JP6892851B2 - 磁心用粉末の製造方法および圧粉磁心の製造方法 - Google Patents
磁心用粉末の製造方法および圧粉磁心の製造方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 56
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- 229910017082 Fe-Si Inorganic materials 0.000 description 2
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
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- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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Description
本発明の圧粉磁心は、純鉄または鉄合金からなる軟磁性粒子と該軟磁性粒子の隣接間にある粒界層とを備える圧粉磁心であって、前記粒界層は、MxFe2-xSiO4(0≦x≦1/M:2価の陽イオンとなる金属元素の一種以上)からなる化合物層を有する。
(1)本発明は、圧粉磁心の原料となる磁心用粉末としても把握できる。すなわち本発明は、純鉄または鉄合金からなる軟磁性粒子と該軟磁性粒子の表面を被覆する被覆層とを有する被覆粒子からなる磁心用粉末であって、前記被覆層は、シリコーン樹脂の表面または内部に、MyFe3-yO4(0≦y≦1/M:2価の陽イオンとなる金属元素の一種以上)で表されるスピネル型フェライトが分散した複合相からなる磁心用粉末でもよい。
上述した磁心用粉末は、例えば、次のような製造方法により得られる。すなわち、純鉄または鉄合金からなる軟磁性粒子の表面をシリコーン樹脂で被覆する樹脂被覆工程と、該シリコーン樹脂の表面または内部に、MyFe3-yO4(0≦y≦1/M:2価の陽イオンとなる金属元素の一種以上)で表されるスピネル型フェライトを生成するフェライト生成工程と、を備える磁心用粉末の製造方法である。
本発明の圧粉磁心は、例えば、上述した磁心用粉末を加圧成形する成形工程を備える製造方法により得られる。磁心用粉末(被覆粒子)の被覆層が複合相からなるときは、さらに、成形工程で得られた成形体を400〜900℃で加熱する焼鈍工程を行うことにより、上述した化合物層を粒界に有する圧粉磁心が得られる。磁心用粉末(被覆粒子)の被覆層が複合相からなるときでも、焼鈍工程を行うことにより、圧粉磁心のヒステリシス損失の低減を図れる。なお、焼鈍工程は非酸化雰囲気中でなされると好適である。
(1)本明細書では、金属元素が単種のみならず、複数種である場合も、便宜的に「M」と略記する。Mが複数種の金属元素を意味する場合、組成割合(原子比率)を示す「x」、「y」は、各金属元素の合計を示す。例えば、MがMnとZnであるとき、「Mx」はMnx1Znx2、x=x1+x2、0<x1・x2を意味する。なお、MxFe2-xSiO4に係る「x」と、MyFe3-yO4に係る「y」とは、同じでも異なっていてもよい。
化合物層はMxFe2-xSiO4(単に「本化合物」ともいう。)からなる。本化合物は、ファイアライト(Fe2SiO4)と同様な斜方晶系の結晶構造からなる。
シリコーン樹脂は、化合物層の生成原料であり、シロキサン結合(−Si−O−Si−結合)を有する高分子化合物である。シリコーン樹脂は、加熱後により軟化しやすく、軟磁性粉末と高い密着性が得られる点で、加熱硬化型樹脂(単に「熱硬化性樹脂」という。)であると好ましい。
フェライトも化合物層の生成原料であり、2価の陽イオンとなる金属元素(M)とFeとOにより、MyFe3-yO4(0≦y≦1、好ましくはy=1)で表される酸化鉄(セラミックス)の一種である。
軟磁性粒子は純鉄または鉄合金からなる。純鉄粉は、高い飽和磁束密度が得られ、圧粉磁心の磁気特性の向上を図り易い。鉄合金粉として、例えば、Si含有鉄合金(Fe−Si合金)粉を用いると、Siによりその電気抵抗率が高められ、圧粉磁心の比抵抗の向上ひいては渦電流損失の低減も図られる。
(1)樹脂被覆工程
樹脂被覆工程は、シリコーン樹脂を軟磁性粒子の表面に塗布することにより行える。シリコーン樹脂の塗布は、例えば、噴霧法や浸漬法等により行える。シリコーン樹脂は、軟磁性粒子の表面を薄く被覆すれば十分であるため、その粘度にも依るが、通常は、溶媒で希釈した樹脂溶液を用いると好ましい。
フェライト生成工程は、例えば、被処理粉末(軟磁性粉末)を反応液(生成液)に浸漬する水溶液法(参照文献:特開2013−191839号公報)、被処理粉末に反応液を噴霧する噴霧法(参照文献:特開2014−183199号公報)、尿素を含む反応液を用いる一液法(参照文献:特開2016−127042号公報)等により行える。いずれの方法によっても、本発明に係るフェライトを生成することが可能である。
