JP5556982B2 - 強磁性金属粒子粉末及びその製造法、並びに磁気記録媒体 - Google Patents
強磁性金属粒子粉末及びその製造法、並びに磁気記録媒体 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims description 145
- 230000005291 magnetic effect Effects 0.000 title claims description 72
- 230000005294 ferromagnetic effect Effects 0.000 title claims description 70
- 239000002923 metal particle Substances 0.000 title claims description 70
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 239000002245 particle Substances 0.000 claims description 127
- 229910052598 goethite Inorganic materials 0.000 claims description 38
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 claims description 38
- 229910052595 hematite Inorganic materials 0.000 claims description 23
- 239000011019 hematite Substances 0.000 claims description 23
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims description 23
- 239000011882 ultra-fine particle Substances 0.000 claims description 19
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- 239000011230 binding agent Substances 0.000 claims description 13
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 230000009467 reduction Effects 0.000 description 12
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- 238000010438 heat treatment Methods 0.000 description 11
- 230000005415 magnetization Effects 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
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- 125000003118 aryl group Chemical group 0.000 description 3
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
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- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
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- 229910052581 Si3N4 Inorganic materials 0.000 description 2
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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 2
- 230000005540 biological transmission Effects 0.000 description 2
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- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
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- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 1
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- RNXZADVBNGOJOL-UHFFFAOYSA-N [Sb+]=O.[Sn+2]=O.[O-2].[Ti+4] Chemical compound [Sb+]=O.[Sn+2]=O.[O-2].[Ti+4] RNXZADVBNGOJOL-UHFFFAOYSA-N 0.000 description 1
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- 150000002505 iron Chemical class 0.000 description 1
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
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- 238000002834 transmittance Methods 0.000 description 1
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- Magnetic Record Carriers (AREA)
- Hard Magnetic Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
<式>
粉体SFD ≦ 0.0001L2−0.0217L+1.75
<式>
粉体SFD ≦ 0.0001L2−0.0217L+1.75
本発明において重要な点は、ゲータイト粒子粉末を加熱処理してヘマタイト粒子粉末とした後、該ヘマタイト粒子粉末を加熱還元して強磁性金属粒子粉末を得る製造法において、前記ゲータイト粒子粉末の加熱処理を、非還元性雰囲気中100〜250℃の温度範囲で行った後、300〜650℃の温度範囲であって、水蒸気が90vol%以上の条件下で行うことによって得られた強磁性金属粒子粉末は、微細な粒子、殊に、平均長軸径が100nm以下の微粒子でありながら、超微細な粒子の存在割合が低減された、良好な粉体の保磁力分布SFDを有するという事実である。
B.粒子径が10nm未満の粒子は平均粒子径(平均長軸径、平均短軸径)を算出するための粒子として用いない。
<加熱脱水処理>
ゲータイト粒子1(平均長軸径:76.2nm、Co含有量(Co/Fe):39.7原子%、Al含有量(Al/Fe):20.2%、Y含有量(Y/Fe):20.4原子%)を空気中180℃で30分間加熱処理を行った後、水蒸気量が98vol%以上の440℃の過熱蒸気を用いて30分間加熱脱水処理を行い、ヘマタイト粒子を得た。
得られたヘマタイト粒子粉末をバッチ式固定層還元装置に入れ、水素ガスを50cm/sで通気しながら550℃で加熱還元した後、窒素ガスに切り替えて80℃まで冷却し、空気を混合して酸素濃度を0.35vol%まで徐々に増加させて表面酸化処理を行い、粒子表面に表面酸化層を形成した。
<非磁性下地層用組成物>
ヘマタイト粒子粉末 100.0重量部、
(粒子形状:紡錘状、平均長軸径:0.099μm、軸比:6.2、BET比表面積値:59.1m2/g)
スルホン酸カリウム基を有する塩化ビニル系共重合樹脂 11.8重量部、
スルホン酸ナトリウム基を有するポリウレタン樹脂 11.8重量部、
シクロヘキサノン 78.3重量部、
メチルエチルケトン 195.8重量部、
トルエン 117.5重量部、
硬化剤(ポリイソシアネート) 3.0重量部、
潤滑剤(ブチルステアレート) 1.0重量部。
強磁性金属粒子粉末 100.0重量部、
スルホン酸カリウム基を有する塩化ビニル系共重合樹脂 10.0重量部、
スルホン酸ナトリウム基を有するポリウレタン樹脂 10.0重量部、
研磨剤(AKP−50) 10.0重量部、
カーボンブラック 1.0重量部、
潤滑剤(ミリスチン酸:ステアリン酸ブチル=1:2) 3.0重量部、
硬化剤(ポリイソシアネート) 5.0重量部、
シクロヘキサノン 65.8重量部、
メチルエチルケトン 164.5重量部、
トルエン 98.7重量部。
出発原料としてのゲータイト粒子として、表1に示す諸特性を有するゲータイト粒子2〜5を準備した。
原料として用いたゲータイト粒子粉末の種類、加熱処理の温度及び時間、加熱脱水処理の温度、時間及び水蒸気量を種々変化させた以外は実施例1−1と同様にして強磁性金属粒子粉末を得た。
実施例2−2〜2−6及び比較例2−1〜2−5:
強磁性金属粒子粉末の種類を種々変化させた以外は、前記実施例2−1と同様にして磁気記録媒体を製造した。
Claims (3)
- 平均長軸径(L)が10〜100nmであり、全粒子に対して長軸径が10nm未満の超微細な粒子の存在割合が15%以下であり、前記平均長軸径(L)と粉体SFDが下記関係式を満たすことを特徴とする強磁性金属粒子粉末。
<式>
粉体SFD ≦ 0.0001L2−0.0217L+1.75 - ゲータイト粒子粉末を加熱処理してヘマタイト粒子粉末とした後、該ヘマタイト粒子粉末を加熱還元して強磁性金属粒子粉末を得る製造法において、前記ゲータイト粒子粉末の加熱処理を、非還元性雰囲気中100〜250℃の温度範囲で行った後、300〜650℃の温度範囲であって、水蒸気が90vol%以上の条件下で行うことを特徴とする請求項1記載の強磁性金属粒子粉末の製造法。
- 非磁性支持体、該非磁性支持体上に形成される非磁性粒子粉末と結合剤樹脂とを含む非磁性下地層及び該非磁性下地層の上に形成される磁性粒子粉末と結合剤樹脂とを含む磁気記録層からなる磁気記録媒体において、前記磁性粒子粉末として請求項1記載の強磁性金属粒子粉末を用いることを特徴とする磁気記録媒体。
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JP2008266731A JP5556982B2 (ja) | 2008-10-15 | 2008-10-15 | 強磁性金属粒子粉末及びその製造法、並びに磁気記録媒体 |
US12/535,978 US20100035087A1 (en) | 2008-08-08 | 2009-08-05 | Process for producing ferromagnetic metal particles and magnetic recording medium |
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JP2008266731A JP5556982B2 (ja) | 2008-10-15 | 2008-10-15 | 強磁性金属粒子粉末及びその製造法、並びに磁気記録媒体 |
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Publication Number | Publication Date |
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