JP3946150B2 - Method for producing composite soft magnetic material having high density, high resistance and high magnetic flux density - Google Patents
Method for producing composite soft magnetic material having high density, high resistance and high magnetic flux density Download PDFInfo
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- JP3946150B2 JP3946150B2 JP2003029385A JP2003029385A JP3946150B2 JP 3946150 B2 JP3946150 B2 JP 3946150B2 JP 2003029385 A JP2003029385 A JP 2003029385A JP 2003029385 A JP2003029385 A JP 2003029385A JP 3946150 B2 JP3946150 B2 JP 3946150B2
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- 239000000696 magnetic material Substances 0.000 title claims description 41
- 239000002131 composite material Substances 0.000 title claims description 39
- 230000004907 flux Effects 0.000 title claims description 21
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 150
- 239000000843 powder Substances 0.000 claims description 92
- 229910052742 iron Inorganic materials 0.000 claims description 73
- 229910001004 magnetic alloy Inorganic materials 0.000 claims description 68
- 229910017061 Fe Co Inorganic materials 0.000 claims description 60
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 48
- 229910000859 α-Fe Inorganic materials 0.000 claims description 43
- 239000011787 zinc oxide Substances 0.000 claims description 24
- 238000005242 forging Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 3
- 239000011701 zinc Substances 0.000 description 34
- 239000002184 metal Substances 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 12
- 229910020516 Co—V Inorganic materials 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 229910052725 zinc Inorganic materials 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000000700 radioactive tracer Substances 0.000 description 4
- 229910052596 spinel Inorganic materials 0.000 description 4
- 239000011029 spinel Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910001297 Zn alloy Inorganic materials 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- FPVKHBSQESCIEP-JQCXWYLXSA-N pentostatin Chemical compound C1[C@H](O)[C@@H](CO)O[C@H]1N1C(N=CNC[C@H]2O)=C2N=C1 FPVKHBSQESCIEP-JQCXWYLXSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Description
【０００１】
【産業上の利用分野】
この発明は、モータ、アクチュエータ、磁気センサなどの製造に使用される高密度、高抵抗および高磁束密度を有する複合軟磁性材の製造方法に関するものである。
【０００２】
【従来の技術】
一般に、モータ、アクチュエータ、磁気センサなどの磁心にはＦｅ−Ｃｏ系鉄基軟磁性合金粉末を燒結して得られた軟磁性材料が用いられることは知られており、さらに、この軟磁性材料の一つとしてフェライトが知られている。このフェライトは（ＭｅＦｅ）3Ｏ4（ただし、ＭｅはＭｎＺｎ，Ｎｉ，Ｍｇ，Ｃｕ，Ｆｅ，Ｃｏのうちの１種または２種以上）の成分組成を有するスピネル型フェライトであることも知られている。前記Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末などを燒結して得られた軟磁性材料は、飽和磁束密度が高いが、高周波特性が悪く、一方、フェライトなど鉄酸化物粉末を焼結して得られた酸化物軟磁性材料は、抵抗が高いために高周波特性に優れ、初透磁率が比較的高いが、飽和磁束密度が低い欠点があり、これらを改善するために、Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の表面にフェライト膜を被覆してなるフェライト膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末が提案されており、このフェライト膜被覆鉄軟磁性粉末を焼結して得られた材料は高抵抗を有し、飽和磁束密度および高周波特性に共に優れると言われている。
