raw material for superconducting materials.
Ｃｕ−（Ｃｒ、 Ｍｏ、 Ｗ） （Ｓ ｔ、 ｐ、
ｃ、 Ｂ）合金組成からなる非晶質単相の粉末は高強度
、高耐食の導電材料の原料として、Ｃｕ−（Ｃｏ、Ｆｅ
）−（Ｓｉ、Ａｌ、Ｐ、Ｃ，Ｂ）合金組成からなる非晶
質単相の粉末は各種電気、電子部品材料の原料として特
に優れている。Cu-(Cr, Mo, W) (S t, p,
c, B) Amorphous single-phase powder consisting of an alloy composition is used as a raw material for conductive materials with high strength and high corrosion resistance.
)-(Si, Al, P, C, B) alloy composition, the amorphous single-phase powder is particularly excellent as a raw material for various electrical and electronic component materials.
本発明の第２発明では、第１発明の合金粉末を焼なまし
処理することにより、非晶質相と析出物又は結晶１ｉＣ
ｕ相と析出物の合金粉末が得られ。In the second invention of the present invention, by annealing the alloy powder of the first invention, an amorphous phase and a precipitate or crystal 1iC
An alloy powder of the u phase and precipitates was obtained.
非晶質相と析出物合金粉末では、非晶質単相よりも超伝
導性１機械的特性、磁気的特性に優れた合金粉末となる
。また、結晶質Ｃｕ相と析出物の合金粉末では、導電性
を有し、かつ超伝導性あるいは機械的特性の優れた合金
粉末となる。The amorphous phase and precipitate alloy powder results in an alloy powder with superior superconductivity, mechanical properties, and magnetic properties compared to an amorphous single phase. Further, an alloy powder of the crystalline Cu phase and the precipitates has electrical conductivity and has excellent superconductivity or mechanical properties.
本発明の第３発明では、非晶質相と酸化物あるいは窒化
物の合金粉末であることから、特に機械的特性に優れた
合金粉末になる。In the third aspect of the present invention, since it is an alloy powder of an amorphous phase and an oxide or nitride, the alloy powder has particularly excellent mechanical properties.
さらに９本発明における合金粉末は、加工性に優れてい
るため１組織を変えることなく、所望の形状に成型でき
、バルク材として多方面に利用できることから、各種工
業用材料、複合材料、超伝導材料、触媒等に広く用いる
ことのできる材料である。Furthermore, the alloy powder of the present invention has excellent workability, so it can be molded into a desired shape without changing one structure, and can be used in a variety of fields as a bulk material, so it can be used in various industrial materials, composite materials, superconducting It is a material that can be widely used for materials, catalysts, etc.
（実施例） 以下２本発明を実施例により具体的に説明する。(Example) The present invention will be specifically explained below with reference to two examples.
実施例１〜２１．比較例１〜９
表１．２に示す合金組成になるように２粒径約５０μｍ
のＣｕ、Ｎｂ、Ｖ、Ｔａ、Ｍｏ、Ｃｒ。Examples 1-21. Comparative Examples 1 to 9 Two grains with a diameter of approximately 50 μm were prepared so as to have the alloy composition shown in Table 1.2.
Cu, Nb, V, Ta, Mo, Cr.
Ｗ、Ｃｏ、Ｆｅ、Ｓｎ、Ｓｔ、Ｇｅ、ＡＩ、Ｂ。W, Co, Fe, Sn, St, Ge, AI, B.
Ｃ及びＰの粉末を直径１０鰭のＷＣ製のボールとともに
ＷＣ製の円筒容器に入れ、１７時間粉砕混練して合金粉
末を作製した。C and P powders were placed in a WC cylindrical container together with a WC ball having a diameter of 10 fins, and the mixture was crushed and kneaded for 17 hours to produce an alloy powder.
このようにして得た合金粉末の組織を、Ｘ線回折により
判定した。The structure of the alloy powder thus obtained was determined by X-ray diffraction.
その結果を表１，２に示す。The results are shown in Tables 1 and 2.
表 １
表 ２
表１，２より明らかなごとく、実施例１〜２１は２本発
明により得られた合金粉末で、非晶質単相となっている
。また、比較例１〜９においては。Table 1 Table 2 As is clear from Tables 1 and 2, Examples 1 to 21 are alloy powders obtained according to the present invention, and have an amorphous single phase. Moreover, in Comparative Examples 1 to 9.
