JP5752128B2 - 製造方法 - Google Patents
製造方法 Download PDFInfo
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- JP5752128B2 JP5752128B2 JP2012530052A JP2012530052A JP5752128B2 JP 5752128 B2 JP5752128 B2 JP 5752128B2 JP 2012530052 A JP2012530052 A JP 2012530052A JP 2012530052 A JP2012530052 A JP 2012530052A JP 5752128 B2 JP5752128 B2 JP 5752128B2
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- metal compound
- boron
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- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000002245 particle Substances 0.000 claims description 119
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 85
- 239000000758 substrate Substances 0.000 claims description 72
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 59
- 229910052796 boron Inorganic materials 0.000 claims description 59
- 238000000034 method Methods 0.000 claims description 54
- 150000002736 metal compounds Chemical class 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 37
- 239000007789 gas Substances 0.000 claims description 36
- 238000003801 milling Methods 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 21
- 238000000576 coating method Methods 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 11
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 229910000760 Hardened steel Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000000976 ink Substances 0.000 description 112
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 91
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 48
- 238000000137 annealing Methods 0.000 description 27
- 239000002071 nanotube Substances 0.000 description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 23
- 229910052739 hydrogen Inorganic materials 0.000 description 21
- 238000006243 chemical reaction Methods 0.000 description 20
- 239000000843 powder Substances 0.000 description 20
- 230000015572 biosynthetic process Effects 0.000 description 19
- 229910000831 Steel Inorganic materials 0.000 description 18
- 239000002184 metal Substances 0.000 description 18
- 229910052751 metal Inorganic materials 0.000 description 18
- 239000010959 steel Substances 0.000 description 18
- 229910002651 NO3 Inorganic materials 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 15
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 15
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- 238000000498 ball milling Methods 0.000 description 13
- 238000001878 scanning electron micrograph Methods 0.000 description 12
- 238000001757 thermogravimetry curve Methods 0.000 description 11
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 10
- 238000002411 thermogravimetry Methods 0.000 description 10
- 230000004584 weight gain Effects 0.000 description 10
- 235000019786 weight gain Nutrition 0.000 description 10
- 238000005121 nitriding Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000001680 brushing effect Effects 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 239000002923 metal particle Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000012495 reaction gas Substances 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000000527 sonication Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000007641 inkjet printing Methods 0.000 description 3
- 229910001960 metal nitrate Inorganic materials 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 238000010422 painting Methods 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 150000001875 compounds Chemical group 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
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- 239000004615 ingredient Substances 0.000 description 2
- 238000005458 nitriding kinetic Methods 0.000 description 2
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- 230000001737 promoting effect Effects 0.000 description 2
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- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 241000870659 Crassula perfoliata var. minor Species 0.000 description 1