【０００３】
このフェライト膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を製造するための方法として、Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の表面に湿式フェライトメッキによりフェライト膜を形成する方法（特許文献１または２参照）、
Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末およびフェライト粉末を高速衝撃撹拌装置に入れて高速回転させることによりＦｅ−Ｃｏ系鉄基軟磁性合金粉末の表面にフェライト粉末を埋め込み、それによってＦｅ−Ｃｏ系鉄基軟磁性合金粉末の表面にフェライト膜を形成する方法（特許文献３参照）などが知られており、これらフェライト膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を仮圧粉成形して仮圧粉成形体を作製し、得られた仮圧粉成形体を水素雰囲気中でばい焼した後、得られたばい焼体を熱間鍛造することにより複合軟磁性材を製造する方法も知られている。
【０００４】
【特許文献１】
特開昭５６−３８４０２号公報
【特許文献２】
特開平１１−１７０２号公報
【特許文献３】
特開平４−２２６００３号公報
【０００５】
【発明が解決しようとする課題】
しかし、前記Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の表面にフェライト膜を被覆してなる従来のフェライト膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末は、成形性および鍛造性が悪いために、室温鍛造しても十分な密度が得られない。そこで、熱間鍛造して複合軟磁性材を製造すると、複合軟磁性材の密度はある程度向上するが、従来のフェライト膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末は鍛造温度までの加熱時に、芯部のＦｅ−Ｃｏ系鉄基軟磁性合金粉末とフェライト間でフェライトの還元反応が起こり、フェライト（Ｆｅ3Ｏ4）層はウスタイト（ＦｅＯ）層に変化するなどして酸素不足のフェライト膜がＦｅ−Ｃｏ系鉄基軟磁性合金粉末表面に形成され、この酸素不足のフェライト膜は固有抵抗値が低く、したがって得られた複合軟磁性材の抵抗値が十分なものではない。
【０００６】
【課題を解決するための手段】
そこで、本発明者らは、かかる課題を解決すべく研究を行った結果、
（イ）Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末にＺｎ粉末を０．１〜１５質量％添加した混合粉末を加熱しながら撹拌すると、Ｚｎは気化してＺｎ蒸気となり、Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の表面にＺｎ層、Ｚｎ−Ｆｅ合金層、またはＺｎ層およびＺｎ−Ｆｅ合金層からなる複合層（以下、Ｚｎ成分層という）が形成され、このＺｎ成分層が形成されたＦｅ−Ｃｏ系鉄基軟磁性合金粉末を酸化雰囲気中で加熱すると、Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の表面に第１層として酸化亜鉛層が形成され、この酸化亜鉛層が形成されたＦｅ−Ｃｏ系鉄基軟磁性合金粉末の表面に第２層としてフェライト層を被覆して積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を作製し、この積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を原料粉末として仮圧粉成形して仮圧粉成形体を作製し、この仮圧粉成形体を水素雰囲気中でばい焼してばい焼体を作製し、得られたばい焼体を温度：８００〜１２００℃で熱間鍛造して得られた複合軟磁性材は、密度、抵抗および磁束密度が向上する、
（ロ）温度：８００〜１２００℃で熱間鍛造して得られた熱間鍛造体をさらに温度：８００〜１０００℃で焼鈍すると密度、抵抗および磁束密度は一層向上する、という研究結果が得られたのである。
【０００７】
この発明は、かかる研究結果に基づいてなされたものであって、
（１）Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の表面に、酸化亜鉛層を形成し、酸化亜鉛層の上にフェライト層を形成してなる積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を作製し、この積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を仮圧粉成形して仮圧粉成形体を作製し、この仮圧粉成形体を水素雰囲気中でばい焼してばい焼体を作製し、得られたばい焼体を温度：８００〜１２００℃で熱間鍛造する高密度、高抵抗および高磁束密度を有する複合軟磁性材の製造方法、
（２）Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の表面に、酸化亜鉛層を形成し、酸化亜鉛層の上にフェライト層を形成してなる積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を作製し、この積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を仮圧粉成形して仮圧粉成形体を作製し、この仮圧粉成形体を水素雰囲気中でばい焼してばい焼体を作製し、得られたばい焼体を温度：８００〜１２００℃で熱間鍛造し、その後さらに温度：８００〜１０００℃で焼鈍する高密度、高抵抗および高磁束密度を有する複合軟磁性材の製造方法、に特徴を有するものである。
