JP3696514B2 - Method for producing alloy powder - Google Patents
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- JP3696514B2 JP3696514B2 JP2001044088A JP2001044088A JP3696514B2 JP 3696514 B2 JP3696514 B2 JP 3696514B2 JP 2001044088 A JP2001044088 A JP 2001044088A JP 2001044088 A JP2001044088 A JP 2001044088A JP 3696514 B2 JP3696514 B2 JP 3696514B2
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- 229910045601 alloy Inorganic materials 0.000 title claims description 75
- 239000000956 alloy Substances 0.000 title claims description 75
- 239000000843 powder Substances 0.000 title claims description 65
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000002245 particle Substances 0.000 claims description 377
- 239000000654 additive Substances 0.000 claims description 63
- 230000000996 additive effect Effects 0.000 claims description 63
- 229910052751 metal Inorganic materials 0.000 claims description 53
- 239000011159 matrix material Substances 0.000 claims description 52
- 239000002184 metal Substances 0.000 claims description 52
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 38
- 239000001257 hydrogen Substances 0.000 claims description 36
- 229910052739 hydrogen Inorganic materials 0.000 claims description 36
- 238000003860 storage Methods 0.000 claims description 32
- 238000005551 mechanical alloying Methods 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 5
- 229910001316 Ag alloy Inorganic materials 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 4
- 229910001020 Au alloy Inorganic materials 0.000 claims description 4
- 229910000531 Co alloy Inorganic materials 0.000 claims description 4
- 229910000599 Cr alloy Inorganic materials 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 4
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 4
- 229910000575 Ir alloy Inorganic materials 0.000 claims description 4
- 229910000914 Mn alloy Inorganic materials 0.000 claims description 4
- 229910001182 Mo alloy Inorganic materials 0.000 claims description 4
- 229910001257 Nb alloy Inorganic materials 0.000 claims description 4
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 4
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 4
- 229910001260 Pt alloy Inorganic materials 0.000 claims description 4
- 229910000629 Rh alloy Inorganic materials 0.000 claims description 4
- 229910000929 Ru alloy Inorganic materials 0.000 claims description 4
- 229910001362 Ta alloys Inorganic materials 0.000 claims description 4
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 4
- 229910000756 V alloy Inorganic materials 0.000 claims description 4
- 229910001080 W alloy Inorganic materials 0.000 claims description 4
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 4
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 4
- 238000003801 milling Methods 0.000 description 19
- 230000001133 acceleration Effects 0.000 description 14
- 239000011812 mixed powder Substances 0.000 description 13
- 238000000498 ball milling Methods 0.000 description 11
- 238000005259 measurement Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 239000011882 ultra-fine particle Substances 0.000 description 7
- 238000006356 dehydrogenation reaction Methods 0.000 description 6
