JP5403222B2 - 磁気記録用金属磁性粒子粉末の製造方法、並びに磁気記録媒体 - Google Patents
磁気記録用金属磁性粒子粉末の製造方法、並びに磁気記録媒体 Download PDFInfo
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- JP5403222B2 JP5403222B2 JP2009026570A JP2009026570A JP5403222B2 JP 5403222 B2 JP5403222 B2 JP 5403222B2 JP 2009026570 A JP2009026570 A JP 2009026570A JP 2009026570 A JP2009026570 A JP 2009026570A JP 5403222 B2 JP5403222 B2 JP 5403222B2
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- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
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- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
- G11B5/70626—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances
- G11B5/70642—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
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- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
- H01F1/112—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles with a skin
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
- H01F1/113—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles in a bonding agent
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Description
その後、酸化反応の反応率(Fe2+/全Fe)が20%以降にAl化合物を添加し、引き続き酸化反応をする成長反応を行ってゲータイト粒子粉末が得られる。
本発明において重要な点は、平均長軸径が5〜100nmの微粒子でありながら、粒子間の凝集が抑制され、該金属磁性粒子粉末を用いた磁気テープ(磁性塗膜)が磁気特性(保磁力Hc)に優れるという事実である。
電子顕微鏡による試料の観察にあたっては、下記方法によって試料を調製した。
即ち、金属磁性粒子粉末を0.04重量部、分散剤を0.12重量部、分散媒(分散溶剤)99.84重量部を超音波分散機にて3分間分散した後、湿式ジェットミルにて10パス分散させた分散体を透過型電子顕微鏡観察用の試料として用いた。
試料支持膜であるメッシュ上に前記分散溶液をのせ、自然乾燥後、試料を観察する。予備分散をしているため、試料支持膜上で均一に分散し、ほぐれた粒子が観察できる。
STEM値(m2/g)=〔(4lw+2w2)/(lw2・ρp)〕×10−4
(但し、ρpは金属磁性粒子粉末の真比重であり、マルチボリウム密度計(島津製作所株式会社)を用いて得られた値の5.5g/cm3を用いた。)
但し、β=装置に起因する機械幅を補正した真の回折ピークの半値幅(ラジアン単位)。
K=シェラー定数(=0.9)、
λ=X線の波長(Cu Kα線 0.1542nm)、
θ=回折角((110)面の回折ピークに対応)。
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重量部、
研磨剤(AKP−50) 10重量部、
潤滑剤(ミリスチン酸:ステアリン酸ブチル=1:2) 3重量部、
硬化剤(ポリイソシアネート) 5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。
炭酸アンモニウムを20molとアンモニア水を60mol(混合アルカリに対し水酸化アンモニア水溶液は規定換算で75mol%に該当する。)を含む混合アルカリ水溶液28lを、気泡分散翼を備えた攪拌機付き反応塔の中に投入し、毎分700回転の速度で攪拌機を回転させながら、毎分60lの流量で窒素ガス雰囲気にしながら50℃に調整する。次いで、Fe2+として20molを含む硫酸第一鉄水溶液16l(硫酸第一鉄に対し混合アルカリ水溶液は規定換算で3.75当量に該当する。)を気泡塔中に投入して30分熟成した後、Co2+として6.0molを含む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2.5時間熟成した。
ここに得た紡錘状ヘマタイト粒子粉末の顆粒状造粒物100g(平均径:2.6mm)を内径72mmのバッチ式固定層還元装置に入れ、層高を7cmとした後、水素ガス空塔速度50cm/sで通気しながら、350℃で排気ガス露点が−30℃に達するまで加熱還元して金属磁性粒子粉末を得た。
ゲータイト粒子の生成において、酸化剤の種類及び添加量、中和温度、Al化合物の添加時期、添加量及び酸化速度を種々変更した以外は、実施例1と同様にしてゲータイト粒子粉末を得た。このときの製造条件及び得られたゲータイト粒子粉末の諸特性を表1に示す。
Claims (2)