非晶質相と結晶相の混合あるいは結晶相のみとなり、非
晶質単相は得られなかった。A mixture of an amorphous phase and a crystalline phase or only a crystalline phase was obtained, and an amorphous single phase was not obtained.
次に、上記で得た実施例１ （ＣｕｓｓＮｂ３ｔｓ ｎ
１３（原子％）〕の非非晶質相の合金粉末を、プレス
成型機により２幅５龍、厚さ１龍の材料を作製した。Next, Example 1 (CussNb3ts n
13 (atomic %)] was used to produce a material with a width of 2 mm and a thickness of 1 mm using a press molding machine.
この材料の超伝導性を、タライオスタットを用いて直流
四端子法で電気抵抗の測定により行ったところ、超伝導
遷移温度（Ｔｃ）が４．４にで、超伝導から常伝導への
遷移幅（ΔＴｃ）が０．０３ Ｋという非常にせまい、
良好な超伝導特性を示した。The superconductivity of this material was determined by measuring the electrical resistance using a taliostat using the DC four-probe method, and the superconducting transition temperature (Tc) was found to be 4.4, indicating a transition from superconductivity to normal conductivity. Very narrow width (ΔTc) of 0.03K,
It showed good superconducting properties.
また、実施例１５ ＣＣｕｓｏｃ ｒ ４ＳＰ ＋ｓ（
原子％）〕の非非晶質相の合金粉末を、ＩＮ ＨＣ１
中３０℃で８時間浸漬したところ、まったく腐食されな
いという良好な耐食性を示した。In addition, Example 15 CCusoc r 4SP +s (
atomic%)] of amorphous phase alloy powder, IN HC1
When immersed for 8 hours at 30°C, it showed good corrosion resistance with no corrosion at all.
実施例２２
実施例１ （Ｃｕｓ５Ｎ ｂ３ｚｓ ｎ’ｓ（原子％
）〕により得た非晶質単相の合金粉末を、３００℃で５
時間焼なまし処理して合金粉末を得た。この合金粉末を
Ｘ線回折により組織を調べたところ、非晶質相と析出物
（ＮｂｓＳｎ）相であった。Example 22 Example 1 (Cus5N b3zs n's (atomic%
)] The amorphous single-phase alloy powder obtained by
An alloy powder was obtained by time annealing treatment. When the structure of this alloy powder was examined by X-ray diffraction, it was found to be an amorphous phase and a precipitate (NbsSn) phase.
次に、この粉末をプレス成型機により２幅５龍。Next, this powder is molded into 2 widths and 5 dragons using a press molding machine.
厚さ１ｍｍの材料にし、実施例１と同様の方法で超伝導
性を測定したところ、超伝導から常伝導への遷移幅（Δ
Ｔｃ＝０．０３Ｋ）を広げることなく。When we measured the superconductivity using a material with a thickness of 1 mm in the same manner as in Example 1, we found that the transition width from superconductivity to normal conduction (Δ
Tc=0.03K) without widening.
超伝導遷移温度（Ｔｃ）が８．９にという、非晶質単相
よりさらに優れた特性を示した。The superconducting transition temperature (Tc) was 8.9, which showed even better characteristics than the amorphous single phase.
実施例２３
実施例１ （ＣｕｓｓＮ ｂｓｔＳ ｎ’ｆｆ（原子
％）〕により得た非晶質単相の合金粉末を、８００℃で
１０時間焼なまし処理して合金粉末を得た。この合金粉
末をＸ線回折により組織を調べたところ、結晶質Ｃｕ相
と析出物（Ｎ ｂ、Ｓ ｎ）相であった。Example 23 The amorphous single-phase alloy powder obtained in Example 1 (CussN bstS n'ff (atomic %)) was annealed at 800° C. for 10 hours to obtain an alloy powder. This alloy powder When the structure was examined by X-ray diffraction, it was found to be a crystalline Cu phase and a precipitate (Nb, Sn) phase.
次に、この粉末をプレス成型機により２幅５Ｂ。Next, this powder is molded into two widths of 5B using a press molding machine.
厚さ１ｆｉの材料にし、実施例１と同様の方法で超伝導
性を測定したところ、超伝導遷移温度（Ｔｃ）が１６．
８にと飛躍的に向上した。When a material with a thickness of 1fi was used and its superconductivity was measured in the same manner as in Example 1, the superconducting transition temperature (Tc) was 16.