- 239000010419 fine particle Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000005266 casting Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910017706 MgZn Inorganic materials 0.000 description 1
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- 229910018007 MmNi Inorganic materials 0.000 description 1
- 229910010340 TiFe Inorganic materials 0.000 description 1
- 229910010380 TiNi Inorganic materials 0.000 description 1
- 229910008340 ZrNi Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 239000000696 magnetic material Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は合金粉末の製造方法、特に、金属マトリックスと添加成分とよりなる合金粒子の集合体である合金粉末を製造すべく、金属マトリックス粒子の集合体と、添加成分粒子の集合体とを用い、メカニカルアロイングおよびメカニカルグラインディングの一方を行う製造方法に関する。
【０００２】
【従来の技術】
従来、この種の製造方法においては、金属マトリックス粒子および添加成分粒子として粒径（通常、１μｍ以上）が同じか、若しくは略同じものを用い、比較的硬い添加成分粒子を十分に微細化して、金属マトリックス粒子内に均一に侵入分散させる、といった方法が採用されている。
【０００３】
【発明が解決しようとする課題】
しかしながら前記従来法においては添加成分粒子の微細化および侵入分散のために、例えば数十時間のミリングを行わなければならず、合金粉末の製造コストが高い、という問題があった。
【０００４】
【課題を解決するための手段】
本発明は、ミリング時間を大幅に短縮し得る前記合金粉末の製造方法を提供することを目的とする。
【０００５】
前記目的を達成するため本発明の第１の特徴によれば、金属マトリックスと添加成分とよりなる合金粒子の集合体である合金粉末を製造すべく、金属マトリックス粒子の集合体と、添加成分粒子の集合体とを用い、メカニカルアロイングおよびメカニカルグラインディングの一方を行って、前記添加成分粒子の集合体における少なくとも一部の添加成分粒子を前記金属マトリックス粒子内に侵入させるようにした高活性な合金粉末の製造方法であって、前記メカニカルアロイングおよびメカニカルグラインディングを行うに当り、前記金属マトリックス粒子の粒径Ｄを Ｄ≧３μｍに、また前記添加成分粒子の粒径ｄを ｄ≦５００ｎｍにそれぞれ設定する、合金粉末の製造方法が提供される。
【０００６】
前記目的を達成するため本発明の第２の特徴によれば、金属マトリックスと添加成分とよりなる合金粒子の集合体である水素吸蔵合金粉末を製造すべく、金属マトリックス粒子の集合体と、添加成分粒子の集合体とを用い、メカニカルアロイングおよびメカニカルグラインディングの一方を行って、前記添加成分粒子の集合体における少なくとも一部の添加成分粒子を前記金属マトリックス粒子内に侵入させるようにした高活性な水素吸蔵合金粉末の製造方法であって、前記金属マトリックス粒子は、粒径Ｄが Ｄ≧５μｍであるＭｇ粒子であり、また前記添加成分粒子６は、粒径ｄがｄ≦１００ｎｍであり、且つＮｉ粒子，Ｎｉ合金粒子，Ｆｅ粒子，Ｆｅ合金粒子，Ｖ粒子，Ｖ合金粒子，Ｍｎ粒子，Ｍｎ合金粒子，Ｔｉ粒子，Ｔｉ合金粒子，Ｃｕ粒子，Ｃｕ合金粒子，Ａｌ粒子，Ａｌ合金粒子，Ｐｄ粒子，Ｐｄ合金粒子，Ｐｔ粒子，Ｐｔ合金粒子，Ｚｒ粒子，Ｚｒ合金粒子，Ａｕ粒子，Ａｕ合金粒子，Ａｇ粒子，Ａｇ合金粒子，Ｃｏ粒子，Ｃｏ合金粒子，Ｍｏ粒子，Ｍｏ合金粒子，Ｎｂ粒子，Ｎｂ合金粒子，Ｃｒ粒子，Ｃｒ合金粒子，Ｚｎ粒子，Ｚｎ合金粒子，Ｒｕ粒子，Ｒｕ合金粒子，Ｒｈ粒子，Ｒｈ合金粒子，Ｔａ粒子，Ｔａ合金粒子，Ｉｒ粒子，Ｉｒ合金粒子，Ｗ粒子およびＷ合金粒子から選択される少なくとも一種であることを特徴とする合金粉末の製造方法が提供される。
【０００７】
金属マトリックス粒子の集合体と、添加成分粒子の集合体とを用い、メカニカルアロイングおよびメカニカルグラインディングの一方を行うに当たって、前記第１の特徴によれば、金属マトリックス粒子の粒径Ｄが Ｄ≧３μｍに、また添加成分粒子の粒径ｄが
ｄ≦５００ｎｍにそれぞれ設定され、また前記第２の特徴によれば、金属マトリックス粒子としてのＭｇ粒子の粒径Ｄが Ｄ≧５μｍに、また添加成分粒子の粒径ｄが ｄ≦１００ｎｍにそれぞれ設定されるが、このようなｎｍサイズの粒径を持つ添加成分粒子は、微粒子または超微粒子であって、非常に高い活性を有するので、添加成分粒子を金属マトリックス粒子内に侵入させるだけでなく、その金属マトリックス粒子表面に保持させておくことによっても、高活性な水素吸蔵合金粉末を得ることが可能である。また添加成分粒子は微粒子または超微粒子であるからミリングによる微細化は不要である。
【０００８】
これらのことから、前記方法によれば合金粉末を得るためのミリング時間を、例えば４０時間から１５分間にする、といったように大幅に短縮することが可能である。ただし、ｄ＞５００ｎｍでは前記ミリング時間が長くなり、また製造エネルギ的にも非効率的となる。
【０００９】
【発明の実施の形態】
図１、２において、合金粉末としての水素吸蔵合金粉末１は、金属マトリックス２と添加成分３とよりなる合金粒子４の集合体である。
【００１０】
水素吸蔵合金粉末１の製造に当っては、金属マトリックス粒子５の集合体（金属マトリックス粉末）と、添加成分粒子６の集合体（添加成分粉末）とを用い、メカニカルアロイングおよびメカニカルグラインディングの一方を行う、といった方法が採用される。
【００１１】
その際、金属マトリックス５の粒径ＤはＤ≧３μｍ、好ましくはＤ≧５μｍに設定され、また添加成分粒子６の粒径ｄは１０ｎｍ≦ｄ≦５００ｎｍ、好ましくはｄ≦１００ｎｍに設定される。両粒径Ｄ、ｄの関係は、好ましくはＤ／１００００≦ｄ≦Ｄ／５０であり、また添加成分粒子の添加量Ｌは０．１原子％≦Ｌ≦６５原子％、好ましくはＬ≦１０原子％である。
【００１２】
金属マトリックス粒子５には、体心立方晶系粒子であるＭｇ粒子，Ｖ粒子，ＴｉＣｒＶ系粒子，ＴｉＣｒＭｎ系粒子等が該当し、また水素と反応する金属元素をＡとし、またそれ以外の金属元素をＢとすると、ＡＢ5 系粒子：ＬａＮｉ5 粒子，ＭｍＮｉ5 （Ｍｍ：ミッシュメタル）粒子，ＣａＮｉ5 粒子等；ＡＢ2 系粒子：ＭｇＺｎ2 粒子，ＺｒＮｉ2 粒子等；ＡＢ系粒子：ＴｉＮｉ粒子，ＴｉＦｅ粒子等；Ａ2 Ｂ系粒子：Ｍｇ2 Ｎｉ粒子，Ｃａ2 Ｆｅ粒子等が該当する。これらの粒子から選択される一種が金属マトリックス粒子として用いられる。添加成分粒子６としては、Ｎｉ粒子，Ｎｉ合金粒子，Ｆｅ粒子，Ｆｅ合金粒子，Ｖ粒子，Ｖ合金粒子，Ｍｎ粒子，Ｍｎ合金粒子，Ｔｉ粒子，Ｔｉ合金粒子，Ｃｕ粒子，Ｃｕ合金粒子，Ａｌ粒子，Ａｌ合金粒子，Ｐｄ粒子，Ｐｄ合金粒子，Ｐｔ粒子，Ｐｔ合金粒子，Ｚｒ粒子，Ｚｒ合金粒子，Ａｕ粒子，Ａｕ合金粒子，Ａｇ粒子，Ａｇ合金粒子，Ｃｏ粒子，Ｃｏ合金粒子，Ｍｏ粒子，Ｍｏ合金粒子，Ｎｂ粒子，Ｎｂ合金粒子，Ｃｒ粒子，Ｃｒ合金粒子，Ｚｎ粒子，Ｚｎ合金粒子，Ｒｕ粒子，Ｒｕ合金粒子，Ｒｈ粒子，Ｒｈ合金粒子，Ｔａ粒子，Ｔａ合金粒子，Ｉｒ粒子，Ｉｒ合金粒子，Ｗ粒子およびＷ合金粒子から選択される少なくとも一種が用いられる。
