JP4707995B2 - 規則配列したナノ構造材料 - Google Patents
規則配列したナノ構造材料 Download PDFInfo
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- JP4707995B2 JP4707995B2 JP2004321602A JP2004321602A JP4707995B2 JP 4707995 B2 JP4707995 B2 JP 4707995B2 JP 2004321602 A JP2004321602 A JP 2004321602A JP 2004321602 A JP2004321602 A JP 2004321602A JP 4707995 B2 JP4707995 B2 JP 4707995B2
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- 239000002086 nanomaterial Substances 0.000 title claims description 33
- 239000002245 particle Substances 0.000 claims description 26
- 239000002105 nanoparticle Substances 0.000 claims description 22
- 239000000758 substrate Substances 0.000 claims description 17
- 239000011148 porous material Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 229910052976 metal sulfide Inorganic materials 0.000 claims description 4
- 239000011146 organic particle Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 description 26
- -1 silane compound Chemical class 0.000 description 26
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- 238000000576 coating method Methods 0.000 description 13
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
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- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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- C03C2217/00—Coatings on glass
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- C03C2217/213—SiO2
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- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
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- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes
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- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T428/00—Stock material or miscellaneous articles
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Description
すなわち、本発明は、基板上に形成された規則配列したドメイン構造の中に、規則配列した直径2〜200nmの空孔が形成されており、かつ該空孔内にナノ粒子が充填されていることを特徴とするナノ構造材料である。
本発明のナノ構造材料におけるドメイン構造は、いかなる製法により製造してもよいが、好ましくは任意に選んだ膜にスタンパを用いて定形の構造を刻印する方法が用いられる。より好ましくは、ゾルゲル膜にスタンパを用いて定形の構造を刻印する方法が用いられる。ゾルゲル膜用の無機・有機ハイブリッドゾルには、(1)分散型、(2)ペンダント型、(3)共重合体型の3つのタイプがあり、いずれを用いても構わないが、高い耐熱性を考慮すると、ペンダント型あるいは共重合体型を用いることが好ましい。
一般式(1)
(R10)m−Si(X)4-m
Yは単結合もしくはエステル基、アミド基、エーテル基、ウレア基を表す。単結合もしくはエステル基、アミド基が好ましく、単結合もしくはエステル基がさらに好ましく、エステル基が特に好ましい。
Lは2価の連結鎖を表す。具体的には、置換もしくは無置換のアルキレン基、置換もしくは無置換のアリーレン基、内部に連結基(例えば、エーテル基、エステル基、アミド基など)を有する置換もしくは無置換のアルキレン基、内部に連結基を有する置換もしくは無置換のアリーレン基が挙げられ、置換もしくは無置換のアルキレン基、置換もしくは無置換のアリーレン基、内部に連結基を有するアルキレン基が好ましく、無置換のアルキレン基、無置換のアリーレン基、エーテル基あるいはエステル基を有するアルキレン基がさらに好ましく、無置換のアルキレン基かエーテルあるいはエステル基を有するアルキレン基が特に好ましい。置換基は、ハロゲン、水酸基、メルカプト基、カルボキシル基、エポキシ基、アルキル基、アリール基等が挙げられ、これら置換基はさらに置換されていても良い。
