JP5472446B2 - ナノヘテロ構造体およびその製造方法 - Google Patents
ナノヘテロ構造体およびその製造方法 Download PDFInfo
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- JP5472446B2 JP5472446B2 JP2012505720A JP2012505720A JP5472446B2 JP 5472446 B2 JP5472446 B2 JP 5472446B2 JP 2012505720 A JP2012505720 A JP 2012505720A JP 2012505720 A JP2012505720 A JP 2012505720A JP 5472446 B2 JP5472446 B2 JP 5472446B2
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- 150000001255 actinides Chemical class 0.000 description 1
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- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
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- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 description 1
- ILZSSCVGGYJLOG-UHFFFAOYSA-N cobaltocene Chemical compound [Co+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 ILZSSCVGGYJLOG-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 229910052732 germanium Inorganic materials 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- NBTOZLQBSIZIKS-UHFFFAOYSA-N methoxide Chemical compound [O-]C NBTOZLQBSIZIKS-UHFFFAOYSA-N 0.000 description 1
- 150000004704 methoxides Chemical class 0.000 description 1
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 1
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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- HZEBHPIOVYHPMT-UHFFFAOYSA-N polonium atom Chemical compound [Po] HZEBHPIOVYHPMT-UHFFFAOYSA-N 0.000 description 1
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- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical class CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- IKNCGYCHMGNBCP-UHFFFAOYSA-N propan-1-olate Chemical compound CCC[O-] IKNCGYCHMGNBCP-UHFFFAOYSA-N 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- QPBYLOWPSRZOFX-UHFFFAOYSA-J tin(iv) iodide Chemical compound I[Sn](I)(I)I QPBYLOWPSRZOFX-UHFFFAOYSA-J 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000003325 tomography Methods 0.000 description 1
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- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- Hard Magnetic Materials (AREA)
Description
互いに混和しない少なくとも第一ポリマーブロック成分と第二ポリマーブロック成分とが結合してなるブロックコポリマーと、前記第一ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2以下である第一無機前駆体と、前記第二ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2以下である第二無機前駆体と、を溶媒に溶解して原料溶液を調製する第一の工程と、