It improved dramatically to 8.
実施例２４
実施例１ （ＣｕｓｓＮｂｓｚＳｎ＋３（原子％）〕
で得た非晶質単相の合金粉末９５％（体積率）と。Example 24 Example 1 (CussNbszSn+3 (atomic %))
95% (volume percentage) of the amorphous single-phase alloy powder obtained.
Ａ ｌ ｚ Ｏｓ粉末５％（体積率）とを、直径１０鶴
の礪逼製のボールとともに瑞逼製の円筒容器内に入れ、
２３時間粉砕混練して合金粉末を作製した。5% (volume percentage) of A l z Os powder was placed in a cylindrical container made from Zuitai along with a ball made of 10 cranes in diameter, and
The mixture was crushed and kneaded for 23 hours to prepare an alloy powder.
このようにして得た合金粉末の組織をＸ線回折により判
定したところ、非晶質相とＡ １ ｚ Ｏｓとからなる
組織であった。When the structure of the alloy powder thus obtained was determined by X-ray diffraction, it was found to be a structure consisting of an amorphous phase and A 1 z Os.
次に、この粉末をプレス成型機により２幅５ｎ＋。Next, this powder was molded into two widths of 5n+ using a press molding machine.
厚さ１龍の材料にし、実施例１と同様の方法で超伝導性
を測定したところ、実施例１と同じ超伝導性を示した。When the superconductivity was measured in the same manner as in Example 1 using a material with a thickness of 1 mm, it showed the same superconductivity as in Example 1.
さらに、この合金粉末の硬度をビッカース硬度計で室温
で測定したところ、非晶質単相では５６００ＰＮであっ
たものが、非晶質相とＡｌｔｏｓの合金粉末では６４０
ＤＰＮにまで上昇した。Furthermore, when the hardness of this alloy powder was measured using a Vickers hardness tester at room temperature, the hardness of the amorphous single phase was 5600 PN, but the hardness of the amorphous phase and Altos alloy powder was 640 PN.
It rose to DPN.
実施例２５
実施例１ （ＣｕｓｓＮ ｂ３ｚｓ ｎ＋ｉ（原子％
）〕で得た非晶質単相の合金粉末９７％（体積率）と。Example 25 Example 1 (CussN b3zs n+i (atomic %
)] with 97% (volume fraction) of the amorphous single-phase alloy powder obtained.
ＡＩＮ粉末３％（体積率）とを、直径２０ａｍのＷＣ製
のボールとともにＷＣ製の円筒容器内に入れ。3% (volume percentage) of AIN powder was placed in a WC cylindrical container along with a WC ball having a diameter of 20 am.
１４時間粉砕混練して合金粉末を作製した。The mixture was crushed and kneaded for 14 hours to prepare an alloy powder.
このようにして得た合金粉末の組織をＸ線回折により判
定したところ、非晶質相と／ＩＮとからなる組織であっ
た。When the structure of the alloy powder thus obtained was determined by X-ray diffraction, it was found to be a structure consisting of an amorphous phase and /IN.
次に、この粉末をプレス成型機により１幅５龍。Next, this powder is molded into 1 width and 5 dragons using a press molding machine.
厚さｌ■ｌの材料にし、実施例１と同様の方法で超伝導
性を測定したところ、実施例１と同じ超伝導性を示した
。When the material was made into a material having a thickness of 1.1 cm and its superconductivity was measured in the same manner as in Example 1, it showed the same superconductivity as in Example 1.
さらに、この合金粉末の硬度をビッカース硬度計で室温
で測定したところ、非晶質単相では５６０ＤＰＮであっ
たものが、非晶質相とＡＩＮの合金粉末では６２０ＤＰ
Ｎにまで上昇した。Furthermore, when the hardness of this alloy powder was measured using a Vickers hardness tester at room temperature, it was 560DPN for the amorphous single phase, but 620DPN for the alloy powder of amorphous phase and AIN.
It rose to N.
（発明の効果）
本発明によれば、簡単な方法で非晶質単相、非晶質相に
均一に分散した析出物、結晶質Ｃｕ相に均一に分散した
析出物、非晶質相と均一に分散した酸化物又は窒化物の
組織を有している合金粉末が得られ、この合金粉末は２
機械的性質、電気的。(Effects of the Invention) According to the present invention, a single amorphous phase, a precipitate uniformly dispersed in an amorphous phase, a precipitate uniformly dispersed in a crystalline Cu phase, and an amorphous phase can be easily formed. An alloy powder having a uniformly dispersed oxide or nitride structure is obtained, and this alloy powder has 2
Mechanical properties, electrical.