【０００８】
この発明の高密度、高抵抗および高磁束密度を有する複合軟磁性材の製造方法をさらに一層具体的に説明する。
この発明の高密度、高抵抗および高磁束密度を有する複合軟磁性材の製造方法において使用するＦｅ−Ｃｏ系鉄基軟磁性合金粉末は、従来から一般に知られているＣｏ：２５〜６０質量％を含有し、残部がＦｅおよび不可避不純物からなる組成、またはＣｏ：２５〜６０質量％、Ｖ：０．５〜５質量％を含有し、残部がＦｅおよび不可避不純物からなる組成を有するＦｅ−Ｃｏ系軟磁性合金粉末を使用することが好ましい。しかし、この発明の高密度および高透磁性を有する複合軟磁性材の製造方法において使用する前記Ｆｅ−Ｃｏ系軟磁性合金粉末は、前記成分組成を有するＦｅ−Ｃｏ系軟磁性合金粉末に限定されるものではなく、その他のＦｅ−Ｃｏ系軟磁性合金粉末を使用することができる。
この発明でフェライトとは、スピネル構造を有するフェライトであり、（ＭｅＦｅ）3Ｏ4（ただし、ＭｅはＭｎ，Ｚｎ，Ｎｉ，Ｍｇ，Ｃｕ，ＦｅもしくはＣｏまたはこれらの混合物）の組成式で表されるスピネルフェライトである。
そして、これらＦｅ−Ｃｏ系鉄基軟磁性合金粉末は平均粒径：３０〜２００μｍの範囲内にあるＦｅ−Ｃｏ系鉄基軟磁性合金粉末を使用することが好ましい。その理由は、３０μｍよりも平均粒径が小さすぎると、粉末の圧縮性が低下し、Ｆｅ−Ｃｏ系鉄基軟磁性合金の体積割合が低くなるために飽和磁束密度の値が低下するので好ましくなく、一方、平均粒径が２００μｍより大きすぎると、Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末内部の渦電流が増大して高周波における透磁率が低下するので好ましくないことによるものである。
【０００９】
これらＦｅ−Ｃｏ系鉄基軟磁性合金粉末に亜鉛粉末を、亜鉛粉末：０．１〜１０質量％（好ましくは０．３〜５質量％）を添加して混合粉末を作製し、この混合粉末を真空または非酸化性ガスの減圧雰囲気中で温度：３５０〜４００℃に保持しながら撹拌すると、金属Ｚｎは気化して蒸発し、気化したＺｎは軟磁性金属粉末の表面に付着して金属Ｚｎ層または／および合金Γ相（Ｆｅ4Ｚｎ9，Ｆｅ3Ｚｎ10またはＦｅの１部をＡｌ，Ｎｉ，Ｃｒ，Ｓｉで置換した同相）を主体とする合金層であるＺｎ成分層が形成され、Ｚｎ成分層被覆Ｆｅ−Ｃｏ系鉄基軟磁性金属粉末が得られる。このとき使用される亜鉛粉末は粒径が３００μｍ以下であることが好ましい。
なお、亜鉛よりも蒸発し難い金属Ｍ（Ｓｉ，Ｐ，Ｓ，Ｋ，Ｃａ，Ｔｉ，Ｖ，Ｃｒ，Ｍｎ，Ｆｅ，Ｃｏ，Ｎｉ，Ｃｕ，Ｓｒ，Ｙ，Ｚｒ，Ｎｂ，Ｍｏ、Ｐｄ，Ｔａ，Ｗ，Ａｕ）を不純物として１０質量％以下含まれるような低純度の亜鉛粉末または亜鉛合金粉末を使用することができる。これは、加熱・攪拌中にＺｎが先に気化してＦｅ−Ｃｏ系鉄基軟磁性金属粉末の表面にＺｎ蒸着膜を形成し、低純度の亜鉛粉末または亜鉛合金粉末に含まれるＭ金属の蒸発は微量であるところからＦｅ−Ｃｏ系鉄基軟磁性金属粉末の表面のＺｎ蒸着膜に含まれるＭ金属量は極めて微量であり、無視できる程度であるからである。
また、比較的低融点の金属Ｍｅ（Ｌｉ，Ｍｇ，Ａｌ，Ｇａ，Ｇｅ，Ａｇ，Ｉｎ，Ｓｎ，Ｓｂ，Ｂａ，Ｂｉ）粉末をＺｎ粉末と共にＦｅ−Ｃｏ系鉄基軟磁性金属粉末と混合あるいはＺｎ−Ｍｅ合金粉末とＦｅ−Ｃｏ系鉄基軟磁性金属粉末と混合して加熱・撹拌すると、軟磁性金属粉末の表面にＺｎとＭｅの合金あるいはＺｎ合金蒸着膜が形成される。
このＺｎ膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を炭酸ガスなどの酸化雰囲気中、温度：３００〜１０００℃で加熱することによりＺｎ膜が酸化されてＦｅ−Ｃｏ系鉄基軟磁性合金粉末の表面に酸化亜鉛膜が形成される。この酸化亜鉛膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末の酸化亜鉛膜上にフェライト層を形成して積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を作製する。フェライト膜は化学メッキ法、高速衝撃撹拌被覆法またはバインダー被覆法により形成することができる。
【００１０】
このようにして得られた積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を仮圧粉成形して仮圧粉成形体を作製し、この仮圧粉成形体を水素雰囲気中でばい焼してばい焼体を作製し、得られたばい焼体を温度：８００〜１２００℃で熱間鍛造し、その後さらに必要に応じて温度：８００〜１０００℃で焼鈍すると高密度、高抵抗および高磁束密度を有する複合軟磁性材が得られる。
かかる熱間鍛造温度まで加熱し、必要に応じて焼鈍しても、酸化亜鉛層の介在によりフェライトが還元されることがなく、酸化亜鉛とフェライト間ではフェライト相中に酸化亜鉛がわずかに拡散するため、焼結後は非磁性相である酸化亜鉛はフェライト層に拡散し、スピネルフェライトとなって、磁気特性を低下させずに高密度、高抵抗および高磁束密度を有する複合軟磁性材が得られる。
この場合、熱間鍛造温度を８００〜１２００℃に定めたのは、熱間鍛造温度が８００℃未満では十分高密度の複合軟磁性材が得られないと共に酸化亜鉛がフェライトに十分拡散されずに酸化亜鉛層として残存するところから磁気特性が低下するので好ましくなく、一方、１２００℃を越える温度で焼結すると、比抵抗の低下が大きいので好ましくない。
また、この発明において仮圧粉成形体を水素雰囲気中でばい焼する温度は仮圧粉成形体に含まれるバインダーを除去するに十分な温度であればいかなる温度でもよいが、２００〜４００℃の範囲内の温度であれば十分である。
【００１１】
【発明の実施の形態】