【００１３】
メカニカルアロイングまたはメカニカルグラインディングにおいて、そのミリング時間ｔは１分間≦ｔ≦５時間といったように、短時間に設定される。このようにミリング時間を短縮すると、図２に明示するように、添加成分粒子６の集合体における、一部の添加成分粒子６は金属マトリックス粒子５内に完全に侵入してその粒子５と結合し、また他の一部の添加成分粒子６は金属マトリックス粒子５の表面に付着してその粒子５と結合し、さらに他の一部の添加成分粒子６は一部分を金属マトリックス粒子５表面に露出させてその粒子５内に埋込まれることにより金属マトリックス粒子５と結合する、といった状態が現出する。
【００１４】
前記のようにｎｍサイズの粒径を持つ添加成分粒子６は超微粒子（または微粒子）であって、非常に高い活性を有する。したがって、前記のように添加成分粒子６を金属マトリックス粒子５内に侵入させるだけでなく、その金属マトリックス粒子５表面に保持させておくことによっても、高活性な水素吸蔵合金粉末１を得ることが可能である。また添加成分粒子６は超微粒子（または微粒子）であるからミリングによる微細化は不要である。なお、両粒径Ｄ、ｄの関係がＤ／１００００＞ｄでは金属マトリックス粒子５と添加成分粒子６とのエネルギ差が大きすぎるため添加成分粒子６が金属マトリックス粒子５内に侵入することができなくなる。
【００１５】
以下、メカニカルアロイングを適用した具体例について説明する。
【００１６】
〔実施例１〕
純度が９９．９％であり、且つ粒径Ｄが１０μｍのＭｇ粒子（金属マトリックス粒子）の集合体と、純度が９９．９％であり、且つ粒径ｄが２０ｎｍのＮｉ粒子（添加成分粒子）の集合体とを、合金組成がＭｇ2 Ｎｉ（ＮｉのＬ＝３３．３原子％）となるように秤量して、合計２．５ｇの混合粉末を得た。この混合粉末を遊星型ボールミル（Furitsch製、Ｐ−５）の容量８０mlのポット（ＪＩＳ ＳＵＳ３１６製）に直径１０mmのボール（ＪＩＳ ＳＵＳ３１６製）１８個と共に入れ、ポット内を１．０ＭＰａの水素ガス雰囲気に保持して、ポット回転数 ７８０rpm 、ディスク回転数３６０rpm 、ミリング時間ｔ １５分間の条件でボールミリングを行った。この場合、ポット内には重力加速度Ｇの９倍の加速度９Ｇが発生していた。ボールミリング後、グローブボックス中で水素吸蔵合金粉末を採取した。この合金粉末を例（Ａ１）とする。
【００１７】
比較のため、前記Ｍｇ粒子の集合体と、純度が９９．９％であり、且つ粒径ｄが１０μｍ、つまりＭｇ粒子と同一粒径のＮｉ粒子の集合体とを用い、ミリング時間ｔを４０時間に設定した、ということ以外は前記と同様の方法で水素吸蔵合金粉末を得た。この合金粉末を例（Ｂ１）とする。
【００１８】
例（Ａ１）、（Ｂ１）は、そのボールミリング過程において水素化されているので、それらに、３５０℃、１時間の条件で真空引きを行う脱水素化処理を施し、次いで、例（Ａ１）、（Ｂ１）についてＰＣＴ測定を行った。図３は例（Ａ１）、（Ｂ１）のＰＣＴ特性（収束時間：５分間；２６０℃、放出）を示す。図３より、例（Ａ１）は例（Ｂ１）のミリング時間の１６０分の１の短時間にて得られたものであるが、例（Ｂ１）と同様のＰＣＴ特性を有することが判る。
【００１９】
〔実施例２〕
純度が９９．９％であり、且つ粒径Ｄが１０μｍのＭｇ粒子（金属マトリックス粒子）の集合体と、純度が９９．９％であり、且つ粒径ｄが２０ｎｍのＦｅ粒子（添加成分粒子）の集合体とを、合金組成がＭｇ97Ｆｅ3 （数値の単位は原子％）となるように秤量して、合計２．５ｇの混合粉末を得た。この混合粉末を遊星型ボールミル（Furitsch製、Ｐ−５）の容量８０mlのポット（ＪＩＳ ＳＵＳ３１６製）に直径１０mmのボール（ＪＩＳ ＳＵＳ３１６製）１８個と共に入れ、ポット内を２．０ＭＰａの水素ガス雰囲気に保持して、ポット回転数 ７８０rpm 、ディスク回転数３６０rpm 、ミリング時間ｔ １５分間の条件でボールミリングを行った。この場合、ポット内には重力加速度Ｇの９倍の加速度９Ｇが発生していた。ボールミリング後、グローブボックス中で水素吸蔵合金粉末を採取した。この合金粉末を例（Ａ２）とする。
【００２０】
比較のため、前記Ｍｇ粒子の集合体と、純度が９９．９％であり、且つ粒径ｄが１０μｍ、つまりＭｇ粒子と同一粒径のＦｅ粒子の集合体とを用い、ミリング時間ｔを３時間に設定した、ということ以外は前記と同様の方法で水素吸蔵合金粉末を得た。この合金粉末を例（Ｂ２）とする。
【００２１】
例（Ａ２）、（Ｂ２）に実施例１と同一条件で脱水素化処理を施し、次いで、例（Ａ２）、（Ｂ２）についてＰＣＴ測定を行った。図４は例（Ａ２）、（Ｂ２）のＰＣＴ特性（収束時間：５分間；３１０℃、放出）を示す。図４より、例（Ａ２）は例（Ｂ２）のミリング時間の１２分の１の短時間にて得られたものであるが、例（Ｂ２）よりも優れたＰＣＴ特性を有することが判る。
【００２２】
図５は例（Ａ２）、（Ｂ２）の、測定温度３１０℃における水素化速度試験結果を示す。この試験においては、真空状態から４．０ＭＰａの高圧水素加圧を行った。図５から、例（Ａ２）は、例（Ｂ２）に比べて水素化速度が速く、且つ水素吸蔵量が大であることが判る。
【００２３】
〔実施例３〕
（１）純度が９９．９％であり、且つ粒径Ｄが１０μｍのＭｇ粒子（金属マトリックス粒子）の集合体と、純度が９９．９％であり、且つ粒径ｄが２０ｎｍのＮｉ粒子（添加成分粒子）の集合体とを、合金組成がＭｇ97Ｎｉ3 （数値の単位は原子％）となるように秤量して、合計２．５ｇの混合粉末を得た。この混合粉末を遊星型ボールミル（Furitsch製、Ｐ−５）の容量８０mlのポット（ＪＩＳ ＳＵＳ３１６製）に直径１０mmのボール（ＪＩＳ ＳＵＳ３１６製）１８個と共に入れ、ポット内を１．０ＭＰａの水素ガス雰囲気に保持して、ポット回転数 ７８０rpm 、ディスク回転数 ３６０rpm 、ミリング時間ｔ １５分間の条件でボールミリングを行った。この場合、ポット内には重力加速度Ｇの９倍の加速度９Ｇが発生していた。ボールミリング後、グローブボックス中で水素吸蔵合金粉末を採取した。この合金粉末を例（Ａ３）とする。
【００２４】
例（Ａ３）に実施例１と同一条件で脱水素化処理を施し、次いで例（Ａ３）についてＰＣＴ測定を行った。図６は例（Ａ３）のＰＣＴ特性（収束時間：５分間；３５０℃、放出）を示し、図６において、１回の水素吸放出を行った場合を１サイクルとして複数の黒三角点を結んだ線で表し、また５００サイクル後を複数の黒丸点を結んだ線で表してある。
【００２５】
図６から、例（Ａ３）は優れたＰＣＴ特性を有し、また良好な耐久性を持つことが判る。
【００２６】
（２）前記（１）同様の混合粉末（Ｍｇ97Ｎｉ3 ）を用い、またポット回転数およびディスク回転数を調節してポット内に発生する加速度を、０．５Ｇ，３Ｇ，６Ｇ，９Ｇに変更した、ということを除き、各加速度下にて前記（１）と同一条件で４種の水素吸蔵合金粉末、即ち、０．５Ｇ適用による例（Ａ４）、３Ｇ適用による例（Ａ５）、６Ｇ適用による例（Ａ６）および９Ｇ適用による例（Ａ７）〔例（Ａ３）に同じ〕を製造した。
【００２７】
例（Ａ４）〜（Ａ７）に実施例１と同一条件で脱水素化処理を施し、次いで例（Ａ４）〜（Ａ７）についてＰＣＴ測定を行った。また前記（１）同様の混合粉末（Ｍｇ97Ｎｉ3 ）を用い、真空アーク溶解、インゴットの鋳造および大気中におけるインゴットの粉砕を順次行って得られた粉末の例（Ｂ３）および前記合金組成（Ｍｇ97Ｎｉ3 ）を持つように秤量された前記Ｍｇ粒子およびＮｉ粒子の集合物を乳鉢で混合した例（Ｃ）についても、同様のＰＣＴ測定を行った。