nは0または1を表す。Xが複数存在するとき、複数のXはそれぞれ同じであっても異なっていても良い。nとして好ましくは0である。
Xは一般式(1)と同義であり、ハロゲン、水酸基、無置換のアルコキシ基が好ましく、塩素、水酸基、無置換の炭素数1〜6のアルコキシ基がさらに好ましく、水酸基、炭素数1〜3のアルコキシ基がさらに好ましく、メトキシ基が特に好ましい。
一般式(1)、一般式(2)の化合物は2種類以上を併用しても良い。以下に一般式(1)、一般式(2)で表される化合物の具体例を示すが、本発明で用いることができる化合物はこれらに限定されるものではない。
加水分解性基がアルコキシドで触媒が有機酸の場合には、有機酸のカルボキシル基やスルホ基がプロトンを供給するために、水の添加量を減らすことができる。シラン化合物のアルコキシド基1モルに対する水の添加量は、通常0〜2モル、好ましくは0〜1.5モル、より好ましくは0〜1モル、特に好ましくは0〜0.5モルである。アルコールを溶媒に用いた場合には、実質的に水を添加しない場合も好適である。
反応は通常25〜100℃で撹拌することにより行われるがシラン化合物の反応性により適宜調節されることが好ましい。
基板の耐熱温度は、300℃以上が好ましく、上記の中から、該当する基板を用いることがさらに好ましい。
本発明における規則配列した空孔の直径は、2〜200nmであり、好ましくは3〜100nm、より好ましくは5〜50nmである。
本発明における規則配列した空孔は、孔径の変動係数が20%以下であることが好ましい。
本発明における規則配列した空孔は、好ましくは、ポリスチレン粒子を自己組織化させて後で除去する方法、ブロックコポリマーのミクロ相分離による球状あるいは柱状の構造を規則的な空孔として利用する方法あるいは疎水性有機溶媒中に疎水ポリマーと両親媒性ポリマーとを溶解した溶液を塗設後、相対湿度50〜95%のガスを一定流速で送風することによってできる規則配列した凝結水滴の蒸発による方法などが用いられる。これらの内、ポリスチレン粒子塗布法よび凝結水滴による方法が好ましく用いられる。
塗布方法は、各種方法を用いることができ、具体的には、スピンコート、ディップコート、エアードクターコート、ブレードコート、ロッドコート、押出しコート、エアナイフコート、スクイズコート、含浸コート、リバースロールコートなどが用いられる。
バインダーは、ポリスチレン粒子の自己組織化構造を形成させた後に塗設しても、また、ポリスチレン粒子分散液にあらかじめ添加しても良い。
本発明に用いるナノ粒子は、目的とするナノ構造体によって任意に選択できるが、好ましくは、金属、金属硫化物、金属酸化物である。
金属の具体例としては、Ag、Au、Pt、Pd、Cu、Ruなどの単独および合金が用いられる。金属硫化物の具体例としては、ZnS、CdS、PdS、In2S3、Au2S、Ag2S、FeSなどが用いられる。金属酸化物の具体例としては、TiO2、SiO2、Ag2O、Cr2O3、ZrO2、SnO2、MnOなどが用いられる。
本発明に用いるナノ粒子として、さらに、平均直径2〜20nmのナノ磁性粒子を用いることが好ましい。ナノ磁性粒子の具体例としては、FePt、CoPt、FePd、Fe2O3、Fe3O4、Sm2Fe17N3、SmCo5、Nd2Fe14Bなどが用いられる。これらのナノ磁性粒子は磁気異方性定数が高く、小サイズでも高い保磁力と熱安定性を示すことで、磁気記録用として有効に用いられる。規則的なナノ構造体を形成させることで、超高密度、高容量の磁気記録媒体として用いることができる。
ナノ磁性粒子の平均直径は、好ましくは2〜20nmであり、より好ましくは3〜10nmである。
分散剤としては、R−NH2、NH2−R−NH2、NH2−R(NH2)−NH2、R−COOH、COOH−R−COOH、COOH−R(COOH)−COOH、R−SO3H、SO3H−R−SO3H、SO3H−R(SO3H)−SO3H、R−SO2H、SO2H−R−SO2H、SO2H−R(SO2H)−SO2Hで表される化合物等を挙げることができる。式中のRは直鎖、分岐または環状の飽和、不飽和の炭化水素である。
(オルガノシランのゾル組成物の調製)
攪拌機、還流冷却器を備えた反応器内において、アクリロイルオキシプロピルトリメトキシシラン(化合物例(18))100gをメチルエチルケトン121gに溶解し、ハイドロキノンモノメチルエーテル0.125g、アルミニウムエチルアセトアセテートジイソプロピレート(30質量%)5.86gおよび水(H2O)23.0gを加え混合したのち、60℃で3時間反応させた後、室温まで冷却してゾル組成物を得た。このゾルは、すべてオリゴマー成分以上(重量平均分子量1000〜2000)であった。
前記のゾル組成物に2−エトキシエタノールを添加して、ゾル濃度を1質量%に調節した後、50rpmで回転している直径65mmで、中心に直径20mmの穴があいたガラス製ディスク基板上に滴下し、4000rpmでスピンコートした。スピンコート後、中心からの距離25mmから60mmの間の円周上に、中心側の弧長が5μmで幅2μmの同心円弧を、幅250nm、深さ20nmの溝で隔離されるように全面に配置した形状に加工した、Niスタンパを刻印したまま150℃で20分加熱した。その後、急冷しながら超音波剥離し、同心円弧が規則配列したドメイン構造を有するゾルゲル膜を形成した。