原料粉末として、いずれも平均粒径：７０μｍを有するＣｏ：３０質量％を含有し、残部がＦｅおよび不可避不純物からなる組成を有するアトマイズＦｅ−Ｃｏ鉄基軟磁性合金粉末、並びにＣｏ：４９質量％、Ｖ：２質量％を含有し、残部がＦｅおよび不可避不純物からなる組成を有するアトマイズＦｅ−Ｃｏ−Ｖ鉄基軟磁性合金粉末を用意した。
【００１２】
実施例１〜５および比較例１〜２
このＦｅ−Ｃｏ磁性合金粉末に対して純亜鉛粉末を１質量％添加し混合して混合粉末を作製し、この混合粉末を電気炉内の円筒状ボードに装入し、円筒状ボードを回転しながら１×１０-5ｔｏｒｒの真空雰囲気中、温度：３８０℃に１時間加熱することにより亜鉛を気化させ、この亜鉛蒸気中にＦｅ−Ｃｏ系鉄基軟磁性合金粉末を曝すことでその表面にＺｎ被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を作製した。
このＺｎ被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を炭酸ガス中、６５０℃で加熱することによりＺｎ蒸着膜を酸化して酸化亜鉛層を形成し、その後、酸化亜鉛層を形成したＦｅ−Ｃｏ系鉄基軟磁性合金粉末の表面に平均粒径：０.７μｍのフェライト粉末を１〜５質量％分散被覆することにより酸化亜鉛層の上にフェライト層を形成し、積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を作製した。
得られた積層酸化物膜被覆Ｆｅ−Ｃｏ系鉄基軟磁性合金粉末を金型に入れ、プレス成形して外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング状仮圧粉成形体を成形し、得られたリング状仮圧粉成形体を水素ガス雰囲気中、表１に示される温度でばい焼することによりバインダーを除去し、リング状ばい焼体を表１に示される温度で熱間鍛造し、必要に応じて焼鈍することにより複合軟磁性材を作製した。このようにして得られた複合軟磁性材の密度および比抵抗を測定してその結果を表１に示した。さらに複合軟磁性材に巻き線を施し、ＢＨトレーサで直流磁気特性を評価し、同じく、その結果を表１に示した。
【００１３】
従来例１
高速衝撃撹拌法により作製した市販のフェライト膜被覆純Ｆｅ−Ｃｏ鉄基軟磁性合金粉末を用意し、この粉末を用いて実施例１と同様にして複合軟磁性材を得た。このようにして得られた複合軟磁性材の密度および比抵抗を測定してその結果を表１に示した。さらに複合軟磁性材に巻き線を施し、ＢＨトレーサで直流磁気特性を評価し、同じく、その結果を表１に示した。
【００１４】
【表１】
表１に示される結果から、実施例１〜５で作製した複合軟磁性材は、従来例１により製造した複合軟磁性材と比べて密度、比抵抗および磁束密度に優れた特性を示すことが分かる。しかし、比較例１〜２で作製した複合軟磁性材は密度、比抵抗および磁束密度のいずれかが劣るので好ましくないことが分かる。
【００１６】
実施例６〜１０および比較例３〜４
先に用意したアトマイズＦｅ−Ｃｏ−Ｖ系鉄基軟磁性合金粉末に対して純亜鉛粉末を２質量％添加し混合して混合粉末を作製し、この混合粉末を電気炉内の円筒状ボードに装入し、円筒状ボードを回転しながら１×１０-5ｔｏｒｒの真空雰囲気中、温度：４００℃に２時間加熱することにより亜鉛金属を気化させ、この亜鉛蒸気中にＦｅ−Ｃｏ−Ｖ系鉄基軟磁性合金粉末を曝すことでその表面にＺｎ層を形成したＺｎ被覆Ｆｅ−Ｃｏ−Ｖ系鉄基軟磁性合金粉末を作製した。
このＺｎ被覆Ｆｅ−Ｃｏ−Ｖ系鉄基軟磁性合金粉末を炭酸ガス中、７５０℃で加熱することにより亜鉛蒸着膜を酸化して酸化亜鉛層を形成し、その後、酸化亜鉛層を形成したＦｅ−Ｃｏ−Ｖ系鉄基軟磁性合金粉末の表面に平均粒径：０.７μｍのフェライト粉末を１〜５質量％分散被覆することにより酸化亜鉛層の上にフェライト層を形成して積層酸化物膜被覆Ｆｅ−Ｃｏ−Ｖ系鉄基軟磁性合金粉末を作製した。
得られた積層酸化物膜被覆Ｆｅ−Ｃｏ−Ｖ系鉄基軟磁性合金粉末を金型に入れ、プレス成形して外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング状仮圧粉成形体を成形し、得られたリング状仮圧粉成形体を水素ガス雰囲気中、表２に示される温度でばい焼することによりバインダーを除去し、リング状ばい焼体を表２に示される温度で熱間鍛造し、必要に応じて焼鈍することにより複合軟磁性材を作製した。このようにして得られた複合軟磁性材の密度および比抵抗を測定してその結果を表２に示した。さらに複合軟磁性材に巻き線を施し、ＢＨトレーサで直流磁気特性を評価し、同じく、その結果を表２に示した。
【００１７】
従来例２
高速衝撃撹拌法により作製した市販のフェライト膜被覆純Ｆｅ−Ｃｏ−Ｖ鉄基軟磁性合金粉末を用意し、この粉末を用いて実施例１と同様にして複合軟磁性材を得た。このようにして得られた複合軟磁性材の密度および比抵抗を測定してその結果を表３に示した。さらに複合軟磁性材に巻き線を施し、ＢＨトレーサで直流磁気特性を評価し、同じく、その結果を表２に示した。
【００１８】
【表２】
表２に示される結果から、実施例６〜１０で作製した複合軟磁性材は、従来の複合軟磁性材と比べて密度及び比抵抗に優れた特性を示すことが分かる。しかし、比較例３〜４で作製した複合軟磁性材は密度、比抵抗および比透磁率の少なくともいずれか一つが劣るので好ましくないことが分かる。
【００２０】
【発明の効果】
この発明によると、簡単な乾式法により高密度、高抵抗および高磁束密度を有しさらに高周波の比透磁率の高い複合軟磁性材を提供することができ、電気および電子産業において優れた効果をもたらすものである。[0001]
[Industrial application fields]
The present invention relates to a method for manufacturing a composite soft magnetic material having a high density, a high resistance and a high magnetic flux density, which are used for manufacturing motors, actuators, magnetic sensors and the like.
