JP6761742B2 - 高周波で用いる磁性粉末およびこれを含有する磁性樹脂組成物 - Google Patents
高周波で用いる磁性粉末およびこれを含有する磁性樹脂組成物 Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims description 29
- 239000011342 resin composition Substances 0.000 title claims description 13
- 230000005415 magnetization Effects 0.000 claims description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 33
- 239000000843 powder Substances 0.000 description 27
- 229910000734 martensite Inorganic materials 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 229910045601 alloy Inorganic materials 0.000 description 12
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910002796 Si–Al Inorganic materials 0.000 description 2
- 229910008458 Si—Cr Inorganic materials 0.000 description 2
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- 229910000859 α-Fe Inorganic materials 0.000 description 2
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- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 241000053208 Porcellio laevis Species 0.000 description 1
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- 229910008318 Si—M Inorganic materials 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
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- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
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- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Description
(1)質量%で、C:0.2〜5.0%、4〜6族の元素,Mn,Niの1種または2種以上を合計で0.1〜30%含み、残部がFeまたは/およびCo(Coは0%を含む)、および不可避的不純物からなり、飽和磁化が1.0T超であり、下記の式(1)を満たすことを特徴とした高周波で用いる磁性粉末。
Co%/(Co%+Fe%)≦0.50 ・・・ (1)
C%+B%+N%+P%≦5.0% ・・・ (2)
Ti%+Zr%+Hf%+V%+Nb%+Ta%+Cr%+Mo%+W%+Mn%+Ni%+Cu%+Al%+Si%≦30 ・・・ (3)
(4)前記(1)〜(3)のいずれか1に記載された高周波で用いる磁性粉末を含有することを特徴とする磁性樹脂組成物にある。
C:0.2〜5.0%
本発明において、CはFRを上昇させるための必須元素である。Cを多く含むFe基合金は、急冷凝固、焼入れ、塑性加工などにより、Cおよび転位を多量に含有するマルテンサイト相が生成し、この相を多く含む粉末のFRが極めて高いことを見出した。したがって、本発明磁性粉末の製造方法としては、水アトマイズ、ガスアトマイズ、ディスクアトマイズなど各種アトマイズ法のような急冷凝固による方法や、粉砕法や扁平加工のような塑性加工をともなう方法によることが好ましい。また、これらの方法で十分なマルテンサイト相が得られない場合、焼入れ処理によりマルテンサイト相を生成させることができる。ここで、C量が0.2%未満ではFRが低く、5.0%を超えると飽和磁化が低下する。好ましい範囲は、0.4を超え4.0%未満、より好ましくは0.8を超え3.5%未満、さらに好ましくは1.5%を超え3.0%未満である。
本発明において、4〜6族の元素(具体的には、Ti,Zr,Hf,V,Nb,Ta,Cr,Mo,W),Mn,Niは、焼入れ性を改善する効果、FRを増加させる効果のほか、粉末の発火性を低下させる効果もある必須元素であり、その合計量で扱うことができる。4〜6族の元素は、詳細な原因は不明であるが、炭化物を形成するためと推測され、特にFR上昇の効果が高い。Mnは焼入れ性改善の効果が特に高い。Niは発火性低下の効果が特に高い。合計量が0.1%未満ではこれらの効果が得られず、30%を超えると飽和磁化が低下する。好ましくは合計量で2%を超え25%未満、より好ましくは4%を超え10%未満である。
本発明において、Fe,Coは飽和磁化が高い強磁性を有するマルテンサイト相を生成するための必須元素である。また、いわゆるスレーターポーリング曲線として知られるように、FeとCoの比率により飽和磁化は影響を受け、Co%/(Co%+Fe%)が0.5を超えると、飽和磁化が低下するとともにコスト高である。好ましくは0.01を超え0.40未満、より好ましくは0.10を超え0.35未満である。
磁性部品の小型化、薄肉化および直流重畳特性の観点から、1.0Tを超える高い飽和磁化が必要である。好ましくは1.10Tを超え、より好ましくは1.25Tを超えるものである。