【００２８】
図７は例（Ａ４）〜（Ａ７）、（Ｂ３）、（Ｃ）のＰＣＴ特性（収束時間：５分間；３１０℃、放出）を示す。図７から明らかなように、乳鉢混合による例（Ｃ）は鋳造による例（Ｂ３）よりも優れたＰＣＴ特性を有する。これは超微粒子である高活性なＮｉ粒子の存在に起因する。また加速度０．５Ｇ適用による例（Ａ４）はＭｇとＮｉの合金化の開始とその進行に伴い例（Ｃ）よりもＰＣＴ特性が向上している。加速度３Ｇおよび６Ｇ適用による例（Ａ５）、（Ａ６）は通常の合金製造における加速度９Ｇ適用による例（Ａ７）と同等のＰＣＴ特性を有する。例（Ａ５）、（Ａ６）においては１つのＭｇ粒子内へ侵入したＮｉ粒子の数は例（Ａ７）に比べて少ないが、Ｍｇ粒子表面には多くの高活性なＮｉ粒子が付着しているため、それに起因して優れたＰＣＴ特性が得られる。
【００２９】
〔実施例４〕
純度が９９．９％であり、且つ粒径Ｄが１００μｍのＴｉ粒子（金属マトリックス粒子）の集合体と、純度がそれぞれ９９．９％であり、且つ粒径ｄがそれぞれ１００ｎｍ以下のＣｒ粒子（添加成分粒子）およびＭｎ粒子（添加成分粒子）の集合体とを、合金組成がＴｉ1.2 ＣｒＭｎ（ＣｒのＬ＝３１．２５原子％、ＭｎのＬ＝３１．２５原子％）となるように秤量して、合計２．５ｇの混合粉末を得た。この混合粉末を遊星型ボールミル（Furitsch製、Ｐ−５）の容量８０mlのポット（ＪＩＳ ＳＵＳ３１６製）に直径１０mmのボール（ＪＩＳ ＳＵＳ３１６製）１８個と共に入れ、ポット内を２．０ＭＰａの水素ガス雰囲気に保持して、ポット回転数 ７８０rpm 、ディスク回転数 ３６０rpm 、ミリング時間ｔ １５分間の条件でボールミリングを行った。この場合、ポット内には重力加速度Ｇの９倍の加速度９Ｇが発生していた。ボールミリング後、グローブボックス中で水素吸蔵合金粉末を採取した。この合金粉末を例（Ａ８）とする。
【００３０】
比較のため、前記混合粉末（Ｔｉ1.2 ＣｒＭｎ）を用い、真空アーク溶解、インゴットの鋳造および大気中におけるインゴットの粉砕を順次行って水素吸蔵合金粉末を得た。この合金粉末を例（Ｂ４）とする。
【００３１】
例（Ａ８）に実施例１と同一条件で脱水素化処理を施し、次いで例（Ａ８）、（Ｂ４）についてＰＣＴ測定を行った。図８は例（Ａ８）、（Ｂ４）のＰＣＴ特性（収束時間：５分間；−１０℃、放出）を示す。図８より、例（Ａ８）は例（Ｂ４）よりも優れたＰＣＴ特性を有することが判る。
【００３２】
〔実施例５〕
純度が９９．９％であり、且つ粒径Ｄが１８０μｍのＭｇ粒子（金属マトリックス粒子）の集合体と、純度がそれぞれ９９．９％であり、且つ粒径ｄがそれぞれ２０ｎｍのＮｉ粒子（添加成分粒子）およびＦｅ粒子（添加成分粒子）の集合体とを、合金組成がＭｇ99.5Ｎｉ0.33Ｆｅ0.17（数値の単位は原子％）となるように秤量して、合計１１００ｇの混合粉末を得た。この混合粉末を横型ボールミルの容量２４．１Ｌのポット（ＪＩＳ ＳＵＳ３１６製）に直径１０mmのボール（ＪＩＳ ＳＵＳ３１６製）５５００個と共に入れ、ポット内を１．０ＭＰａの水素ガス雰囲気に保持して、ポット回転数 ６０rpm 、ミリング時間ｔ ６０分間の条件でボールミリングを行った。この場合、ポット内には重力加速度Ｇと同等の１Ｇが発生していた。ボールミリング後、大気中で水素吸蔵合金粉末を採取した。この合金粉末を例（Ａ９）とする。
【００３３】
例（Ａ９）に実施例１と同一条件で脱水素化処理を施し、次いで例（Ａ９）についてＰＣＴ測定を行った。図９は例（Ａ９）のＰＣＴ特性（収束時間：５分間；３１０℃、吸蔵・放出）を示す。図９より、例（Ａ９）は優れたＰＣＴ特性を有し、特に、吸蔵・放出のヒステリシスが小さいことが判る。
【００３４】
なお、本発明は水素吸蔵合金以外の合金粉末、例えば磁性材料粉末、セラミックス分散強化合金用複合粉末、耐熱合金粉末、熱電材料粉末、傾斜機能材料粉末、ニッケル−水素電池の負極用水素吸蔵合金粉末等の製造にも適用される。また添加成分粒子としてはセラミック粒子、金属間化合物粒子等を使用することもある。
【００３５】
【発明の効果】
金属マトリックス粒子の集合体と、添加成分粒子の集合体とを用い、メカニカルアロイングおよびメカニカルグラインディングの一方を行って、添加成分粒子の集合体における少なくとも一部の添加成分粒子を金属マトリックス粒子内に侵入させるようにした高活性な合金粉末を製造するに当り、本発明の第１の特徴によれば、金属マトリックス粒子の粒径ＤがＤ≧３μｍに、また添加成分粒子の粒径ｄがｄ≦５００ｎｍにそれぞれ設定され、また、本発明の第２の特徴によれば、金属マトリックス粒子としてのＭｇ粒子の粒径ＤがＤ≧５μｍに、また添加成分粒子の粒径ｄがｄ≦１００ｎｍにそれぞれ設定される。
【００３６】
このようなｎｍサイズの粒径を持つ添加成分粒子は、微粒子または超微粒子であって、非常に高い活性を有するので、添加成分粒子を金属マトリックス粒子内に侵入させるだけでなく、その金属マトリックス粒子表面に保持させておくことによっても、高活性な水素吸蔵合金粉末を得ることが可能である。しかも上記添加成分粒子は、ｎｍサイズの微粒子または超微粒子であるからミリングによる微細化は不要であって、ミリング時間を大いに短縮することができる。
【図面の簡単な説明】
【図１】 水素吸蔵合金粉末の説明図である。
【図２】 合金粒子の要部を破断した説明図である。
【図３】 水素吸蔵合金粉末の例（Ａ１）、（Ｂ１）のＰＣＴ特性図である。
【図４】 水素吸蔵合金粉末の例（Ａ２）、（Ｂ２）のＰＣＴ特性図である。
【図５】 水素吸蔵合金粉末の例（Ａ２）、（Ｂ２）の水素吸蔵特性図である。
【図６】 水素吸蔵合金粉末の例（Ａ３）のＰＣＴ特性図である。
【図７】 水素吸蔵合金粉末の例（Ａ４）〜（Ａ７）、（Ｂ３）、（Ｃ）のＰＣＴ特性図である。
【図８】 水素吸蔵合金粉末の例（Ａ８）、（Ｂ４）のＰＣＴ特性図である。
【図９】 水素吸蔵合金粉末の例（Ａ９）の水素吸蔵・放出特性図である。
【符号の説明】
１………水素吸蔵合金粉末（合金粉末）
２………金属マトリックス
３………添加成分
４………合金粒子
５………金属マトリックス粒子
６………添加成分粒子[0001]
BACKGROUND OF THE INVENTION
The present invention uses a method for producing an alloy powder, and in particular, an aggregate of metal matrix particles and an aggregate of additive component particles to produce an alloy powder that is an aggregate of alloy particles composed of a metal matrix and an additive component. The present invention relates to a manufacturing method for performing one of mechanical alloying and mechanical grinding.
[0002]
[Prior art]