[0002]
[Prior art]
In general, it is known that a soft magnetic material obtained by sintering Fe-Co-based iron-based soft magnetic alloy powder is used for a magnetic core of a motor, an actuator, a magnetic sensor, etc. One is known as ferrite. This ferrite is also known to be a spinel type ferrite having a component composition of (MeFe) 3 O 4 (wherein Me is one or more of MnZn, Ni, Mg, Cu, Fe, Co). Yes. The soft magnetic material obtained by sintering the Fe—Co-based iron-based soft magnetic alloy powder has a high saturation magnetic flux density, but has poor high frequency characteristics, while it is obtained by sintering iron oxide powder such as ferrite. The resulting oxide soft magnetic material has a high resistance due to its high resistance and a relatively high initial magnetic permeability, but has a drawback of a low saturation magnetic flux density. A ferrite film-coated Fe-Co iron-based soft magnetic alloy powder obtained by coating a ferrite film on the surface of a soft magnetic alloy powder has been proposed, and a material obtained by sintering this ferrite film-coated iron soft magnetic powder Has high resistance and is said to be excellent in both saturation magnetic flux density and high frequency characteristics.
[0003]
As a method for producing the ferrite film-coated Fe—Co iron-based soft magnetic alloy powder, a method of forming a ferrite film on the surface of the Fe—Co iron-based soft magnetic alloy powder by wet ferrite plating (Patent Document 1 or 2),
Fe-Co based iron-based soft magnetic alloy powder and ferrite powder are placed in a high-speed impact stirrer and rotated at high speed to embed ferrite powder on the surface of the Fe-Co based iron-based soft magnetic alloy powder, thereby Fe-Co based A method of forming a ferrite film on the surface of an iron-based soft magnetic alloy powder (see Patent Document 3) is known. These ferrite film-coated Fe-Co iron-based soft magnetic alloy powders are temporarily compacted by temporary compaction. A method is also known in which a compacted green body is prepared, and the obtained temporary green compact is roasted in a hydrogen atmosphere, and then the resulting roasted body is hot forged to produce a composite soft magnetic material. ing.
[0004]
[Patent Document 1]
JP 56-38402 A [Patent Document 2]
Japanese Patent Laid-Open No. 11-1702 [Patent Document 3]
JP-A-4-226003
[Problems to be solved by the invention]
However, the conventional ferrite film-coated Fe-Co iron-based soft magnetic alloy powder obtained by coating the surface of the Fe-Co iron-based soft magnetic alloy powder with a ferrite film has poor formability and forgeability, Even if it is forged at room temperature, sufficient density cannot be obtained. Therefore, when the composite soft magnetic material is manufactured by hot forging, the density of the composite soft magnetic material is improved to some extent, but the conventional ferrite film-coated Fe-Co iron-based soft magnetic alloy powder is heated to the forging temperature, A ferrite reduction reaction takes place between the Fe—Co iron-based soft magnetic alloy powder and ferrite in the core, and the ferrite (Fe 3 O 4 ) layer changes to a wustite (FeO) layer. The ferrite film formed on the surface of the Fe—Co-based iron-based soft magnetic alloy powder and having an oxygen deficiency has a low specific resistance value, and thus the obtained composite soft magnetic material has an insufficient resistance value.