本発明において、B,N,PはCほどではないがFRを上昇させる効果があり、B,PはCと同様に半金属・半導体元素であり、NはCと同様にFeに対し侵入型元素であり、それぞれ、Cの一部と置換することができる。合計で2%を超えると、合金の硬さが過度に上昇し、この粉末を含有する磁性部品の製造の際に掛けられるプレスによる磁性粉末の充填率増加が十分でなくなる。好ましくは合計で0.01%を超え1%未満、より好ましくは0.1を超え0.5%未満である。また、C%+B%+N%+P%が5.0%を超えると、飽和磁化が低下する。好ましい範囲は、0.4を超え4.0%未満、より好ましくは0.8を超え3.5%未満、さらに好ましくは1.5%を超え3.0%未満である。
本発明において、Cu,Al,Siは耐食性を改善することができるため、必要に応じ添加可能な元素である。ただし、10%を超えて添加すると焼入れ性が劣化し、十分なFRが得られない。好ましくは0.1を超え5%未満、より好ましくは2%を超え3%未満である。また、Ti%+Zr%+Hf%+V%+Nb%+Ta%+Cr%+Mo%+W%+Mn%+Ni%+Cu%+Al%+Si%が30%を超えると飽和磁化が低下する。好ましくは合計量で2%を超え25%未満、より好ましくは4%を超え10%未満である。
(粉末の作製)
水アトマイズ法、ガスアトマイズ法、ディスクアトマイズ法または溶融による合金化後の粉砕法(鋳造粉砕法)のいずれかにより所定の成分の粉末を作製し、所定の目開きの網を用い分級した振るい下の粒度を評価に用いた。各種アトマイズは従来提案されている一般的な方法で可能であり、アルミナ製坩堝を溶解に用い、坩堝下の直径2mmのノズルから合金溶湯を出湯し、これに高圧水を噴霧し溶湯を分断、高圧ガス(アルゴンまたは窒素)を噴霧し溶湯を分断、または回転ディスクにより遠心力で溶湯を分断することで実施した。なお、N量は高濃度のNを含む原料を選定すること、もしくは/および、アトマイズに高圧窒素ガスを選定することで調整可能である。これら粉末の一部には、Ar雰囲気炉により、焼入れおよび/もしくは焼戻し処理を実施した。これら処理は、所定の温度、時間で保持した後、炉冷とした。
得られた粉末の平均粒径、飽和磁化、平均結晶粒径、マルテンサイト相および残留オーステナイト相の面積率、透磁率を評価した。平均粒径はレーザー回折法、飽和磁化はVSM装置により評価した。平均結晶粒径、マルテンサイト相および残留オーステナイト相の面積率は、樹脂埋め研磨試料をエッチングした光学顕微鏡像を画像解析し評価した。
磁性樹脂組成物として、薄肉の磁性シートを作製し、透磁率を評価した。粉末以外の磁性シートの構成としては、従来提案されている一般的な構成が適用可能であり、磁性シート作製も従来提案されている一般的な方法で可能である。トルエンに塩素化ポリエチレンを溶解し、これに得られた粉末を混合、分散した。この分散液をポリエステル樹脂に厚さ400μm程度に塗布し、常温常湿で乾燥させた。その後、130℃、15MPaの圧力でプレス加工し、磁性シートを得た。磁性シートのサイズは150mm×150mmで厚さは200μmである。なお、磁性シート中の粉末の体積充填率はいずれも約65%であった。次に、この磁性シートを、外径7mm、内径3mmのドーナツ状に切り出し、インピーダンス測定器により、室温でインピーダンス特性の周波数特性を測定し、その結果から得られた透磁率(μ’およびμ”)よりtanδを算出し、これが0.1となる周波数、すなわちFRにより高周波特性の評価とした。
それに加えて、総合的評価は以下の通りである。
(1)保磁力メータにより測定した実施例粉末の保磁力は、いずれも2400A/m以上であり、測定上限範囲以上であった。
(2)埋め込み研磨試料を用いた光学顕微鏡観察の結果、実施例粉末の主相はいずれもマルテンサイト相であった。
(3)実施例および比較例の粉末を45μm以下に分級し、試料1gにてハルトマン式爆発実験を行った結果、比較例No.81〜92のみが大きな炎が発生した。
(4)比較例No.72〜75の磁性シートは、厚さ250〜300μmであり、実施例および他の比較例の磁性シートの厚さ180〜220μmと比較し厚かった。すなわち、比較例No.72〜75の粉末は、プレス加工によるシートの充填率増加が十分ではない。
比較例No.65は、C含有量が高く、かつ式(2)の値が大きいために、飽和磁化が低い。比較例No.66は、C含有量が低いために、tanδが0.1に到達する周波数FRが低い。比較例No.67は、比較例No.66と同様に、C含有量が0のために、FRが低い。比較例No.68は、4〜6族の元素,Mn,Niの1種または2種以上の合計(A)の含有量が高いために、飽和磁化が低い。比較例No.69は、(A)の含有量が高く、かつ式(3)の値が大きいために、飽和磁化が低い。
特許出願人 山陽特殊製鋼株式会社
代理人 弁理士 椎 名 彊
Claims (4)
- 質量%で、C:0.2〜5.0%、4〜6族の元素,Mn,Niの1種または2種以上を合計で0.1〜30%含み、残部がFeまたは/およびCo(Coは0%を含む)、および不可避的不純物からなり、飽和磁化が1.0T超であり、下記の式(1)を満たすことを特徴とした高周波で用いる磁性粉末。
Co%/(Co%+Fe%)≦0.50 ・・・ (1) - 上記Cの一部がB,N,Pの1種または2種以上に置換されており、
質量%で、B,N,Pの1種または2種以上を合計で2%以下含み、下記の式(2)を満たすことを特徴とした請求項1に記載の高周波で用いる磁性粉末。
C%+B%+N%+P%≦5.0%・・・ (2) - 質量%で、C:0.2〜5.0%、4〜6族の元素,Mn,Niの1種または2種以上を合計で0.1〜30%、Cu,Al,Siの1種または2種以上を合計で10%以下含み、残部がFeまたは/およびCo(Coは0%を含む)、および不可避的不純物からなり、飽和磁化が1.0T超であり、下記の式(1)及び式(3)を満たすことを特徴とした高周波で用いる磁性粉末。
Co%/(Co%+Fe%)≦0.50 ・・・ (1)
Ti%+Zr%+Hf%+V%+Nb%+Ta%+Cr%+Mo%+W%+Mn%+Ni%+Cu%+Al%+Si%≦30・・・ (3) - 請求項1〜3のいずれか1項に記載された高周波で用いる磁性粉末を含有することを特徴とする磁性樹脂組成物。
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