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000012669 liquid formulation Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- -1 nitrogen nitride Chemical class 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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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
- C01B21/0641—Preparation by direct nitridation of elemental boron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/14—Compounds containing boron and nitrogen, phosphorus, sulfur, selenium or tellurium
- C01B35/146—Compounds containing boron and nitrogen, e.g. borazoles
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
- C04B35/62286—Fibres based on nitrides
- C04B35/6229—Fibres based on nitrides based on boron nitride
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M103/06—Metal compounds
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/602—Nanotubes
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
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Description
・優れた熱伝導性、
・優れた機械的性質、
・強力な耐酸化性及び高い温度安定性(高温で化学的に無害)、
・安定な広いバンドギャップ(6eVに近い)、
・優れた放射線遮蔽(同位体10Bの存在による)、
・優れた圧電性、及び
・オプトエレクトロニクス性
がある。
(a)金属化合物及び平均粒度100nm未満のホウ素粒子を基材に施す工程(ホウ素粒子は、媒体中に分散したホウ素粒子を含む液体組成物の形態で施される)、
(b)基材を、窒素含有気体雰囲気中800〜1300℃の温度で加熱して、それにより、基材上に窒化ホウ素ナノチューブを成長させる工程
を含み、金属化合物が、加熱工程(b)中に窒化ホウ素ナノチューブの成長を促進するように選択されたものである方法を提供する。
(a)媒体中に溶解又は分散した金属化合物で基材をコートする工程、
(b)コートされた基材に、平均粒度100nm未満のホウ素粒子を含むインクを、インクジェット印刷、はけ塗装、吹き付け及び他の方法によって施す工程、
(c)基材を、回転/傾注管状炉中、窒素含有気体雰囲気中800〜1300℃の温度で加熱して、それにより、基材上に窒化ホウ素ナノチューブを成長させる工程
を含み、金属化合物が、工程(c)における加熱中に窒化ホウ素ナノチューブの成長を促進するように選択されたものである方法を提供する。
本発明にしたがって、BNNTを成長させることが望まれる基材表面へのホウ素粒子の塗布を容易にするためにインクが使用される。インクは、特定の粒度特性を有するホウ素粒子及び媒体を含む。媒体は、ホウ素粒子の均一な分散を可能にし、必要に応じて粒子を所望の形状で基材に施しやすくするためのものである。インクの使用はまた、多様な従来の好都合な塗布技術によってホウ素粒子を基材に施すことを可能にする。インクの使用はまた、ホウ素粒子の配合に関して融通を利かせ、これが、製造されるBNNTの特性、たとえば濃密度に影響することができる。
(a)媒体中に分散した平均粒度100nm未満のホウ素粒子及び媒体中に溶解又は分散した金属化合物を含むインクを基材に施す工程、
(b)基材を、窒素含有気体雰囲気中800〜1300℃の温度で加熱して、それにより、基材上に窒化ホウ素ナノチューブを成長させる工程
を含み、金属化合物が、工程(b)における加熱中に窒化ホウ素ナノチューブの成長を促進するように選択されたものである方法を提供する。
・B粉末が回転炉管に沿って転がり、反応ガスと十分に反応することができるため、不活性雰囲気下、一度により多くの材料を処理することができる。
・回転する加熱管がナノチューブの最小限の凝集及びより良好な分散を保証する。
・B粉末の十分な窒化による、より高いチューブ密度。
回転管状炉は主に、ばらのBNナノチューブを大量生産する場合に使用される。
B+N→BN
を経てBNNTを製造した。
乾燥B粒子のボールミル粉砕及びアニーリングの方法に比べ、液体インク法は、BNNTの密度及び純度を大きく改善する。TGAを使用して、アニーリング工程におけるエタノール及び硝酸塩の役割を調査した。図8aのTGA曲線は、N2−5%H2ガス中での加熱中のBインクの重量変化を示す。分析においては、0.02M Fe(NO3)3エタノール溶液を使用してBインク(溶液1ml中B100mg)を調製し、加熱速度は毎分20℃であった。アニーリング中のBインクの三つの異なる物理的及び化学的変化に関連する三つの異なる区分を曲線中に見ることができる。室温から145℃までの第一の区分にかけて、試料重量は34mgから4mgまで劇的に落ち込んだ。この急激な重量損失は、エタノール蒸発及びN2−5%H2ガスによる掃去によって生じたものである。145℃から400℃までの次の区分にかけて、試料重量は安定化した。しかし、この区分中、硝酸塩Fe(NO3)3が金属酸化物Fe2O3へと熱分解し、それがさらに還元されて、触媒として作用してナノチューブ成長を支援するナノサイズ金属粒子になった。最後の区分は400℃から1100℃までであり、ここでは、B粒子とN2ガスとの間の窒化反応のおかげで、BNの形成とともに試料重量が回復した。
Claims (14)
- 窒化ホウ素ナノチューブを製造する方法であって、ホウ素粒子及び金属化合物を含む液体組成物を加熱することを含み、加熱が、窒化ホウ素ナノチューブを成長させる窒素含有気体雰囲気中800〜1300℃の温度で実施され、ホウ素粒子が100nm未満の平均粒度を有し、金属化合物が、加熱中に窒化ホウ素ナノチューブの成長を促進するように選択されたものである方法。
- ホウ素粒子が10nm〜100nmの平均粒度を有する、請求項1記載の方法。
- ホウ素粒子が、乾燥した不活性ガス雰囲気中でより大きな粒度のホウ素粒子をミル粉砕することによって製造される、請求項1記載の方法。
- ミル粉砕が無水アンモニア中で実施される、請求項3記載の方法。
- ミル粉砕が硬化鋼ボールを使用して実施される、請求項4記載の方法。
- ミル粉砕が還元性雰囲気中で実施される、請求項5記載の方法。
- 金属化合物が、Fe、Cr、Ni、Co、Mo及びWの一つ以上から選択される、請求項1記載の方法。
- 金属化合物が、インク組成物に可溶性である塩の形態で使用される、請求項7記載の方法。
- 金属化合物がFe(NO3)3及びCO(NO3)3から選択される、請求項7記載の方法。
- 基材上に窒化ホウ素ナノチューブを製造する方法であって、以下の工程:
(a)媒体中に分散した平均粒度100nm未満のホウ素粒子及び媒体中に溶解又は分散した金属化合物を含むインクを基材に施す工程、
(b)基材を、窒素含有気体雰囲気中800〜1300℃の温度で加熱して、それにより、基材上に窒化ホウ素ナノチューブを成長させる工程
を含み、金属化合物が、工程(b)における加熱中に窒化ホウ素ナノチューブの成長を促進するように選択されたものである方法。 - 基材上に窒化ホウ素ナノチューブを製造する方法であって、以下の工程:
(a)媒体中に溶解又は分散した金属化合物で基材をコートする工程、
(b)コートされた基材に、平均粒度100nm未満のホウ素粒子を含むインクを施す工程、
(c)基材を、窒素含有気体雰囲気中800〜1300℃の温度で加熱して、それにより、基材上に窒化ホウ素ナノチューブを成長させる工程
を含み、金属化合物が、工程(c)における加熱中に窒化ホウ素ナノチューブの成長を促進するように選択されたものである方法。 - 請求項10又は請求項11記載の方法によって製造された窒化ホウ素ナノチューブでコートされた基材。
- レーザ装置、機械加工部品固体潤滑剤、電界放出装置又は他の電子装置における請求項12記載の基材の使用。
- 基材を酸化又は化学的攻撃から保護する方法であって、請求項10又は請求項11記載の方法によって製造された窒化ホウ素ナノチューブで基材をコートすることを含む方法。
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