[0006]
[Means for Solving the Problems]
Then, as a result of conducting research to solve such a problem, the present inventors,
(A) When a mixed powder obtained by adding 0.1 to 15% by mass of Zn powder to Fe—Co based iron-based soft magnetic alloy powder is stirred while heating, Zn is vaporized to become Zn vapor, and Fe—Co based iron based On the surface of the soft magnetic alloy powder, a Zn layer, a Zn—Fe alloy layer, or a composite layer composed of a Zn layer and a Zn—Fe alloy layer (hereinafter referred to as a Zn component layer) is formed, and the Fe on which the Zn component layer is formed. When the Co-based iron-based soft magnetic alloy powder is heated in an oxidizing atmosphere, a zinc oxide layer is formed as a first layer on the surface of the Fe-Co-based iron-based soft magnetic alloy powder, and the Fe-cobalt in which this zinc oxide layer is formed The surface of the Co-based iron-based soft magnetic alloy powder is coated with a ferrite layer as a second layer to produce a laminated oxide film-coated Fe-Co-based iron-based soft magnetic alloy powder, and this laminated oxide film-coated Fe-Co Iron-based soft magnetic alloy powder as raw material powder Powder compacting is performed to prepare a temporary compacted body, and this temporary compacted compact is roasted in a hydrogen atmosphere to prepare a roasted body, and the obtained roasted body is heated at a temperature of 800 to 1200 ° C. The composite soft magnetic material obtained by hot forging improves the density, resistance and magnetic flux density.
(B) A study result is obtained that the density, resistance and magnetic flux density are further improved when the hot forged body obtained by hot forging at 800 to 1200 ° C is further annealed at 800 to 1000 ° C. It was.
[0007]
The present invention has been made based on the results of such research,
(1) Fe-Co-based iron-based soft magnetism coated with a laminated oxide film in which a zinc oxide layer is formed on the surface of an Fe-Co-based iron-based soft magnetic alloy powder and a ferrite layer is formed on the zinc oxide layer An alloy powder is prepared, and this laminated oxide film-coated Fe-Co-based iron-based soft magnetic alloy powder is temporarily compacted to produce a temporary compacted body, and this temporary compacted body is placed in a hydrogen atmosphere. A method for producing a composite soft magnetic material having a high density, a high resistance and a high magnetic flux density, wherein a roasted body is produced by baking, and the obtained roasted body is hot forged at a temperature of 800 to 1200 ° C.
(2) Fe-Co iron-based soft magnetic alloy coated with a laminated oxide film in which a zinc oxide layer is formed on the surface of Fe-Co iron-based soft magnetic alloy powder and a ferrite layer is formed on the zinc oxide layer An alloy powder is prepared, and this laminated oxide film-coated Fe-Co-based iron-based soft magnetic alloy powder is temporarily compacted to produce a temporary compacted body, and this temporary compacted body is placed in a hydrogen atmosphere. A roasted body is produced by baking, and the obtained roasted body is hot forged at a temperature of 800 to 1200 ° C., and then annealed at a temperature of 800 to 1000 ° C., with high density, high resistance and high magnetic flux density. It has the characteristics in the manufacturing method of the composite soft magnetic material which has.
[0008]
The method for producing a composite soft magnetic material having high density, high resistance and high magnetic flux density according to the present invention will be described more specifically.
The Fe—Co-based iron-based soft magnetic alloy powder used in the method for producing a composite soft magnetic material having high density, high resistance and high magnetic flux density according to the present invention is conventionally known as Co: 25-60 mass%. In which the balance is composed of Fe and inevitable impurities, or Co: 25-60 mass%, V: 0.5-5 mass%, and the balance is composed of Fe and inevitable impurities. It is preferable to use a soft magnetic alloy powder. However, the Fe—Co based soft magnetic alloy powder used in the method for producing a composite soft magnetic material having high density and high permeability according to the present invention is limited to the Fe—Co based soft magnetic alloy powder having the above component composition. Other Fe—Co based soft magnetic alloy powders can be used.
The ferrite in the present invention is a ferrite having a spinel structure, and is represented by a composition formula of (MeFe) 3 O 4 (where Me is Mn, Zn, Ni, Mg, Cu, Fe or Co or a mixture thereof). Spinel ferrite.
The Fe—Co iron-based soft magnetic alloy powder is preferably an Fe—Co iron-based soft magnetic alloy powder having an average particle size of 30 to 200 μm. The reason is that if the average particle diameter is too small than 30 μm, the compressibility of the powder is lowered, and the volume fraction of the Fe—Co-based iron-based soft magnetic alloy is lowered, so the value of the saturation magnetic flux density is lowered. On the other hand, if the average particle diameter is larger than 200 μm, the eddy current inside the Fe—Co-based iron-based soft magnetic alloy powder increases and the magnetic permeability at high frequency decreases, which is not preferable.
[0009]
Zinc powder and zinc powder: 0.1 to 10% by mass (preferably 0.3 to 5% by mass) are added to these Fe—Co-based iron-based soft magnetic alloy powders to produce mixed powders. Is stirred in a vacuum or in a reduced-pressure atmosphere of a non-oxidizing gas at a temperature of 350 to 400 ° C., the metal Zn evaporates and evaporates, and the vaporized Zn adheres to the surface of the soft magnetic metal powder and becomes metal Zn. A Zn component layer, which is an alloy layer mainly composed of a layer or / and an alloy Γ phase (Fe 4 Zn 9 , Fe 3 Zn 10 or the same phase in which part of Fe is replaced with Al, Ni, Cr, Si), is formed, A Zn component layer-coated Fe—Co-based iron-based soft magnetic metal powder is obtained. The zinc powder used at this time preferably has a particle size of 300 μm or less.