Conventionally, in this type of manufacturing method, the same or substantially the same particle size (usually 1 μm or more) is used as the metal matrix particles and the additive component particles, and the relatively hard additive component particles are sufficiently refined, A method of uniformly penetrating and dispersing in the metal matrix particles is employed.
[0003]
[Problems to be solved by the invention]
However, the conventional method has a problem that milling for several tens of hours, for example, must be performed in order to make the additive component particles finer and penetrate and disperse, and the production cost of the alloy powder is high.
[0004]
[Means for Solving the Problems]
An object of the present invention is to provide a method for producing the alloy powder capable of greatly reducing the milling time.
[0005]
In order to achieve the above object, according to a first aspect of the present invention , an aggregate of metal matrix particles and additive component particles are used to produce an alloy powder that is an aggregate of alloy particles including a metal matrix and additive components. And performing one of mechanical alloying and mechanical grinding to allow at least some of the additive component particles in the aggregate of additive component particles to enter the metal matrix particles. In the method for producing an alloy powder, in performing the mechanical alloying and mechanical grinding, the particle size D of the metal matrix particles is set to D ≧ 3 μm, and the particle size d of the additive component particles is set to d ≦ 500 nm. A method for producing the alloy powder, which is set respectively , is provided.
[0006]
In order to achieve the above object, according to a second aspect of the present invention, in order to produce a hydrogen storage alloy powder that is an aggregate of alloy particles composed of a metal matrix and an additive component, The assembly of the component particles is used to perform one of mechanical alloying and mechanical grinding so that at least a part of the additive component particles in the aggregate of the additive component particles enter the metal matrix particles. A method for producing an active hydrogen storage alloy powder, wherein the metal matrix particles are Mg particles having a particle size D of D ≧ 5 μm, and the
[0007]
In performing one of mechanical alloying and mechanical grinding using the aggregate of metal matrix particles and the aggregate of additive component particles, according to the first feature, the particle size D of the metal matrix particles is D ≧ D The particle size d of the additive component particles is 3 μm.
d ≦ 500 nm is set, and according to the second feature, the particle diameter D of the Mg particles as the metal matrix particles is set to D ≧ 5 μm, and the particle diameter d of the additive component particles is set to d ≦ 100 nm. but is the additive component particles having a particle size of such a nm size, a fine or ultrafine particles, because they have a very high activity, the additive component particles not only penetrate into the metal matrix particles, It is possible to obtain a highly active hydrogen storage alloy powder by keeping the surface of the metal matrix particles. Further, since the additive component particles are fine particles or ultrafine particles, miniaturization by milling is not necessary.