(1)成形工程
磁心用粉末は、高圧で成形されるほど、高密度で高磁束密度の圧粉磁心が得られる。但し、過大な成形圧力は、生産性の低下やコストの増加を招く。そこで成形圧力は600〜1600MPaさらには800〜1200MPaで調整されるとよい。なお、金型潤滑温間高圧成形法(日本特許公報特許3309970号公報、日本特許4024705号公報等に詳細)を用いると、金型寿命を延しつつ超高圧成形が可能になる。
焼鈍工程により、成形工程で軟磁性粒子へ導入される歪みが除去され、その歪みに起因したヒステリシス損失が低減される。複合相で被覆された軟磁性粒子(被覆粒子)からなる磁心用粉末を用いた場合、その焼鈍工程により、MxFe2-xSiO4からなる化合物層が圧粉磁心の粒界層として形成される。
圧粉磁心は、比抵抗(特に焼鈍後の比抵抗)が100μΩm以上、1000μΩm以上さらには10000μΩm以上であると好ましい。
(1)軟磁性粉末(原料粉末)
軟磁性粉末として、純鉄からなるガスアトマイズ粉を用いた。その粒度は、212〜106μmとした。粒度の特定は前述した通りである。
熱硬化性樹脂であるシリコーン樹脂(信越化学工業株式会社製 信越シリコーンKR220L)を、イソプロピルアルコールに溶解させた樹脂溶液を調製した。この樹脂溶液を、加熱(60〜100℃)および撹拌している原料粉末に対して噴霧塗布した(塗布工程)。噴霧量は、原料粉末(100質量%)に対してシリコーン樹脂が0.2質量%となるように調整した。
樹脂被覆工程後の軟磁性粉末を、マントルヒーターにより大気中で130℃に加熱しつつ撹拌し、その粉末へフェライト生成液(反応液)を噴霧した。生成液として、次の2種類を用意した。一方の生成液は、モル比で0.5:0.5:2に秤量した塩化マンガン(MnCl2)、塩化亜鉛(ZnCl2)および塩化鉄(FeCl2)をイオン交換水に溶解させて調製した(試料1)。他方の生成液は、塩化鉄(FeCl2)のみをイオン交換水に溶解させて調製した(試料2)。これらの生成液はpH8とした。
比較試料として、上述した樹脂被覆工程を施さずに、試料1と同じ生成液を用いてフェライト生成工程のみを行った磁心用粉末も製造した(試料C1)。
(1)成形工程
各試料に係る磁心用粉末を金型潤滑温間高圧成形法(参照文献:特許3309970号公報、特許4024705号公報)により、1200MPaで成形した。こうしてリング形状(40×30×4mm)の成形体を得た。
各試料に係る成形体を加熱炉に入れて、窒素雰囲気(非酸化雰囲気)中で600℃×1時間加熱した。こうして各試料に係る圧粉磁心を得た。
各試料に係る焼鈍工程前・後の圧粉磁心の比抵抗を、それぞれデジタルマルチメータ(株式会社エーディーシー製R6581)を用いて4端子法(JIS K7194)により測定した。得られた測定結果を図2に示した。
各試料に係る圧粉磁心の断面(主に粒界層)を、透過型電子顕微鏡(TEM)およびエネルギー分散型X線分光法(EDX)により観察した。これにより得られた元素マッピング像の一例(試料1)を図3に示した。
(1)比抵抗と保磁力
図2から明らかなように、熱処理(焼鈍)前および熱処理後の両方で、試料1、2は試料C1よりも高い比抵抗を示した。特に、熱処理後を比較すると明らかなように、試料C1の比抵抗は100μΩm未満にまで急減したのに対して、試料1、2の比抵抗は105μΩm前後という非常に高い状態が維持されていることがわかった。
図3から明らかなように、試料1の粒界層は、Fe、Si、O、MnおよびZnからなり、その厚さは約70nmであった。また、その組成分析結果から、粒界層は、(Mn、Zn)xFe2-xSiO4(x=約0.2)からなる化合物層であることが確認された。同様に、試料2の粒界層も、Fe2SiO4(x=0)からなる化合物層であることを確認している。
Claims (5)
- 純鉄または鉄合金からなる軟磁性粒子の表面に、熱硬化性樹脂であるシリコーン樹脂を塗布する塗布工程と該塗布工程後のシリコーン樹脂を熱硬化させる硬化工程とからなる樹脂被覆工程と、
該熱硬化させたシリコーン樹脂の表面または内部に、MyFe3-yO4(0<y≦1/M:MnおよびZnを少なくとも含む2価の陽イオンとなる金属元素)で表されるスピネル型フェライトを生成するフェライト生成工程と、
を備える磁心用粉末の製造方法。 - 前記フェライト生成工程は、前記シリコーン樹脂の表面に、フェライト生成液を噴霧する噴霧法によりなされる請求項1に記載の磁心用粉末の製造方法。
- 前記Mは、Ni、MgまたはCuの一種以上をさらに含む請求項1または2に記載の磁心用粉末の製造方法。
- 前記yは、0.1≦y≦0.5である請求項1〜3のいずれかに記載の磁心用粉末の製造方法。
- 請求項1〜4のいずれかに記載の製造方法で得られた磁心用粉末を加圧成形する成形工程と、
前記成形工程で得られた成形体を400〜900℃で加熱する焼鈍工程と、
を備える圧粉磁心の製造方法。
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