In addition, metal M (Si, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Sr, Y, Zr, Nb, Mo, Pd, Ta, which is harder to evaporate than zinc. , W, Au), low-purity zinc powder or zinc alloy powder containing 10% by mass or less as impurities can be used. This is because Zn vaporizes first during heating and stirring to form a Zn deposited film on the surface of the Fe-Co-based iron-based soft magnetic metal powder, and the M metal contained in the low-purity zinc powder or zinc alloy powder. This is because the amount of M metal contained in the Zn deposited film on the surface of the Fe—Co-based iron-based soft magnetic metal powder is extremely small and negligible because evaporation is very small.
Further, a metal Me (Li, Mg, Al, Ga, Ge, Ag, In, Sn, Sb, Ba, Bi) powder having a relatively low melting point is mixed with an Fe—Co-based iron-based soft magnetic metal powder together with a Zn powder. When the Zn-Me alloy powder and the Fe-Co iron-based soft magnetic metal powder are mixed and heated and stirred, an alloy of Zn and Me or a deposited Zn alloy film is formed on the surface of the soft magnetic metal powder.
The Zn film is heated by heating the Zn film-coated Fe—Co based iron-based soft magnetic alloy powder at a temperature of 300 to 1000 ° C. in an oxidizing atmosphere such as carbon dioxide gas, whereby the Fe—Co based iron based soft magnetic alloy powder. A zinc oxide film is formed on the surface. A ferrite layer is formed on the zinc oxide film of the zinc oxide film-coated Fe-Co iron-based soft magnetic alloy powder to produce a laminated oxide film-coated Fe-Co iron-based soft magnetic alloy powder. The ferrite film can be formed by a chemical plating method, a high-speed impact stirring coating method, or a binder coating method.
[0010]
The laminated oxide film-coated Fe—Co iron-based soft magnetic alloy powder thus obtained is temporarily compacted to produce a temporary compacted body, and this temporary compacted body is placed in a hydrogen atmosphere. A roasted body is produced by baking, and the obtained roasted body is hot-forged at a temperature of 800 to 1200 ° C., and then further annealed at a temperature of 800 to 1000 ° C. as necessary. A composite soft magnetic material having a high magnetic flux density is obtained.
Even if heated to such a hot forging temperature and annealed as necessary, the ferrite is not reduced by the inclusion of the zinc oxide layer, and the zinc oxide slightly diffuses between the zinc oxide and the ferrite in the ferrite phase. Therefore, after sintering, zinc oxide, which is a non-magnetic phase, diffuses into the ferrite layer and becomes spinel ferrite, and a composite soft magnetic material having high density, high resistance, and high magnetic flux density is obtained without deteriorating magnetic properties. It is done.
In this case, the hot forging temperature was set to 800 to 1200 ° C. because if the hot forging temperature was less than 800 ° C., a sufficiently high density composite soft magnetic material could not be obtained and the zinc oxide was not sufficiently diffused into the ferrite. Since the magnetic properties are lowered from the point where it remains as the zinc oxide layer, sintering at a temperature exceeding 1200 ° C. is not preferred because the specific resistance is greatly lowered.
In this invention, the temperature at which the green compact is roasted in a hydrogen atmosphere may be any temperature as long as it is sufficient to remove the binder contained in the green compact, but is 200 to 400 ° C. A temperature within the range is sufficient.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
As raw material powders, all contain Co: 30% by mass having an average particle diameter of 70 μm, and the balance Fe-Co iron-based soft magnetic alloy powder having a composition consisting of Fe and inevitable impurities, and Co: 49% by mass V: 2% by mass Atomized Fe—Co—V iron-based soft magnetic alloy powder having a composition consisting of Fe and inevitable impurities was prepared.
[0012]
Examples 1-5 and Comparative Examples 1-2
1% by mass of pure zinc powder is added to and mixed with the Fe-Co magnetic alloy powder to produce a mixed powder. The mixed powder is charged into a cylindrical board in an electric furnace, and the cylindrical board is rotated. However, in a vacuum atmosphere of 1 × 10 −5 torr, the zinc was vaporized by heating to 380 ° C. for 1 hour, and the surface of the zinc vapor was exposed to the Fe—Co-based iron-based soft magnetic alloy powder. A Zn-coated Fe—Co-based iron-based soft magnetic alloy powder was prepared.
The Zn-coated Fe—Co iron-based soft magnetic alloy powder is heated in carbon dioxide gas at 650 ° C. to oxidize the Zn vapor-deposited film to form a zinc oxide layer, and then to form the zinc oxide layer Fe—Co The ferrite layer is formed on the zinc oxide layer by dispersing and coating 1 to 5% by mass of ferrite powder having an average particle diameter of 0.7 μm on the surface of the iron-based soft magnetic alloy powder, and the laminated oxide film-coated Fe- Co-based iron-based soft magnetic alloy powder was prepared.