[0008]
From these facts, according to the above method, the milling time for obtaining the alloy powder can be greatly shortened, for example, from 40 hours to 15 minutes. However, when d> 500 nm , the milling time becomes long, and the production energy becomes inefficient.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
1 and 2, a hydrogen
[0010]
In the production of the hydrogen
[0011]
At that time, the particle size D is D ≧ 3 [mu] m of
[0012]
The
[0013]
In mechanical alloying or mechanical grinding, the milling time t is set to a short time such that 1 minute ≦ t ≦ 5 hours. When the milling time is shortened in this way, as shown in FIG. 2, some of the
[0014]
As described above, the
[0015]
Hereinafter, specific examples to which mechanical alloying is applied will be described.
[0016]
[Example 1]
Aggregates of Mg particles (metal matrix particles) having a purity of 99.9% and a particle size D of 10 μm, and Ni particles (additive component particles) having a purity of 99.9% and a particle size d of 20 nm ) Was weighed so that the alloy composition was Mg 2 Ni (L = 33.3 atomic% of Ni) to obtain a total of 2.5 g of mixed powder. This mixed powder is put in a planetary ball mill (manufactured by Furitsch, P-5) with a capacity of 80 MPa in a pot (manufactured by JIS SUS316) together with 18 balls having a diameter of 10 mm (manufactured by JIS SUS316). The ball milling was performed under the conditions of a pot rotation speed of 780 rpm, a disk rotation speed of 360 rpm, and a milling time t of 15 minutes. In this case, an acceleration 9G that is nine times the gravitational acceleration G occurred in the pot. After ball milling, hydrogen storage alloy powder was collected in a glove box. This alloy powder is taken as an example (A1).
[0017]
For comparison, an aggregate of Mg particles and an aggregate of Ni particles having a purity of 99.9% and a particle diameter d of 10 μm, that is, the same particle diameter as the Mg particles are used, and the milling time t is 40. A hydrogen storage alloy powder was obtained in the same manner as described above except that the time was set. This alloy powder is taken as an example (B1).
[0018]
Since Examples (A1) and (B1) are hydrogenated in the ball milling process, they are subjected to dehydrogenation treatment in which vacuuming is performed at 350 ° C. for 1 hour, and then Example (A1) , (B1) was subjected to PCT measurement. FIG. 3 shows the PCT characteristics (convergence time: 5 minutes; 260 ° C., release) of Examples (A1) and (B1). FIG. 3 shows that Example (A1) was obtained in a short time that is 1/160 of the milling time of Example (B1), but has the same PCT characteristics as Example (B1).
[0019]
[Example 2]
Aggregates of Mg particles (metal matrix particles) having a purity of 99.9% and a particle diameter D of 10 μm, and Fe particles (additive component particles) having a purity of 99.9% and a particle diameter d of 20 nm ) Was weighed so that the alloy composition was Mg 97 Fe 3 (the unit of numerical values was atomic%), and a total of 2.5 g of mixed powder was obtained. This mixed powder is put in a planetary ball mill (manufactured by Furitsch, P-5) with a capacity of 18 MPa in a pot (manufactured by JIS SUS316) with a capacity of 80 ml and a hydrogen gas atmosphere of 2.0 MPa. The ball milling was performed under the conditions of a pot rotation speed of 780 rpm, a disk rotation speed of 360 rpm, and a milling time t of 15 minutes. In this case, an acceleration 9G that is nine times the gravitational acceleration G occurred in the pot. After ball milling, hydrogen storage alloy powder was collected in a glove box. This alloy powder is taken as an example (A2).
[0020]
For comparison, an aggregate of Mg particles and an aggregate of Fe particles having a purity of 99.9% and a particle diameter d of 10 μm, that is, the same particle diameter as that of the Mg particles, and a milling time t of 3 are used. A hydrogen storage alloy powder was obtained in the same manner as described above except that the time was set. This alloy powder is taken as an example (B2).
[0021]
Examples (A2) and (B2) were subjected to dehydrogenation treatment under the same conditions as in Example 1, and then PCT measurement was performed on Examples (A2) and (B2). FIG. 4 shows the PCT characteristics (convergence time: 5 minutes; 310 ° C., release) of Examples (A2) and (B2). FIG. 4 shows that the example (A2) is obtained in a time shorter than 1/12 of the milling time of the example (B2), but has a PCT characteristic superior to that of the example (B2).
[0022]
FIG. 5 shows the hydrogenation rate test results of Examples (A2) and (B2) at a measurement temperature of 310 ° C. In this test, high pressure hydrogen pressurization of 4.0 MPa was performed from a vacuum state. From FIG. 5, it can be seen that Example (A2) has a higher hydrogenation rate and a larger hydrogen storage capacity than Example (B2).
[0023]
Example 3
(1) An aggregate of Mg particles (metal matrix particles) having a purity of 99.9% and a particle diameter D of 10 μm, and Ni particles having a purity of 99.9% and a particle diameter d of 20 nm ( The aggregate of the additive component particles) was weighed so that the alloy composition was Mg 97 Ni 3 (the unit of numerical values was atomic%) to obtain a total of 2.5 g of mixed powder. This mixed powder is put in a planetary ball mill (manufactured by Furitsch, P-5) with a capacity of 80 MPa in a pot (manufactured by JIS SUS316) together with 18 balls having a diameter of 10 mm (manufactured by JIS SUS316). The ball milling was performed under the conditions of a pot rotation speed of 780 rpm, a disk rotation speed of 360 rpm, and a milling time t of 15 minutes. In this case, an acceleration 9G that is nine times the gravitational acceleration G occurred in the pot. After ball milling, hydrogen storage alloy powder was collected in a glove box. This alloy powder is taken as an example (A3).
[0024]
Example (A3) was subjected to dehydrogenation treatment under the same conditions as in Example 1, and then PCT measurement was performed on Example (A3). FIG. 6 shows the PCT characteristics (convergence time: 5 minutes; 350 ° C., release) of Example (A3). In FIG. 6, a plurality of black triangle points are connected with one hydrogen absorption / release as one cycle. It is represented by an ellipse, and after 500 cycles is represented by a line connecting a plurality of black dots.
[0025]
From FIG. 6, it can be seen that the example (A3) has excellent PCT characteristics and good durability.
