JP4719431B2 - 六方晶フェライト磁性粉末、その製造方法および磁気記録媒体 - Google Patents
六方晶フェライト磁性粉末、その製造方法および磁気記録媒体 Download PDFInfo
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- JP4719431B2 JP4719431B2 JP2004182593A JP2004182593A JP4719431B2 JP 4719431 B2 JP4719431 B2 JP 4719431B2 JP 2004182593 A JP2004182593 A JP 2004182593A JP 2004182593 A JP2004182593 A JP 2004182593A JP 4719431 B2 JP4719431 B2 JP 4719431B2
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- hexagonal ferrite
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Description
このような目的を達成するため、例えば、非磁性支持体上に、六方晶フェライト磁性粉末を結合剤中に分散してなる磁性層を設けた磁気記録媒体が提案されている(例えば下記特許文献1参照)。
また、六方晶フェライト磁性粉末の改良としては、下記特許文献2〜5に開示されている。
しかしながら、前記の従来技術では、〜1Gbpsiという現在要求されている高密度記録用の磁気記録媒体を得ることはできなかった。
(1)平均板径が15〜30nm、平均板状比が3.0〜4.9、Hcが2020〜5000Oe(161.6〜400kA/m)、SFDが0.3〜0.7であり、かつ、4価元素(M4)であるZrをFe1原子に対して0.004〜0.045原子含み、CoおよびZnから選択された少なくとも1種の2価元素(M2)をFe1原子に対して0.004〜0.045原子含むことを特徴とする六方晶フェライト磁性粉末。
(2)六方晶フェライト生成原料と、前記六方晶フェライト生成原料に含まれるFe1原子に対して0.004〜0.045原子の4価元素(M4)であるZrを混合し、得られた原料混合物を溶融し、急冷して非晶質体を得る工程と、次いで前記非晶質体を熱処理して六方晶フェライトを析出させる工程とを有することを特徴とする(1)に記載の六方晶フェライト磁性粉末を製造する方法。
(3)非磁性支持体上に六方晶フェライト磁性粉末を結合剤中に分散してなる磁性層を設けた磁気記録媒体において、前記六方晶フェライト磁性粉末が(1)に記載の六方晶フェライト磁性粉末であることを特徴とする磁気記録媒体。
(4)前記非磁性支持体と磁性層との間に非磁性粉体を結合剤中に分散した非磁性層を設けたことを特徴とする(3)に記載の磁気記録媒体。
本発明の六方晶フェライト磁性粉末は、平均板径15〜30nm、好ましくは18〜28nmであり、平均板状比が3.0〜4.9、好ましくは3.0〜4.2であり、保磁力HCが2020〜5000Oe(161.6〜400kA/m)、好ましくは2100〜4200Oe(168〜336kA/m)であり、かつ磁化反転分布SFDが0.3〜0.7、好ましくは0.3〜0.6である。平均板径が15nm未満では十分な磁気特性が得られず、30nmを超えるとノイズが大きくなり、高密度記録用の磁気記録媒体に必要なSN比が確保できない。平均板状比が3.0未満であると磁気特性のバランスが得られず、4.9を超えると磁性層中で磁性粉末充填率が低くなるとともにスタッキングによるノイズ低下が見られる。Hcが2020Oe未満では短波長記録の自己減磁によると思われる出力低下が大きい。また平均板径15〜30nmの範囲において、5000Oeを超えるHcを有する磁性粉末の製造は困難である。またSFDが0.7を超えると出力低下が大きい。なおSFD0.3未満を有する磁性粉末の製造は困難である。
これらの4価元素(M4)を添加することにより、ノイズの増加を抑制しながら、平均板状比を増加させ、SFDの低減が可能となる。4価元素(M4)の添加量が0.004原子未満では、平均板状比増加が起こらず、SFDが低減しない。逆に0.045原子を超えると、平均板状比が増加しすぎて分散しずらい粉末となり、媒体特性を悪化させる。
