JP5700191B2 - 強磁性金属粒子粉末の製造法、磁気記録媒体 - Google Patents
強磁性金属粒子粉末の製造法、磁気記録媒体 Download PDFInfo
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- JP5700191B2 JP5700191B2 JP2009198902A JP2009198902A JP5700191B2 JP 5700191 B2 JP5700191 B2 JP 5700191B2 JP 2009198902 A JP2009198902 A JP 2009198902A JP 2009198902 A JP2009198902 A JP 2009198902A JP 5700191 B2 JP5700191 B2 JP 5700191B2
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- particle powder
- ferromagnetic metal
- metal particle
- magnetic recording
- magnetic
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- 239000000843 powder Substances 0.000 title claims description 149
- 239000002923 metal particle Substances 0.000 title claims description 97
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- 238000004519 manufacturing process Methods 0.000 title claims description 30
- 239000002245 particle Substances 0.000 claims description 88
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 claims description 39
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- 238000007254 oxidation reaction Methods 0.000 claims description 36
- 239000012298 atmosphere Substances 0.000 claims description 32
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- 238000010438 heat treatment Methods 0.000 claims description 28
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- 229910052595 hematite Inorganic materials 0.000 claims description 24
- 239000011019 hematite Substances 0.000 claims description 24
- 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 24
- 239000006249 magnetic particle Substances 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 14
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- 239000011230 binding agent Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 38
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002577 polybenzoxazole Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- KVOIJEARBNBHHP-UHFFFAOYSA-N potassium;oxido(oxo)alumane Chemical compound [K+].[O-][Al]=O KVOIJEARBNBHHP-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- POWFTOSLLWLEBN-UHFFFAOYSA-N tetrasodium;silicate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])[O-] POWFTOSLLWLEBN-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Description
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、前記ヘマタイト粒子粉末を加熱還元して金属粒子粉末とした後、気相において酸化処理を行うことにより金属粒子表面に酸化被膜を形成し、更に、該酸化被膜を有する金属粒子粉末を、不活性ガス雰囲気下で200℃以上、300℃未満の温度範囲で加熱処理することにより、平均長軸径が60nm以下である微細な強磁性金属磁性粒子粉末の磁気特性と耐酸化性を同時に向上することができるという事実である。
<ゲータイト核晶粒子の生成反応>
炭酸水素アンモニウム20molとアンモニア水60molを含む混合アルカリ水溶液28Lを反応塔容器の中に入れ、攪拌しながら窒素ガスを流し、非酸化性雰囲気下で50℃に調整した。次いで、1.25mol/Lの硫酸第一鉄水溶液16Lを反応容器に入れて30分熟成した後、1.5mol/Lの硫酸コバルト水溶液4L(全Feに対しCo換算で30原子%に該当する。)を添加し3時間熟成した。
次いで、前記ゲータイト核晶粒子を含有する懸濁液に1.6mol/Lの硫酸アルミニウム水溶液1.25L(全Feに対しAl換算で10原子%に該当する。)を添加し、1L/min.の流量で空気を通気しながら全Fe2+の50%が酸化するまで酸化反応を行った。
得られたゲータイト粒子含有スラリーを濾過後、0.029Nの炭酸ナトリウム水溶液を用いて洗浄し、更に濾液の電気伝導度が100μS以下になるまで水洗した。
上記で得られた水洗後のゲータイト粒子を水中に再分散し、攪拌しながら炭酸ナトリウム水溶液を添加して水溶液のpH値を8.8に調整し、次いで、塩化イットリウム水溶液(全Feに対してY換算で22原子%相当量)を添加して攪拌混合し、炭酸ナトリウム水溶液を添加してスラリーのpH値を9.3に調整した。その後、常法により濾過、水洗、乾燥し、ゲータイト粒子粉末の乾燥固形物を得た(ゲータイト粒子1)。
上記で得られたゲータイト粒子1を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400℃で加熱還元した後、窒素ガスに切り替えて60℃まで冷却し、水蒸気10vol%と酸素濃度0.40vol%になるよう空気を混合し、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。
実施例1−1の条件を種々変更することにより、表1に示す酸化被膜を形成した金属粒子粉末を前駆体として準備した。
不活性ガス雰囲気下における加熱処理条件を種々変更することにより、強磁性金属粒子粉末を得た。このときの製造条件及び得られた強磁性金属粒子粉末の諸特性を表2及び表3に示す。
実施例2−2〜2−4及び比較例2−1〜2−3:
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 (4)
- 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、前記ヘマタイト粒子粉末を加熱還元して金属粒子粉末とした後、気相において酸化処理を行うことにより金属粒子表面に酸化被膜を形成し、更に、該酸化被膜を有する金属粒子粉末を、不活性ガス雰囲気下、200℃以上300℃未満の温度範囲で加熱処理する平均長軸径が60nm以下である強磁性金属粒子粉末の製造法であって、不活性ガス雰囲気下で加熱処理後の保磁力Hcと加熱処理前の保磁力Hcbとの差(Hc−Hcb)が5.7kA/m以上であることを特徴とする強磁性金属粒子粉末の製造法。
- 得られる強磁性金属粒子粉末のBET比表面積値が65m2/g以上である請求項1記載の強磁性金属粒子粉末の製造法。
- 得られる強磁性金属粒子粉末の保磁力Hcが143.2kA/m以上である請求項1又は2に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1〜3のいずれかに記載の強磁性金属粒子粉末の製造法によって得られた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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