[0026]
(2) The same mixed powder (Mg 97 Ni 3 ) as in (1) above is used, and the acceleration generated in the pot is adjusted to 0.5G, 3G, 6G, and 9G by adjusting the pot rotation speed and disk rotation speed. Except that it is changed, four hydrogen storage alloy powders under the same conditions as in (1) under the respective accelerations, that is, examples using 0.5G (A4), examples using 3G (A5), and 6G Example (A6) by application and Example (A7) by application of 9G [same as Example (A3)] were prepared.
[0027]
Examples (A4) to (A7) were subjected to dehydrogenation treatment under the same conditions as in Example 1, and then PCT measurements were performed on Examples (A4) to (A7). In addition, using the same mixed powder (Mg 97 Ni 3 ) as described in (1) above, an example of the powder (B3) obtained by sequentially performing vacuum arc melting, ingot casting, and ingot pulverization in the atmosphere, and the alloy composition ( The same PCT measurement was performed for Example (C) in which the aggregate of Mg particles and Ni particles weighed to have Mg 97 Ni 3 ) was mixed in a mortar.
[0028]
FIG. 7 shows the PCT characteristics (convergence time: 5 minutes; 310 ° C., release) of Examples (A4) to (A7), (B3), and (C). As is apparent from FIG. 7, the mortar mixed example (C) has a PCT characteristic superior to the cast example (B3). This is due to the presence of highly active Ni particles that are ultrafine particles. Further, in the example (A4) using the acceleration of 0.5 G, the PCT characteristics are improved as compared with the example (C) with the start and progress of alloying of Mg and Ni. Examples (A5) and (A6) by applying accelerations 3G and 6G have the same PCT characteristics as the example (A7) by applying acceleration 9G in normal alloy production. In Examples (A5) and (A6), the number of Ni particles that have penetrated into one Mg particle is smaller than in Example (A7), but many highly active Ni particles adhere to the Mg particle surface. As a result, excellent PCT characteristics can be obtained.
[0029]
Example 4
Aggregates of Ti particles (metal matrix particles) having a purity of 99.9% and a particle diameter D of 100 μm, and Cr particles having a purity of 99.9% and a particle diameter d of 100 nm or less (each The additive component particles) and the aggregate of Mn particles (additive component particles) are weighed so that the alloy composition is Ti 1.2 CrMn (L = 31.25 atomic% of Cr, L = 31.25 atomic% of Mn). Thus, a total of 2.5 g of mixed powder was obtained. This mixed powder is put in a planetary ball mill (manufactured by Furitsch, P-5) with a capacity of 18 MPa in a pot (manufactured by JIS SUS316) with a capacity of 80 ml and a hydrogen gas atmosphere of 2.0 MPa. The ball milling was performed under the conditions of a pot rotation speed of 780 rpm, a disk rotation speed of 360 rpm, and a milling time t of 15 minutes. In this case, an acceleration 9G that is nine times the gravitational acceleration G occurred in the pot. After ball milling, hydrogen storage alloy powder was collected in a glove box. This alloy powder is taken as an example (A8).
[0030]
For comparison, a hydrogen storage alloy powder was obtained by sequentially performing vacuum arc melting, ingot casting, and ingot pulverization in the air using the mixed powder (Ti 1.2 CrMn). This alloy powder is taken as an example (B4).
[0031]
Example (A8) was subjected to dehydrogenation treatment under the same conditions as in Example 1, and then PCT measurement was performed on Examples (A8) and (B4). FIG. 8 shows the PCT characteristics (convergence time: 5 minutes; −10 ° C., release) of Examples (A8) and (B4). From FIG. 8, it can be seen that Example (A8) has better PCT characteristics than Example (B4).
[0032]
Example 5
Aggregates of Mg particles (metal matrix particles) with a purity of 99.9% and a particle size D of 180 μm, and Ni particles (additional) with a purity of 99.9% and a particle size d of 20 nm each Component particles) and aggregates of Fe particles (additional component particles) were weighed so that the alloy composition would be Mg 99.5 Ni 0.33 Fe 0.17 (the unit of numerical values is atomic%) to obtain a total of 1100 g of mixed powder. . This mixed powder is put together with 5500 balls (made by JIS SUS316) with a diameter of 24.1L in a pot with a horizontal ball mill capacity of 24.1L (made by JIS SUS316), and the inside of the pot is maintained in a 1.0 MPa hydrogen gas atmosphere to rotate the pot. Ball milling was performed under the conditions of several 60 rpm and milling time t 60 minutes. In this case, 1G equivalent to the gravitational acceleration G was generated in the pot. After ball milling, hydrogen storage alloy powder was collected in the atmosphere. This alloy powder is taken as an example (A9).
[0033]
Example (A9) was subjected to dehydrogenation treatment under the same conditions as in Example 1, and then PCT measurement was performed on Example (A9). FIG. 9 shows the PCT characteristics (convergence time: 5 minutes; 310 ° C., occlusion / release) of Example (A9). From FIG. 9, it can be seen that the example (A9) has excellent PCT characteristics, and in particular, the hysteresis of occlusion / release is small.
[0034]
In the present invention, alloy powders other than hydrogen storage alloys, such as magnetic material powders, composite powders for ceramic dispersion strengthened alloys, heat resistant alloy powders, thermoelectric material powders, functionally graded material powders, hydrogen storage alloy powders for negative electrodes of nickel-hydrogen batteries Etc. Moreover, ceramic particles, intermetallic compound particles, or the like may be used as additive component particles.
[0035]
【The invention's effect】
Using the aggregate of metal matrix particles and the aggregate of additive component particles, performing either mechanical alloying or mechanical grinding, and at least some of the additive component particles in the aggregate of additive component particles are contained in the metal matrix particles. per to produce a highly active alloy powder so as to penetrate, according to the first aspect of the present invention, the particle diameter D D ≧ 3 [mu] m of the metal matrix particles and the particle size d of the added component particles Further, according to the second feature of the present invention, the particle size D of the Mg particles as the metal matrix particles is D ≧ 5 μm, and the particle size d of the additive component particles is d ≦ 100 nm. Respectively.
[0036]
The additive component particle having such a particle size of nm size is a fine particle or an ultrafine particle and has a very high activity, so that not only the additive component particle enters the metal matrix particle but also the metal matrix particle. It is also possible to obtain a highly active hydrogen storage alloy powder by keeping it on the surface. Moreover the additive component particles, refining by milling from a nm-sized fine particles or ultrafine particles not be required, it is possible to greatly shorten the milling time.
[Brief description of the drawings]
FIG. 1 is an explanatory view of a hydrogen storage alloy powder.