少なくとも、前記第一無機前駆体が導入された前記第一ポリマーブロック成分からなる第一ポリマー相と、前記第二無機前駆体が導入された前記第二ポリマーブロック成分からなる第二ポリマー相と、が自己組織化により規則的に配置したナノ相分離構造体を形成せしめる相分離処理と、前記第一無機前駆体および前記第二無機前駆体をそれぞれ第一無機成分および第二無機成分に変換せしめる変換処理と、前記ナノ相分離構造体から前記ブロックコポリマーを除去する除去処理とを含み、前記第一無機成分と前記第二無機成分とからなるナノヘテロ構造体を得る第二の工程と、
を含む方法である。
溶解度パラメータδ[(cal/cm3)1/2]=(ΔE/V)1/2
(式中、ΔEはモル蒸発エネルギー[cal]、Vはモル体積[cm3]を示す。)
に基づいて求められる値である。
互いに混和しない少なくとも第一ポリマーブロック成分と第二ポリマーブロック成分とが結合してなるブロックコポリマーと、前記第一ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2以下である第一無機前駆体と、前記第二ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2以下である第二無機前駆体と、を溶媒に溶解して原料溶液を調製する第一の工程と、
少なくとも、前記第一無機前駆体が導入された前記第一ポリマーブロック成分からなる第一ポリマー相と、前記第二無機前駆体が導入された前記第二ポリマーブロック成分からなる第二ポリマー相と、が自己組織化により規則的に配置したナノ相分離構造体を形成せしめる相分離処理と、前記第一無機前駆体および前記第二無機前駆体をそれぞれ第一無機成分および第二無機成分に変換せしめる変換処理と、前記ナノ相分離構造体から前記ブロックコポリマーを除去する除去処理とを含み、前記第一無機成分と前記第二無機成分とからなるナノヘテロ構造体を得る第二の工程と、
を含む方法である。以下に、それぞれの工程を説明する。
係る工程は、以下に説明するブロックコポリマーと以下に説明する無機前駆体とを溶媒に溶解して原料溶液を調製する工程である。
この工程は、以下に詳述する相分離処理と変換処理と除去処理とを含み、第一無機成分と第二無機成分とからなるナノヘテロ構造体を調製する工程である。
ブロックコポリマーとしてのポリスチレン−b−ポリ(4−ビニルピリジン)(PS−b−P4VP)0.1g、Ti前駆体としての塩化チタン0.038g、Sn前駆体としてのヨウ化スズ0.032gを10mLのトルエンに溶解し、原料溶液を得た。なお、PS−b−P4VPのPSの分子量は22×103、P4VPの分子量は22×103であった。また、Ti前駆体およびSn前駆体と各構成要素との間の溶解度パラメータの差は以下の表2に示す通りであった。
実施例1と同様にして得られた原料溶液を熱処理後の厚みが約500μmとなるように熱処理容器に入れ、窒素雰囲気中で850℃で6時間熱処理し、さらに空気中で600℃で1時間熱処理することによって無機構造体を得た。
ブロックコポリマーとしてのポリメタクリル酸メチル−b−ポリアクリロニトリル(PMMA−b−PAN)0.1g、Co前駆体としてのアセチルアセトナートコバルト0.057g、Ti前駆体としての塩化チタン0.030gを10mLのトルエンに溶解し、原料溶液を得た。なお、PMMA−b−PANのPMMAの分子量は27×103、PAAの分子量は24×103であった。また、Co前駆体およびTi前駆体と各構成要素との間の溶解度パラメータの差は以下の表3に示す通りであった。
ブロックコポリマーとしてのポリスチレン−b−ポリ(4−ビニルピリジン)(PS−b−P4VP)0.1g、硬磁性体であるFePt前駆体(Fe前駆体およびPt前駆体)としてのFe(acac)3 0.071gおよびPt(acac)2 0.079g、軟磁性体であるCo前駆体としてのCoCl2(4Me−Py)(cobalt dichloride bis-4-methyl pyridine)0.035gを10mLのトルエンに溶解し、原料溶液を得た。なお、PS−b−P4VPのPSの分子量は22×103、P4VPの分子量は22×103であった。また、FePt前駆体(Fe前駆体およびPt前駆体)およびCo前駆体と各構成要素との間の溶解度パラメータの差は以下の表4に示す通りであった。
非特許文献1に記載された方法にしたがって、粒径を制御したナノ粒子を出発物質として複合材料を作製した。すなわち、5nmの平均粒径を有するPdナノ粒子(Pd=0.17mmol)を含む1−オクタノール溶液20mLにオレイン酸6.8mmol、オレイルアミン6.8mmol、Fe(acac)3 0.43mmolを溶解した後、180℃で加熱することにより、Pdナノ粒子表面にγ−Fe2O3相を異方的に成長させたPd/γ−Fe2O3ナノ粒子を合成した。これを還元雰囲気(Ar+4%H2)中で焼成処理することにより、複合材料(FePd/Fe)を得た。
比較例2で用いたPdナノ粒子に代えて8.2nmの平均粒径を有するPtナノ粒子(Pt=0.17mmol)を用いた以外は比較例2と同様にして複合材料(FePt/Fe)を得た。得られた複合材料について実施例1と同様に透過型電子顕微鏡(TEM)で観察したところ、Feマトリックス中に分散したFePtナノ粒子には粒径や粒子間隔に大きな分布があり、周期的な構造は形成されていないことが確認された。また、得られた複合材料について実施例1と同様に小角X線回折パターンを測定したところ、周期構造に特徴的な回折ピークパターン(ピーク位置の回折スペクトルの大きさ(q)の比)は確認されなかった。
実施例1と同様にして得られた原料溶液を熱処理後の厚みが約500μmとなるように熱処理容器に入れ、アンモニア雰囲気中で550℃で6時間熱処理することによって無機構造体を得た。