The obtained laminated oxide film-coated Fe—Co-based iron-based soft magnetic alloy powder is placed in a mold and press-molded to form a ring-shaped temporary compact having outer diameter: 35 mm, inner diameter: 25 mm, and height: 5 mm. The molded body is molded, and the obtained ring-shaped temporary compacted body is roasted at a temperature shown in Table 1 in a hydrogen gas atmosphere to remove the binder, and the ring-shaped roasted body is shown in Table 1. A composite soft magnetic material was produced by hot forging at a temperature and annealing as necessary. The density and specific resistance of the composite soft magnetic material thus obtained were measured and the results are shown in Table 1. Further, the composite soft magnetic material was wound, and the DC magnetic characteristics were evaluated with a BH tracer. The results are also shown in Table 1.
[0013]
Conventional Example 1
A commercially available ferrite film-coated pure Fe—Co iron-based soft magnetic alloy powder prepared by a high-speed impact stirring method was prepared, and a composite soft magnetic material was obtained using this powder in the same manner as in Example 1. The density and specific resistance of the composite soft magnetic material thus obtained were measured and the results are shown in Table 1. Further, the composite soft magnetic material was wound, and the DC magnetic characteristics were evaluated with a BH tracer. The results are also shown in Table 1.
[0014]
[Table 1]
From the results shown in Table 1, it can be seen that the composite soft magnetic materials produced in Examples 1 to 5 have excellent properties in density, specific resistance, and magnetic flux density as compared with the composite soft magnetic material produced in Conventional Example 1. I understand. However, it can be seen that the composite soft magnetic materials prepared in Comparative Examples 1 and 2 are not preferable because any one of density, specific resistance, and magnetic flux density is inferior.
[0016]
Examples 6-10 and Comparative Examples 3-4
2% by mass of pure zinc powder is added to the previously prepared atomized Fe-Co-V iron-based soft magnetic alloy powder and mixed to prepare a mixed powder. This mixed powder is applied to a cylindrical board in an electric furnace. The zinc metal was vaporized by heating and heating to 400 ° C. for 2 hours in a vacuum atmosphere of 1 × 10 −5 torr while rotating the cylindrical board, and Fe—Co—V system in this zinc vapor A Zn-coated Fe-Co-V iron-based soft magnetic alloy powder in which a Zn layer was formed on the surface of the iron-based soft magnetic alloy powder was produced.
The Zn-coated Fe—Co—V-based iron-based soft magnetic alloy powder is heated in carbon dioxide gas at 750 ° C. to oxidize the zinc vapor-deposited film to form a zinc oxide layer. -A ferrite layer is formed on a zinc oxide layer by dispersing and coating 1 to 5% by mass of a ferrite powder having an average particle size of 0.7 μm on the surface of a Co—V iron-based soft magnetic alloy powder, thereby forming a laminated oxide Film-coated Fe—Co—V-based iron-based soft magnetic alloy powder was prepared.
The obtained laminated oxide film-coated Fe—Co—V iron-based soft magnetic alloy powder is put into a mold and press-molded to have a ring-shaped temporary shape having an outer diameter: 35 mm, an inner diameter: 25 mm, and a height: 5 mm. The green compact is molded, and the resulting ring-shaped temporary green compact is roasted at a temperature shown in Table 2 in a hydrogen gas atmosphere to remove the binder. A composite soft magnetic material was produced by hot forging at the indicated temperature and annealing as necessary. The density and specific resistance of the composite soft magnetic material thus obtained were measured and the results are shown in Table 2. Further, the composite soft magnetic material was wound and the DC magnetic characteristics were evaluated with a BH tracer. The results are also shown in Table 2.
[0017]
Conventional example 2
A commercially available ferrite film-coated pure Fe—Co—V iron-based soft magnetic alloy powder prepared by a high-speed impact stirring method was prepared, and a composite soft magnetic material was obtained using this powder in the same manner as in Example 1. The density and specific resistance of the composite soft magnetic material thus obtained were measured and the results are shown in Table 3. Further, the composite soft magnetic material was wound and the DC magnetic characteristics were evaluated with a BH tracer. The results are also shown in Table 2.
[0018]
[Table 2]
From the results shown in Table 2, it can be seen that the composite soft magnetic materials produced in Examples 6 to 10 have characteristics excellent in density and specific resistance as compared with conventional composite soft magnetic materials. However, it can be seen that the composite soft magnetic materials produced in Comparative Examples 3 to 4 are not preferable because at least one of density, specific resistance, and relative permeability is inferior.
[0020]
【The invention's effect】
According to the present invention, it is possible to provide a composite soft magnetic material having a high density, a high resistance and a high magnetic flux density and a high relative permeability at a high frequency by a simple dry method, and has an excellent effect in the electrical and electronic industries. Is what it brings.
Claims (4)
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