好ましい2価元素(M2)は、Mg、Co、Ni、Cu、Zn、PdおよびCdからなる群から選択された少なくとも1種であり、とくにCo、Znが好ましい。なお、2価元素(M2)としてCoを選択した場合は、保磁力低減効果が大きいため、その添加量は、Fe1原子に対して0.004〜0.030原子が好ましい。
すなわち、六方晶フェライト生成原料と、前記の4価元素(M4)と、必要に応じて2価元素(M2)とを混合し、得られた原料混合物を溶融し、急冷して非晶質体を得、次いで前記非晶質体を熱処理して六方晶フェライトを析出させることにより、本発明の六方晶フェライト磁性粉末が得られる。
(a)B2O3=50,AO=40,Fe2O3=10モル%
(b)B2O3=45,AO=45,Fe2O3=10モル%
(c)B2O3=25,AO=25,Fe2O3=50モル%
(d)B2O3=30,AO=20,Fe2O3=50モル%
本発明に用いられる支持体では可撓性支持体が好ましく、例えば、ポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)等のポリエステル類、ポリオレフイン類、セルローストリアセテート、ポリカーボネート、ポリアミド、ポリイミド、ポリアミドイミド、ポリスルフオン、アラミドなどの芳香族ポリアミドなどの公知のフィルムが使用できる。これらの支持体にはあらかじめコロナ放電処理、プラズマ処理、易接着処理、熱処理、除塵処理、などをおこなってもよい。本発明の目的を達成するには、支持体として中心線平均表面粗さが通常、0.03μm以下、好ましくは0.02μm以下、さらに好ましくは0.01μm以下のものを使用することが好ましい。また、これらの支持体は単に中心線平均表面粗さが小さいだけではなく、1μm以上の粗大突起がないことが好ましい。さらに表面の粗さ形状は、必要に応じて支持体に添加されるフィラーの大きさと量により自由にコントロールされるものである。これらのフィラーとしては一例としてはCa、Si、Tiなどの酸化物や炭酸塩の他、アクリル系などの有機微粉末が挙げられる。
本発明の磁性層に用いられる結合剤は、従来公知の熱可塑性樹脂、熱硬化性樹脂、反応型樹脂やこれらの混合物である。熱可塑性樹脂としては、例えば、塩化ビニル、酢酸ビニル、ビニルアルコール、マレイン酸、アクリル酸、アクリル酸エステル、塩化ビニリデン、アクリロニトリル、メタクリル酸、メタクリル酸エステル、スチレン、ブタジエン、エチレン、ビニルブチラール、ビニルアセタール、ビニルエーテル等を構成単位として含む重合体又は共重合体、ポリウレタン樹脂、各種ゴム系樹脂を挙げることができる。
次に非磁性層に関する詳細な内容について説明する。本発明の磁気記録媒体は、支持体上に結合剤及び非磁性粉末を含む非磁性層を有することができる。非磁性層に使用できる非磁性粉末は、無機物質でも有機物質でもよい。また、カーボンブラック等も使用できる。無機物質としては、例えば金属、金属酸化物、金属炭酸塩、金属硫酸塩、金属窒化物、金属炭化物、金属硫化物などが挙げられる。
本発明で用いられる磁気記録媒体の厚み構成は、支持体の好ましい厚みが3〜80μmである。また、支持体と非磁性層又は磁性層の間に下塗り層を設けた場合、下塗り層の厚みは、0.01〜0.8μm、好ましくは0.02〜0.6μmである。
本発明で用いられる磁気記録媒体の磁性層塗布液を製造する工程は、少なくとも混練工程、分散工程、及びこれらの工程の前後に必要に応じて設けた混合工程からなる。個々の工程はそれぞれ2段階以上に分かれていてもかまわない。本発明で用いられる六方晶フェライト磁性粉末、非磁性粉末、結合剤、カーボンブラック、研磨材、帯電防止剤、潤滑剤、溶剤などすべての原料はどの工程の最初又は途中で添加してもかまわない。また、個々の原料を2つ以上の工程で分割して添加してもかまわない。例えば、ポリウレタンを混練工程、分散工程、分散後の粘度調整のための混合工程で分割して投入してもよい。本発明の目的を達成するためには、従来の公知の製造技術を一部の工程として用いることができる。混練工程ではオープンニーダ、連続ニーダ、加圧ニーダ、エクストルーダなど強い混練力をもつものを使用することが好ましい。これらの混練処理の詳細については特開平1−106338号公報、特開平1−79274号公報に記載されている。また、磁性層用液及び非磁性層用液を分散させるには、ガラスビーズを用いることができる。このようなガラスビーズは、高比重の分散メディアであるジルコニアビーズ、チタニアビーズ、スチールビーズが好適である。これら分散メディアの粒径と充填率は最適化して用いられる。分散機は公知のものを使用することができる。