平均直径21nm(変動係数5%)のポリスチレン粒子の分散液(1質量%)に、対ポリスチレン粒子で35体積%となる量の前記ゾル組成物を添加した塗布液を、前記規則配列したドメイン構造上にスピンコートした。60℃で乾燥した後、トルエンでポリスチレン粒子を溶解し、規則配列したナノ空孔を形成した。さらに、このナノ空孔膜を150℃で20分乾燥して、硬いゲル膜とした。
平均直径5nm(変動係数8%)のFePtナノ粒子にオレイン酸を吸着させて分散したデカン分散液を前記規則配列したナノ空孔上にスピンコートした。200℃で20分乾燥してナノ構造体を形成した。
実施例1で示した内の、規則配列したドメイン構造の形成を無くしたナノ構造体を形成した。
高分解能の走査型電子顕微鏡で観察した結果、ランダムなドメイン構造の中に、部分的に規則配列したナノ粒子の構造体であった。
実施例1で示したものと同じ規則配列したナノ構造体を作製し、Ar+H2(5%)ガス雰囲気中で475℃30分間加熱処理し、冷却後、その上に、前記ゾル組成物を0.05質量%に希釈した液をスピンコートし、150℃20分乾燥した。
平均表面粗さ(Ra)が0.8nmの平滑な強磁性媒体が得られた。
(オルガノシランのゾル組成物の調製)
攪拌機、還流冷却器を備えた反応器、メタクリロイルオキシプロピルトリメトキシシラン(化合物例(19))100g、シュウ酸120g、エタノール450gを加え混合したのち、70℃で5時間反応させた後、室温まで冷却してゾル組成物を得た。このゾルは、すべてオリゴマー成分以上(重量平均分子量1000〜2000)であった。
前記のゾル組成物に2−エトキシエタノールを添加して、ゾル濃度を1質量%に調節した後、50rpmで回転している50mm角のガラス基板上に滴下し、4000rpmでスピンコートした。スピンコート後、一辺が5μmの正方形が幅500nm、深さ30nmの溝で隔離されるように全面に配置した形状に加工した、Niスタンパを刻印したまま150℃で20分加熱した。その後、急冷しながら超音波剥離し、正方形が規則配列したドメイン構造を有するゾルゲル膜を形成した。
平均直径30nm(変動係数5%)のポリスチレン粒子の分散液(1質量%)に、対ポリスチレン粒子で35体積%となる量の前記ゾル組成物を添加した塗布液を、前記規則配列したドメイン構造上にスピンコートした。60℃で乾燥した後、トルエンでポリスチレン粒子を溶解し、規則配列したナノ空孔を形成した。さらに、このナノ空孔膜を150℃で20分乾燥して、硬いゲル膜とした。
平均直径10nm(変動係数10%)のAuナノ粒子にドデカンチオールを吸着させて分散したデカン分散液を前記規則配列したナノ空孔内にスピンコートした。200℃で20分乾燥してナノ構造体を形成した。
Claims (7)
- 基板上に形成されたゾルゲル膜からなる規則配列したドメイン構造の中に、規則配列した直径2〜200nmの空孔が形成されており、かつ該空孔内にナノ粒子が充填されていることを特徴とするナノ構造材料。
- 規則配列したドメイン構造が同心円弧、台形、長方形または正方形であり、その1辺が0.1〜100μmであることを特徴とする請求項1に記載のナノ構造材料。
- 基板の耐熱温度が300℃以上であることを特徴とする請求項1または2に記載のナノ構造材料。
- 規則配列した空孔内に充填されたナノ粒子が金属、金属硫化物、金属酸化物または有機物粒子であることを特徴とする請求項1〜3のいずれかに記載のナノ構造材料。
- 規則配列した空孔内に充填されたナノ粒子が平均直径2〜20nmのナノ磁性粒子であることを特徴とする請求項4に記載のナノ構造材料。
- 規則配列したドメイン構造の周囲が、幅10nm〜10μmで高さ2〜100nmの枠で囲まれていることを特徴とする請求項1〜5のいずれかに記載のナノ構造材料。
- 規則配列した空孔の孔径の変動係数が20%以下であることを特徴とする請求項1〜6のいずれかに記載のナノ構造材料。
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EP20050805944 EP1817779B1 (en) | 2004-11-05 | 2005-11-04 | Regularly arrayed nanostructured material |
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US8821736B1 (en) * | 2013-02-20 | 2014-09-02 | HGST Netherlands B.V. | Method for making a perpendicular magnetic recording disk with template layer formed of nanoparticles embedded in a polymer material |
US9236076B2 (en) * | 2013-02-20 | 2016-01-12 | HGST Netherlands B.V. | Perpendicular magnetic recording disk with template layer formed of nanoparticles embedded in a polymer material |
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JP2003318010A (ja) * | 2002-04-22 | 2003-11-07 | Fuji Photo Film Co Ltd | ハニカム構造体の空孔に磁性材料微粒子を含有する材料 |
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