磁気的性質、超伝導性、耐食性、耐摩耗性に優れている
。Excellent magnetic properties, superconductivity, corrosion resistance, and wear resistance.
また２本発明によって得られた合金粉末は、加工性に優
れていることから、所望の形状に成型することができる
。Furthermore, the alloy powder obtained by the present invention has excellent workability and can be molded into a desired shape.
さらに２本発明によれば、数千人程度の微細粉末にもす
ることが可能である。Furthermore, according to the present invention, it is possible to make a fine powder of several thousand particles.
特許出願人 増 本 健ユニ亭力株ｖｃ
Ｒ社Patent applicant Masumoto Kenyunitei Rikisha VC
Company R
Claims (3)
Ｃｕ粉末、Ｃｕ−Ｎ（ＮはＡｌ、Ｓｉ、Ｓｎ、Ｇｅ、Ｂ
、Ｐ、Ｃからなる群より選ばれる一種又は二種以上の元
素）粉末、Ｍ（ＭはＮｂ、Ｖ、Ｔａ、Ｗ、Ｃｒ、Ｍｏ、
Ｃｏ、Ｆｅからなる群より選ばれる一種又は二種以上の
元素）粉末、Ｍ−Ｎ粉末及びＮ粉末からなる群より選ば
れる少なくとも二種の粉末を式〔ＣＵ＿１＿０＿０＿−
＿（＿Ｘ＿＋＿Ｙ＿）−Ｍ＿Ｘ−Ｎ＿Ｙ〕（Ｘは２０〜
６０原子％、Ｙは１０〜３０原子％である。）で示され
る割合で混合して、組織が非晶質相である合金粉末を得
ることを特徴とする合金粉末の製造法。(1) When producing alloy powder by mechanical alloying method,
Cu powder, Cu-N (N is Al, Si, Sn, Ge, B
, P, one or more elements selected from the group consisting of C) powder, M (M is Nb, V, Ta, W, Cr, Mo,
One or more elements selected from the group consisting of Co, Fe) powder, at least two powders selected from the group consisting of M-N powder and N powder with the formula [CU_1_0_0_-
＿(＿X＿+＿Y＿)−M_X−N_Y〕(X is from 20 to
60 atom %, and Y is 10 to 30 atom %. ) A method for producing an alloy powder, which is characterized in that the alloy powder is mixed in the proportions shown in (a) to obtain an alloy powder whose structure is an amorphous phase.
Ｃｕ粉末、Ｃｕ−Ｎ（ＮはＡｌ、Ｓｉ、Ｓｎ、Ｇｅ、Ｂ
、Ｐ、Ｃからなる群より選ばれる一種又は二種以上の元
素）粉末、Ｍ（ＭはＮｂ、Ｖ、Ｔａ、Ｗ、Ｃｒ、Ｍｏ、
Ｃｏ、Ｆｅからなる群より選ばれる一種又は二種以上の
元素）粉末、Ｍ−Ｎ粉末及びＮ粉末からなる群より選ば
れる少なくとも二種の粉末を式〔Ｃｕ＿１＿０＿０＿−
＿（＿Ｘ＿＋＿Ｙ＿）−Ｍ＿Ｘ−Ｎ＿Ｙ〕（Ｘは２０〜
６０原子％、Ｙは１０〜３０原子％である。）で示され
る割合で混合して、組織が非晶質相である合金粉末を得
、次いで、この粉末を焼なまし処理して、組織が非晶質
相と析出物又は結晶質Ｃｕ相と析出物である合金粉末を
得ることを特徴とする合金粉末の製造法。(2) When producing alloy powder by mechanical alloying method,
Cu powder, Cu-N (N is Al, Si, Sn, Ge, B
, P, one or more elements selected from the group consisting of C) powder, M (M is Nb, V, Ta, W, Cr, Mo,
One or more elements selected from the group consisting of Co, Fe) powder, at least two powders selected from the group consisting of M-N powder and N powder with the formula [Cu_1_0_0_-
＿(＿X＿+＿Y＿)−M_X−N_Y〕(X is from 20 to
60 atom %, and Y is 10 to 30 atom %. ) to obtain an alloy powder whose structure is an amorphous phase, and then this powder is annealed so that its structure consists of an amorphous phase and a precipitate or a crystalline Cu phase. A method for producing alloy powder, characterized by obtaining alloy powder as a precipitate.