本発明の磁気記録媒体が磁気ディスクの場合、Hc(面内)は、好ましくは160〜350kA/m(更に好ましくは180〜340kA/m、特に好ましくは200〜320kA/m)であり、SQ(角型比)は、好ましくは0.40〜0.60(更に好ましくは0.45〜0.60、特に好ましくは0.50〜0.60)であり、Bm(最大磁束密度)は、好ましくは1000〜2000mT(更に好ましくは1200〜2000mT、特に好ましくは1500〜2000mT)である。
本発明で用いられる磁気記録媒体のヘッドに対する摩擦係数は、温度−10〜40℃、湿度0〜95%の範囲において0.5以下であり、好ましくは0.3以下である。また、表面固有抵抗は、好ましくは磁性面104〜1012Ω/sq、帯電位は−500V〜+500V以内が好ましい。磁性層の0.5%伸びでの弾性率は、面内各方向で好ましくは0.98〜19.6GPa(100〜2000kg/mm2)、破断強度は、好ましくは98〜686MPa(10〜70kg/mm2)、磁気記録媒体の弾性率は、面内各方向で好ましくは0.98〜14.7GPa(100〜1500kg/mm2)、残留のびは、好ましくは0.5%以下、100℃以下のあらゆる温度での熱収縮率は、好ましくは1%以下、さらに好ましくは0.5%以下、最も好ましくは0.1%以下である。
<六方晶フェライト磁性粉末の作成>
BaOを31モル%、B2O3を31モル%、組成式BaO・Fe12-(3(x+y)+Z)/2Cox Zny MzNb(x+y-z)/2 O18(式中、Mは4価元素を表す)で表されるBaフェライト成分38モル%を得るために、各元素に対応する原料を秤量し十分に混合した。白金ルツボに混合原料を投入し高周波加熱装置を用いて1350℃で加熱溶融した。全ての原料を溶融したのち、均質化するため1時間攪拌し、均質化した熔融物を高速回転させた水冷双ローラー上に注いで圧延急冷し、非晶質体を作製した。得られた非晶質体を熱処理炉で、所定の結晶化温度で5時間保持してBaフェライト結晶を析出させた。その後、析出物を粉砕したのち、10%の酢酸溶液中で、溶液温度を80℃以上に制御しながら、4時間攪拌し酸処理を行い、BaOおよびB2O3を溶解した。続いて、これらのBaOおよびB2O3成分および酸成分を除去するため、水洗を十分に繰り返した。最後に、スラリーを乾燥させ、磁性粉末を得た。得られた磁性粉末の特性を表1に組成成分と共に示す。なお平均板径及び平均板厚は、透過型電子顕微鏡で40万倍の粒子写真を測定し、粒子側面が見える粒子300ヶの板径および板厚を測定し平均値を求めた。また、平均板状比は、(板径/板厚)の算術平均とした。磁気特性(Hc、SFD)は、振動試料型磁束計(東栄工業社製)を用い、23℃で印加磁界10KOeで測定した。
磁性層形成用塗料
バリウムフェライト磁性粉末 100部
ポリウレタン樹脂 12部
質量平均分子量 10000
スルホン酸官能基 0.5meq/g
α−アルミナ
HIT60(住友化学社製) 8部
カ−ボンブラック(粒子サイズ0.015μm)
#55(旭カーボン社製) 0.5部
ステアリン酸 0.5部
ブチルステアレート 2部
メチルエチルケトン 180部
シクロヘキサノン 100部
非磁性粉体 α酸化鉄 100部
平均長軸長0.09μm、BET法による比表面積 50m2/g
pH 7
DBP吸油量27〜38ml/100g、
表面処理層Al2O3 8質量%
カ−ボンブラック 25部
コンダクテックスSC−U(コロンビアンカーボン社製)
塩化ビニル共重合体
MR104(日本ゼオン社製) 13部
ポリウレタン樹脂
UR8200(東洋紡社製) 5部
フェニルホスホン酸 3.5部
ブチルステアレート 1部
ステアリン酸 2部
メチルエチルケトン 205部
シクロヘキサノン 135部