ブロックコポリマーとしてのポリスチレン−b−ポリ(4−ビニルピリジン)(PS−b−P4VP)0.1g、硬磁性体であるFe前駆体としてのFe(acac)3 0.071g、軟磁性体であるCo前駆体としてのCoCl2(4Me−Py)(cobalt dichloride bis-4-methyl pyridine)0.035gを10mLのトルエンに溶解し、原料溶液を得た。なお、PS−b−P4VPのPSの分子量は22×103、P4VPの分子量は22×103であった。次に、得られた原料溶液を熱処理後の厚みが約500μmとなるように熱処理容器に入れ、アルゴン雰囲気中で900℃で12時間熱処理することによって無機構造体を得た。
実施例5と同様にして得られた原料溶液を熱処理後の厚みが約500μmとなるように熱処理容器に入れ、B4Cと共に真空中(10−3Torr)で1150℃で6時間熱処理することによって無機構造体を得た。
Claims (11)
- 互いに混和しない少なくとも第一ポリマーブロック成分と第二ポリマーブロック成分とが結合してなるブロックコポリマーと、前記第一ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2以下である第一無機前駆体と、前記第二ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2以下である第二無機前駆体と、を溶媒に溶解して原料溶液を調製する第一の工程と、
少なくとも、前記第一無機前駆体が導入された前記第一ポリマーブロック成分からなる第一ポリマー相と、前記第二無機前駆体が導入された前記第二ポリマーブロック成分からなる第二ポリマー相と、が自己組織化により規則的に配置したナノ相分離構造体を形成せしめる相分離処理と、前記第一無機前駆体および前記第二無機前駆体をそれぞれ第一無機成分および第二無機成分に変換せしめる変換処理と、前記ナノ相分離構造体から前記ブロックコポリマーを除去する除去処理とを含み、前記第一無機成分と前記第二無機成分とからなるナノヘテロ構造体を得る第二の工程と、
を含むナノヘテロ構造体の製造方法。 - 前記第一ポリマーブロック成分と前記第一無機前駆体との溶解度パラメータの差は、前記第一ポリマーブロック成分と前記第二無機前駆体との溶解度パラメータの差よりも小さい請求項1に記載のナノヘテロ構造体の製造方法。
- 前記第一ポリマーブロック成分と前記第一無機前駆体との溶解度パラメータの差は、前記第一ポリマーブロック成分と前記第二無機前駆体との溶解度パラメータの差よりも小さく、且つ、前記第二ポリマーブロック成分と前記第二無機前駆体との溶解度パラメータの差は、前記第二ポリマーブロック成分と前記第一無機前駆体との溶解度パラメータの差よりも小さい請求項1に記載のナノヘテロ構造体の製造方法。
- 前記第一ポリマーブロック成分と前記第二無機前駆体との溶解度パラメータの差が2(cal/cm3)1/2超である請求項1〜3のうちのいずれか一項に記載のナノヘテロ構造体の製造方法。
- 前記第一無機前駆体は前記第二ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2超であり、前記第二無機前駆体は前記第一ポリマーブロック成分との溶解度パラメータの差が2(cal/cm3)1/2超である請求項1〜4のうちのいずれか一項に記載のナノヘテロ構造体の製造方法。
- 前記第一無機前駆体および前記第二無機前駆体のうちの少なくとも一方は前記溶媒との溶解度パラメータの差が2(cal/cm3)1/2以下である請求項1〜5のうちのいずれか一項に記載のナノヘテロ構造体の製造方法。
- 前記第二の工程が、前記相分離処理、前記変換処理および前記除去処理として、前記原料溶液を熱処理する工程を含む請求項1〜6のうちのいずれか一項に記載のナノヘテロ構造体の製造方法。
- 前記熱処理を不活性ガス雰囲気中で行なう請求項7に記載のナノヘテロ構造体の製造方法。
- 前記不活性ガス雰囲気中での熱処理の後に、酸化ガス雰囲気中で前記第一無機成分および前記第二無機成分を酸化せしめる酸化処理、または、還元ガス雰囲気中で前記第一無機成分および前記第二無機成分を還元せしめる還元処理を更に含む請求項8に記載のナノヘテロ構造体の製造方法。
- 前記ナノヘテロ構造体が、前記第一無機成分および前記第二無機成分のうちの一方からなるマトリックス中に前記第一無機成分および前記第二無機成分のうちの他方が三次元的且つ周期的に配置しており、繰り返し構造の一単位の長さの平均値が1nm〜100nmである三次元的周期構造を有しているものである請求項1〜9のうちのいずれか一項に記載のナノヘテロ構造体の製造方法。
- 前記マトリックス中に三次元的且つ周期的に配置している前記無機成分の形状が、球状、柱状およびジャイロイド状からなる群から選択される形状である請求項10に記載のナノヘテロ構造体の製造方法。
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JP2014111305A (ja) | 2014-06-19 |
US9914666B2 (en) | 2018-03-13 |
US20150376071A1 (en) | 2015-12-31 |
WO2011115165A1 (ja) | 2011-09-22 |
US20130037740A1 (en) | 2013-02-14 |
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