- アルミニウム含有量が全Feに対してAl換算で4〜50原子%のゲータイト粒子粉末に加熱処理を行ってヘマタイト粒子粉末を得、該ヘマタイト粒子粉末を200〜600℃で加熱還元する金属磁性粒子粉末の製造方法において、前記ゲータイト粒子粉末として、第一鉄塩水溶液と、炭酸水素アルカリ水溶液又は炭酸アルカリ水溶液と水酸化アルカリ水溶液との混合アルカリ水溶液とからなる反応溶液に、酸化反応前に全Feに対して0.5〜5mol%の過硫酸塩を添加した後、酸化反応を行って得られたゲータイト粒子粉末を用いることを特徴とする磁気記録用金属磁性粒子粉末の製造方法。
- 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記載の磁気記録用金属磁性粒子粉末の製造方法によって得られた金属磁性粒子粉末を用い、該金属磁性粒子粉末はBET法により測定した比表面積S BET 値と電子顕微鏡写真に示されている粒子から計測された長軸径及び短軸径から算出した表面積S TEM 値との比(S BET /S TEM 値)が0.5〜2.0であることを特徴とする磁気記録媒体。
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JP2009026570A JP5403222B2 (ja) | 2008-02-06 | 2009-02-06 | 磁気記録用金属磁性粒子粉末の製造方法、並びに磁気記録媒体 |
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JP2009026570A JP5403222B2 (ja) | 2008-02-06 | 2009-02-06 | 磁気記録用金属磁性粒子粉末の製造方法、並びに磁気記録媒体 |
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JP5403222B2 true JP5403222B2 (ja) | 2014-01-29 |
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CN105834449B (zh) * | 2016-05-04 | 2017-09-22 | 苏州思美特表面材料科技有限公司 | 一种利用微纳米气泡作为晶种诱导生产银粉的制备方法 |
JP6823323B2 (ja) * | 2019-02-01 | 2021-02-03 | 大陽日酸株式会社 | 強磁性粉末、組成物、成形品、強磁性粉末の製造方法 |
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DE2556406A1 (de) * | 1975-12-15 | 1977-06-16 | Bayer Ag | Verfahren zur kontinuierlichen herstellung von eisenoxidhydroxid |
US4414021A (en) * | 1982-05-06 | 1983-11-08 | Welbon William W | Process for the synthesis of iron powder |
US5552073A (en) * | 1988-09-26 | 1996-09-03 | Seisan Kaihatsu Kagaku Kenkyusho | Ferromagnetic fine particles of ε iron carbide and method for producing the same |
DE10010940A1 (de) * | 2000-03-06 | 2001-09-13 | Bayer Ag | Verfahren zur Herstellung von Eisenoxid und seine Verwendung |
JP2002327202A (ja) * | 2001-04-27 | 2002-11-15 | Toda Kogyo Corp | 鉄を主成分とする複合金属磁性粒子粉末及びその製造法並びに磁気記録媒体 |
US7172642B2 (en) * | 2001-12-04 | 2007-02-06 | Toda Kogyo Corporation | Magnetic metal particles containing iron as main component, process for producing the same and magnetic recording medium using the same |
JP4534085B2 (ja) * | 2004-03-24 | 2010-09-01 | Dowaエレクトロニクス株式会社 | 高密度化に対応した塗布型磁気記録媒体用磁性粉末およびその製造方法 |
JP4431769B2 (ja) * | 2005-09-15 | 2010-03-17 | Dowaエレクトロニクス株式会社 | 強磁性粉末ならびにそれを用いた塗料および磁気記録媒体 |
JP5418754B2 (ja) * | 2008-10-15 | 2014-02-19 | 戸田工業株式会社 | 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 |
JP5447767B2 (ja) * | 2008-08-08 | 2014-03-19 | 戸田工業株式会社 | 強磁性金属粒子粉末の製造法 |
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2009
- 2009-02-03 US US12/364,658 patent/US20090202867A1/en not_active Abandoned
- 2009-02-06 JP JP2009026570A patent/JP5403222B2/ja active Active
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JP2009211799A (ja) | 2009-09-17 |
US20120042750A1 (en) | 2012-02-23 |
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