上記の塗料のそれぞれについて、各成分をニ−ダで混練した。1.0mmφのジルコニアビーズを分散部の容積に対し65%充填する量を入れた横型サンドミルに、塗布液をポンプで通液し、2000rpmで120分間(実質的に分散部に滞留した時間)、分散させた。得られた分散液にポリイソシアネ−トを非磁性層の塗料には5.0部、磁性層の塗料には2.5部を加え、さらにメチルエチルケトン3部を加え、1μmの平均孔径を有するフィルターを用いて濾過し、非磁性層形成用および磁性層形成用の塗布液をそれぞれ調整した。
得られた非磁性層形成用塗布液を、4μmポリエチレンテレフタレートベース上に乾燥後の厚さが1.5μmになるように塗布乾燥させた後、磁性層形成用塗布液を磁性層の厚さが0.10μmになるように逐次重層塗布をおこない、磁性層がまだ湿潤状態にあるうちに6000G(600mT)の磁力を持つコバルト磁石と6000Gの磁力を持つソレノイドにより配向させ乾燥させた。次いで7段のカレンダで温度90℃、線圧300kg/cm(294kN/m)にて処理を行った。その後、厚み0.5μmのバック層(カ−ボンブラック 平均粒子サイズ:17nm 100部、炭酸カルシウム 平均粒子サイズ:40nm 80部、αアルミナ 平均粒子サイズ:200nm 5部をニトロセルロ−ス樹脂、ポリウレタン樹脂、ポリイソシアネ−トに分散)を塗布した。3.8mmの幅にスリットし、スリット品の送り出し、巻き取り装置を持った装置に不織布とカミソリブレ−ドが磁性面に押し当たるように取り付け、テ−プクリ−ニング装置で磁性層の表面のクリ−ニングを行い、磁気テープ媒体を得た。
結果を表2に示す。なお表2において実施例および比較例番号は、表1に示した磁性粉末の実施例および比較例番号に対応している。
表1および2の結果から、本発明の磁性粉末は、比較例に比べて、板径が小さくてもSFDの増加が抑制されていることが分かる。また、良好な出力特性および低ノイズ性も示していることが分かる。
<ディスク用塗料の作成>
磁性層形成用塗料
バリウムフェライト磁性粉末 100部
ポリウレタン樹脂 12部
質量平均分子量 10000
スルホン酸官能基 0.5meq/g
ダイアモンド微粒子
平均粒径0.10μm 2部
カ−ボンブラック(粒子サイズ0.015μm)
#55(旭カーボン社製) 0.5部
ステアリン酸 0.5部
ブチルステアレート 2部
メチルエチルケトン 230部
シクロヘキサノン 150部
非磁性粉体 α酸化鉄 100部
平均長軸長0.09μm、BET法による比表面積 50m2/g
pH 7
DBP吸油量27〜38ml/100g、
表面処理層Al2O3 8質量%
カ−ボンブラック 25部
コンダクテックスSC−U(コロンビアンカーボン社製)
塩化ビニル共重合体
MR104(日本ゼオン社製) 13部
ポリウレタン樹脂
UR8200(東洋紡社製) 5部
フェニルホスホン酸 3.5部
ブチルステアレート 1部
ステアリン酸 2部
メチルエチルケトン 205部
シクロヘキサノン 135部
上記の塗料のそれぞれについて、各成分をニ−ダで混練した。1.0mmφのジルコニアビーズを分散部の容積に対し65%充填する量を入れた横型サンドミルに、塗布液をポンプで通液し、2000rpmで120分間(実質的に分散部に滞留した時間)、分散させた。得られた分散液にポリイソシアネ−トを非磁性層の塗料には6.5部、磁性層の塗料には2.5部を加え、さらにメチルエチルケトン7部を加え、1μmの平均孔径を有するフィルターを用いて濾過し、非磁性層形成用および磁性層形成用の塗布液をそれぞれ調整した。
得られた非磁性層形成用塗布液を、62μmポリエチレンテレフタレートベース上に乾燥後の厚さが1.5μmになるように塗布乾燥させた後、磁性層形成用塗布液を磁性層の厚さが0.10μmになるように逐次重層塗布をおこない、乾燥後、7段のカレンダで温度90℃、線圧300kg/cmにて処理を行った。これらの操作を非磁性支持体の両面に施した。3.5吋に打ち抜き、表面研磨処理を施して磁気ディスク媒体を得た。
結果を表3に示す。なお表3において実施例および比較例番号は、表1に示した磁性粉末の実施例および比較例番号に対応している。
表3の結果から、本発明の磁性粉末は、比較例に比べて、板径が小さくてもSFDの増加が抑制されていることが分かる。また、良好な出力特性および低ノイズ性も示していることが分かる。
Claims (4)
