JP7276625B2 - 窒化ホウ素ナノチューブの製造方法 - Google Patents
窒化ホウ素ナノチューブの製造方法 Download PDFInfo
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- JP7276625B2 JP7276625B2 JP2022562199A JP2022562199A JP7276625B2 JP 7276625 B2 JP7276625 B2 JP 7276625B2 JP 2022562199 A JP2022562199 A JP 2022562199A JP 2022562199 A JP2022562199 A JP 2022562199A JP 7276625 B2 JP7276625 B2 JP 7276625B2
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 89
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 34
- 239000006227 byproduct Substances 0.000 claims description 33
- 229920000642 polymer Polymers 0.000 claims description 31
- 239000006185 dispersion Substances 0.000 claims description 30
- 229910052582 BN Inorganic materials 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 10
- 239000002071 nanotube Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920003174 cellulose-based polymer Polymers 0.000 claims 1
- 239000000047 product Substances 0.000 description 23
- 229910003472 fullerene Inorganic materials 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 17
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 15
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
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- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
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- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 description 1
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- SMEGJBVQLJJKKX-HOTMZDKISA-N [(2R,3S,4S,5R,6R)-5-acetyloxy-3,4,6-trihydroxyoxan-2-yl]methyl acetate Chemical compound CC(=O)OC[C@@H]1[C@H]([C@@H]([C@H]([C@@H](O1)O)OC(=O)C)O)O SMEGJBVQLJJKKX-HOTMZDKISA-N 0.000 description 1
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- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- BGECDVWSWDRFSP-UHFFFAOYSA-N borazine Chemical compound B1NBNBN1 BGECDVWSWDRFSP-UHFFFAOYSA-N 0.000 description 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 1
- 239000001191 butyl (2R)-2-hydroxypropanoate Substances 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
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-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Carbon And Carbon Compounds (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Inorganic Fibers (AREA)
Description
である。
なお、本発明において、「合成後の生成物」とは、合成した直後の状態の生成物のみではなく、BNNTを合成した後であって、本発明にかかる工程よりも前に、他の処理を施したものを含む。すなわち、窒化ホウ素ナノチューブを含む原料としては、合成したままの生成物に限らず、合成したままの生成物に含まれる副生成物を他の処理等によりある程度除去した窒化ホウ素ナノチューブ生成物も含む。したがって、以下の説明において、「合成後の生成物」は、後述する本発明にかかるBNNTの製造工程に用いられる窒化ホウ素ナノチューブを含む原料を全て含むものとする。
なお、カーボンナノチューブ(CNT)のポリマー分散剤として広く適用されるカルボキシメチルセルロース(CMC)は、sp3結合性のCH基を有するイオン性ポリマーであり、水系溶媒が用いられる。このCMCを細径のBNNTの分散剤として適用した場合、BNNT周辺にミセルが形成され、ミセルによって形成される疎水性空間にBNNTが内包されることでBNNTが可溶化する。しかし、ミセルのサイズが物質の形状に追従し、形状によらず可溶化するため、BNNT以外の副生成物も可溶化する。このため、CMCは、細径のBNNTのみを選択的に可溶化させにくいと考えられる。一方、sp3結合性のCH基を有する非イオン性ポリマーの場合、有機溶媒を使用するため、BNNT周辺にミセルは形成されない。このため、BNNTと不純物(BNNT以外の副生成物)の形状やサイズの差異により、それぞれへの分散剤の吸着性および、これらの可溶化性に差異が生じ、BNNTと不純物を分離しやすく、選択的にBNNTを分散できると考えられる。
まず、評価に用いられる窒化ホウ素ナノチューブ分散液を下記の方法で準備した。まず、小型プラズマ装置(TEKNA Plasma Systems inc.製 TekNanо―15)を用い、以下の要領で副生成物を含有するBNNT生成物、すなわち窒化ホウ素ナノチューブを含む原料を合成した。始めに、反応容器内をアルゴンガスでパージした。次に、中央領域にアルゴンガス(流速:10L/min)を流し、アルゴン(30L/min)と水素(2.5L/min)の混合ガスを流すことにより、プラズマを閉じ込める管の外周にシースガスを流す。窒素ガスは、トーチノズル(10L/min)と反応容器を取り囲むポーラスウォール(47L/min)の両方を通して流される。プラズマ着火から数分後、反応容器とサイクロンの間に設置した熱電対の温度が一定になった時点で、素原料のh-BN粉末(平均粒径:5μm)をプラズマトーチの上部に設置したフィーダから、アルゴン(2.5L/min)をキャリアガスとして連続供給した。供給速度は0.5g/min、運転時間は2hr、反応チャンバ内圧力は1atmとした。合成が終了した後、装置を分解して、プラズマトーチ、リアクタ、サイクロン及びフィルター部に付着した生成物を回収した。
また、実施例1、実施例2、比較例1、比較例2について、それぞれ、以下の式にて、分散したBNNTの収率を求めた。
収率(%)={([合成後の生成物質量]―[遠心分離後の残渣の質量])/[合成後の生成物質量]}×100
その結果、実施例1(55%)>実施例2(51%)>比較例1(32%)>比較例2(20%)の順で、収率が高いことが分かった。
比較例1の分散液は、sp2結合性の主鎖を持つため、sp3結合性の主鎖を有するEC、PVBと比較して剛直であり、特に細径のBNNTに巻き付きにくく、分散性が劣ったものと考えられる。
これらの結果より、本発明の分散剤を適用した場合、比較例の分散剤を適用した場合に比べて、副生成物の残量が少なく(BNNTの純度が高く)、かつ、BNNTの収率が高くなることがわかった。
102・・・BNフラーレン
103・・・h-BN薄片
302・・・エチルセルロース
Claims (2)
- 窒化ホウ素ナノチューブを含む原料と、
sp3結合性のCH基を有する非イオン性ポリマー分散剤と、
有機溶媒と、を混合し、懸濁液を得る工程と、
得られた懸濁液を遠心分離し、原料に含まれる副生成物を除去し、窒化ホウ素ナノチューブを含む分散液を得る工程と、
を有することを特徴とする窒化ホウ素ナノチューブの製造方法。 - 前記ポリマー分散剤が、セルロース系ポリマー又はビニル系ポリマーを含むことを特徴とする請求項1に記載の窒化ホウ素ナノチューブの製造方法。
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JP2011102203A (ja) | 2009-11-10 | 2011-05-26 | Teijin Ltd | 窒化ホウ素ナノチューブ誘導体、その分散液、及び該窒化ホウ素ナノチューブ誘導体の製造方法 |
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