FIG. 2 is an explanatory view in which a main part of alloy particles is broken.
FIG. 3 is a PCT characteristic diagram of examples (A1) and (B1) of hydrogen storage alloy powder.
FIG. 4 is a PCT characteristic diagram of examples (A2) and (B2) of hydrogen storage alloy powder.
FIG. 5 is a hydrogen storage characteristic diagram of examples (A2) and (B2) of hydrogen storage alloy powder.
FIG. 6 is a PCT characteristic diagram of an example (A3) of a hydrogen storage alloy powder.
FIG. 7 is a PCT characteristic diagram of examples (A4) to (A7), (B3), and (C) of the hydrogen storage alloy powder.
FIG. 8 is a PCT characteristic diagram of examples (A8) and (B4) of hydrogen storage alloy powder.
FIG. 9 is a hydrogen storage / release characteristic diagram of an example (A9) of a hydrogen storage alloy powder.
[Explanation of symbols]
1 ……… hydrogen storage alloy powder (alloy powder)
2 .........
Claims (4)
前記メカニカルアロイングおよびメカニカルグラインディングを行うに当り、前記金属マトリックス粒子（５）の粒径Ｄを Ｄ≧３μｍに、また前記添加成分粒子（６）の粒径ｄを ｄ≦５００ｎｍにそれぞれ設定することを特徴とする、合金粉末の製造方法。In order to produce an alloy powder (1) that is an aggregate of alloy particles (4) composed of a metal matrix (2) and an additive component (3), an aggregate of metal matrix particles (5) and additive component particles (6 ) And performing either mechanical alloying or mechanical grinding, and at least some of the additive component particles (6) in the aggregate of additive component particles (6) are converted into the metal matrix particles (5). A method for producing a highly active alloy powder that is allowed to penetrate into the inside,
In performing the mechanical alloying and mechanical grinding, the particle size D of the metal matrix particles (5) is set to D ≧ 3 μm, and the particle size d of the additive component particles (6) is set to d ≦ 500 nm. A method for producing an alloy powder, characterized in that
前記金属マトリックス粒子（５）は粒径ＤがＤ≧５μｍであるＭｇ粒子であり、また前記添加成分粒子（６）は、粒径ｄがｄ≦１００ｎｍであり、且つＮｉ粒子，Ｎｉ合金粒子，Ｆｅ粒子，Ｆｅ合金粒子，Ｖ粒子，Ｖ合金粒子，Ｍｎ粒子，Ｍｎ合金粒子，Ｔｉ粒子，Ｔｉ合金粒子，Ｃｕ粒子，Ｃｕ合金粒子，Ａｌ粒子，Ａｌ合金粒子，Ｐｄ粒子，Ｐｄ合金粒子，Ｐｔ粒子，Ｐｔ合金粒子，Ｚｒ粒子，Ｚｒ合金粒子，Ａｕ粒子，Ａｕ合金粒子，Ａｇ粒子，Ａｇ合金粒子，Ｃｏ粒子，Ｃｏ合金粒子，Ｍｏ粒子，Ｍｏ合金粒子，Ｎｂ粒子，Ｎｂ合金粒子，Ｃｒ粒子，Ｃｒ合金粒子，Ｚｎ粒子，Ｚｎ合金粒子，Ｒｕ粒子，Ｒｕ合金粒子，Ｒｈ粒子，Ｒｈ合金粒子，Ｔａ粒子，Ｔａ合金粒子，Ｉｒ粒子，Ｉｒ合金粒子，Ｗ粒子およびＷ合金粒子から選択される少なくとも一種であることを特徴とする合金粉末の製造方法。In order to produce hydrogen storage alloy powder (1) which is an aggregate of alloy particles (4) composed of metal matrix (2) and additive component (3), aggregate of metal matrix particles (5) and additive component particles using a collection of (6), I one row of mechanical alloying and mechanical grinding, the metal matrix particles at least part of the additive component particles (6) in the assembly of the additive component particles (6) (5) A method for producing a highly active hydrogen storage alloy powder that is allowed to penetrate into the interior ,
The metal matrix particles (5) are Mg particles having a particle diameter D of D ≧ 5 μm, and the additive component particles (6) have a particle diameter d of d ≦ 100 nm, and Ni particles, Ni alloy particles, Fe particles, Fe alloy particles, V particles, V alloy particles, Mn particles, Mn alloy particles, Ti particles, Ti alloy particles, Cu particles, Cu alloy particles, Al particles, Al alloy particles, Pd particles, Pd alloy particles, Pt Particles, Pt alloy particles, Zr particles, Zr alloy particles, Au particles, Au alloy particles, Ag particles, Ag alloy particles, Co particles, Co alloy particles, Mo particles, Mo alloy particles, Nb particles, Nb alloy particles, Cr particles , Cr alloy particles, Zn particles, Zn alloy particles, Ru particles, Ru alloy particles, Rh particles, Rh alloy particles, Ta particles, Ta alloy particles, Ir particles, Ir alloy particles, W particles and W alloy particles Manufacturing method of the alloy powder, characterized in that at least one element.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001044088A JP3696514B2 (en) | 2000-05-31 | 2001-02-20 | Method for producing alloy powder |
| EP01113224A EP1174385B1 (en) | 2000-05-31 | 2001-05-30 | Process for producing hydrogen absorbing alloy powder, hydrogen absorbing alloy powder, and hydrogen-storing tank for mounting in vehicle |
| DE60106149T DE60106149T2 (en) | 2000-05-31 | 2001-05-30 | Hydrogen-absorbing alloy powder and method for producing the same and fuel tank for storing hydrogen |
| US09/866,783 US6656246B2 (en) | 2000-05-31 | 2001-05-30 | Process for producing hydrogen absorbing alloy powder, hydrogen absorbing alloy powder, and hydrogen-storing tank for mounting in vehicle |
| US10/674,018 US7060120B1 (en) | 2000-05-31 | 2003-09-30 | Hydrogen absorbing alloy powder and hydrogen storing tank for mounting in a vehicle |
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| JP2001044088A JP3696514B2 (en) | 2000-05-31 | 2001-02-20 | Method for producing alloy powder |
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| JP5188317B2 (en) * | 2008-08-08 | 2013-04-24 | 本田技研工業株式会社 | Hydrogen storage material and method for producing the same |
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