- 平均板径が15〜30nm、平均板状比が3.0〜4.9、Hcが2020〜5000Oe(161.6〜400kA/m)、SFDが0.3〜0.7であり、かつ、4価元素(M4)であるZrをFe1原子に対して0.004〜0.045原子含み、CoおよびZnから選択された少なくとも1種の2価元素(M2)をFe1原子に対して0.004〜0.045原子含むことを特徴とする六方晶フェライト磁性粉末。
- 六方晶フェライト生成原料と、前記六方晶フェライト生成原料に含まれるFe1原子に対して0.004〜0.045原子の4価元素(M4)であるZrを混合し、得られた原料混合物を溶融し、急冷して非晶質体を得る工程と、次いで前記非晶質体を熱処理して六方晶フェライトを析出させる工程とを有することを特徴とする請求項1に記載の六方晶フェライト磁性粉末を製造する方法。
- 非磁性支持体上に六方晶フェライト磁性粉末を結合剤中に分散してなる磁性層を設けた磁気記録媒体において、前記六方晶フェライト磁性粉末が請求項1に記載の六方晶フェライト磁性粉末であることを特徴とする磁気記録媒体。
- 前記非磁性支持体と磁性層との間に非磁性粉体を結合剤中に分散した非磁性層を設けたことを特徴とする請求項3に記載の磁気記録媒体。
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US11/156,654 US20050282043A1 (en) | 2004-06-21 | 2005-06-21 | Hexagonal ferrite magnetic powder, process for producing the same, and magnetic recording medium |
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JP5185200B2 (ja) * | 2009-06-02 | 2013-04-17 | 富士フイルム株式会社 | 六方晶フェライト磁性粉末およびその製造方法、ならびに磁気記録媒体およびその製造方法 |
JP5697399B2 (ja) * | 2010-03-31 | 2015-04-08 | 富士フイルム株式会社 | 六方晶フェライト磁性粒子およびその製造方法、磁気記録媒体用磁性粉、ならびに磁気記録媒体 |
EP2640527A4 (en) * | 2010-11-15 | 2016-03-09 | Trustees Of The University Of Alabama For And On Behalf Of The University Of Alabama Board Of | M-TYPE HEXAFERRITE ANTENNAS FOR USE IN WIRELESS COMMUNICATION DEVICES |
JP5712595B2 (ja) * | 2010-12-15 | 2015-05-07 | 戸田工業株式会社 | 磁気記録媒体用六方晶フェライト粒子粉末及び磁気記録媒体 |
JP5712594B2 (ja) * | 2010-12-15 | 2015-05-07 | 戸田工業株式会社 | 磁気記録媒体用六方晶フェライト粒子粉末 |
JP5231590B2 (ja) * | 2011-03-28 | 2013-07-10 | 富士フイルム株式会社 | 磁気記録用磁性粉およびその製造方法、ならびに磁気記録媒体 |
CN103304228A (zh) * | 2012-03-16 | 2013-09-18 | 西北师范大学 | 自蔓延燃烧合成钯铜铁氧体纳米粉体的方法 |
JP7273953B2 (ja) * | 2019-05-14 | 2023-05-15 | 富士フイルム株式会社 | 電波吸収体 |
CN114477301B (zh) * | 2022-02-25 | 2023-09-29 | 武汉苏泊尔炊具有限公司 | 不粘材料及其制备方法和应用 |
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JPH03248505A (ja) * | 1990-02-27 | 1991-11-06 | Toshiba Corp | 磁気記録用磁性粉の製造方法 |
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