Ｃｕ粉末、Ｃｕ−Ｎ（ＮはＡｌ、Ｓｉ、Ｓｎ、Ｇｅ、Ｂ
、Ｐ、Ｃからなる群より選ばれる一種又は二種以上の元
素）粉末、Ｍ（ＭはＮｂ、Ｖ、Ｔａ、Ｗ、Ｃｒ、Ｍｏ、
Ｃｏ、Ｆｅからなる群より選ばれる一種又は二種以上の
元素）粉末、Ｍ−Ｎ粉末及びＮ粉末からなる群より選ば
れる少なくとも二種の粉末を式〔Ｃｕ＿１＿０＿０＿−
＿（＿Ｘ＿＋＿Ｙ＿）−Ｍ＿Ｘ−Ｎ＿Ｙ〕（Ｘは２０〜
６０原子％、Ｙは１０〜３０原子％である。）で示され
る割合で混合して、組織が非晶質相である合金粉末を得
、次いで、この粉末と酸化物又は窒化物粉末とを混合し
て、組織が非晶質相と酸化物又は窒化物である合金粉末
を得ることを特徴とする合金粉末の製造法。(3) When producing alloy powder by mechanical alloying method,
Cu powder, Cu-N (N is Al, Si, Sn, Ge, B
, P, one or more elements selected from the group consisting of C) powder, M (M is Nb, V, Ta, W, Cr, Mo,
One or more elements selected from the group consisting of Co, Fe) powder, at least two powders selected from the group consisting of M-N powder and N powder with the formula [Cu_1_0_0_-
＿(＿X＿+＿Y＿)−M_X−N_Y〕(X is from 20 to
60 atom %, and Y is 10 to 30 atom %. ) to obtain an alloy powder whose structure is an amorphous phase, and then this powder and an oxide or nitride powder are mixed to form an amorphous phase and an oxide or nitride powder. A method for producing an alloy powder, characterized by obtaining an alloy powder that is a nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62054990A JPH0791562B2 (en) | 1987-03-10 | 1987-03-10 | Alloy powder manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62054990A JPH0791562B2 (en) | 1987-03-10 | 1987-03-10 | Alloy powder manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63223101A true JPS63223101A (en) | 1988-09-16 |
| JPH0791562B2 JPH0791562B2 (en) | 1995-10-04 |
Family
ID=12986086
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62054990A Expired - Lifetime JPH0791562B2 (en) | 1987-03-10 | 1987-03-10 | Alloy powder manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0791562B2 (en) |
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| WO2006034054A1 (en) * | 2004-09-16 | 2006-03-30 | Belashchenko Vladimir E | Deposition system, method and materials for composite coatings |
| CN104801708A (en) * | 2015-05-15 | 2015-07-29 | 福建农林大学 | Full metal component iron-based amorphous alloy powder for powder metallurgy and preparation method thereof |
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1987
- 1987-03-10 JP JP62054990A patent/JPH0791562B2/en not_active Expired - Lifetime
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| EP1921699A3 (en) * | 1998-09-18 | 2010-12-22 | Canon Kabushiki Kaisha | Electrode material for anode of rechargeable lithium battery, electrode structural body using said electrode material, rechargeable lithium battery using said electrode structural body, process for producing said electrode structural body, and process for producing said rechargeable lithium battery |
| KR20030006564A (en) * | 2001-07-13 | 2003-01-23 | (주)나인디지트 | Manufacturing method of W-Cu alloy |
| WO2006034054A1 (en) * | 2004-09-16 | 2006-03-30 | Belashchenko Vladimir E | Deposition system, method and materials for composite coatings |
| US7670406B2 (en) | 2004-09-16 | 2010-03-02 | Belashchenko Vladimir E | Deposition system, method and materials for composite coatings |
| CN104801708A (en) * | 2015-05-15 | 2015-07-29 | 福建农林大学 | Full metal component iron-based amorphous alloy powder for powder metallurgy and preparation method thereof |
| CN114974722A (en) * | 2022-07-04 | 2022-08-30 | 中山大学 | Intermetallic compound superconductor and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0791562B2 (en) | 1995-10-04 |
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