JP7440726B2 - 新規sp2-sp3ハイブリッドクリスタル窒化ホウ素 - Google Patents
新規sp2-sp3ハイブリッドクリスタル窒化ホウ素 Download PDFInfo
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 212
- 229910052582 BN Inorganic materials 0.000 title claims description 211
- 239000013078 crystal Substances 0.000 title claims description 52
- 238000009396 hybridization Methods 0.000 claims description 54
- 230000005496 eutectics Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 description 48
- 238000001035 drying Methods 0.000 description 25
- 239000000463 material Substances 0.000 description 17
- 238000000619 electron energy-loss spectrum Methods 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 13
- 238000004098 selected area electron diffraction Methods 0.000 description 13
- 230000005540 biological transmission Effects 0.000 description 10
- 239000012535 impurity Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000011160 research Methods 0.000 description 7
- 241000234282 Allium Species 0.000 description 6
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 229910052796 boron Inorganic materials 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 229910003460 diamond Inorganic materials 0.000 description 5
- 239000010432 diamond Substances 0.000 description 5
- 229910052984 zinc sulfide Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical group [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000002106 nanomesh Substances 0.000 description 3
- 239000002071 nanotube Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 nitride Boron nitride Chemical class 0.000 description 1
- 238000009931 pascalization Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C30B1/00—Single-crystal growth directly from the solid state
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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Description
窒化ホウ素原料をプレプレス金型に入れて、プレス機によって、窒化ホウ素原料を窒化ホウ素原料本体(raw material body)にプレ成形した後、真空熱圧焼結炉内に入れてプレ加熱する工程(1)と、
工程(1)でプレ加熱された窒化ホウ素原料本体をアセンブリブロックに入れた後、窒化ホウ素原料本体を含むアセンブリブロックを乾燥させる(例えば、乾燥ボックス内で乾燥させる)工程(2)と、
工程(2)で乾燥されたアセンブリブロック(任意に選択して冷却した後)をプレス機に入れて高温高圧操作を行う工程(3)と、
放圧後、プレス機から取り出したアセンブリブロックを冷却し、sp2-sp3ハイブリダイゼーションクリスタル窒化ホウ素を得る工程(4)と、を含む。
1種類以上の窒化ホウ素原料(例えば、hBN、rBN、窒化ホウ素ナノチューブ、非晶質窒化ホウ素及びオニオン窒化ホウ素等を含むsp2ハイブリダイゼーション窒化ホウ素原料)をプレプレス金型に入れ、プレス機によって窒化ホウ素原料が直円筒形の本体にプレ成形した後、真空熱圧焼結炉内に入れてプレ加熱を行い、プレ加熱温度が200~1800℃であり、プレ加熱時間が5~60minであり、プレ加熱圧力が20~50MPaである工程(1)と、
工程(1)でプレ加熱された窒化ホウ素原料本体をアセンブリブロックに入れた後、窒化ホウ素原料本体を含むアセンブリブロックを乾燥ボックス内に入れて乾燥し、乾燥温度が100~200℃であり、乾燥時間が1~3hである工程(2)と、
工程(2)のアセンブリブロックを取り出して室温まで冷却し、続いてアメリカRockland Research社製T25型プレス機に入れて高温高圧操作を行い、合成圧力が3~25GPaであり、温度が600~2500℃であり、保温時間が5~120minである工程(3)と、
プレス機を冷却し圧力開放し後、プレス機からアセンブリブロックを取り出し、サンプル周囲のアセンブリブロックを除去して、新規sp2-sp3ハイブリッドクリスタル窒化ホウ素-Gradia窒化ホウ素を得る工程(4)と、を含む。
工程(1):hBN原料をプレプレス金型に入れ、プレス機を用いて40MPaの圧力で約5minプレプレスして、円筒形の本体を得た後、真空熱圧焼結炉内に入れてプレ加熱を行い、プレ加熱温度を1500℃前後に制御し、プレ加熱時間を約40minに制御する。
工程(1):窒化ホウ素ナノチューブをプレプレス金型に入れ、プレス機を用いて30MPaの圧力で約10minプレプレスして、円筒形の本体を得た後、真空熱圧焼結炉内に入れてプレ加熱を行う。プレ加熱温度は1400℃前後に制御し、プレ加熱する焼き時間は15~20minに制御する。
工程(1):オニオン窒化ホウ素をプレプレス金型に入れ、プレス機を用いて50MPaの圧力で15minプレプレスして、円筒形の本体を得る。
実施例3の工程(1)~(4)を繰り返すが、工程(3)における合成圧力及び温度を20GPa及び800℃とする。
工程(1):hBN原料を希塩酸溶液に入れて不純物を除去し、酸洗浄後、hBN原料を分離し、メタノールで複数回洗浄する。洗浄後の窒化ホウ素原料を乾燥処理して、精製されたhBN原料を得る。原料をプレプレス金型に入れ、プレス機を用いて20MPaの圧力で5minプレ成形して、円筒形の本体を得た後、真空熱圧焼結炉内に入れてプレ加熱を行う。プレ加熱圧力が30MPa、プレ加熱温度が1200℃、プレ加熱時間が20分である。
工程(1):cBN原料粉末に対して精製、真空加熱等の前処理を行い、原料粉末に吸着された酸素、吸着水及び結合水等の不純物を除去する。具体的には、酸溶解による不純物の除去によって精製し、精製後の原料粉末は真空ホットプレス炉の金型内に充填される。真空ホットプレス炉の真空度が5*10-2以下で、温度が1600℃、圧力が30MPaであり、15min保持する。
立方晶窒化ホウ素(cBN)を原料として、実施例5の工程(1)~(4)を繰り返すが、工程(3)における合成圧力及び温度は6GPa及び1700℃とする。
工程(1):hBN原料を希塩酸溶液に入れて不純物を除去し、酸洗浄後、hBN原料を分離して、メタノールで複数回洗浄する。洗浄後の窒化ホウ素原料を乾燥処理して、精製されたhBN原料を得る。原料をプレプレス金型に入れ、プレス機を用いて20MPaの圧力で55minプレ成形して、円筒形の本体を得た後、真空熱圧焼結炉内に入れてプレ加熱を行う。プレ加熱圧力が30MPa、プレ加熱温度が1200℃、プレ加熱時間が20分である。
Claims (2)
- 基本構造ユニットがsp2ハイブリダイゼーションのグラファイト様構造ユニット及びsp3ハイブリダイゼーションのダイヤモンド様構造ユニットからなり、前記グラファイト様構造ユニットと前記ダイヤモンド様構造ユニットが、特定の共晶面を介して共有結合により互いに結合されており、
その空間群が4(P2 1 )又は6(Pm)又は8(Cm)である単結晶であるか、或いは、4(P2 1 )又は6(Pm)又は8(Cm)の空間群を有する二相又は多相からなる多結晶である、
ことを特徴とするsp2-sp3ハイブリッドクリスタル窒化ホウ素。 - 前記sp2-sp3ハイブリッドクリスタル窒化ホウ素の結晶構造は、その内部のsp2ハイブリダイゼーションのグラファイト様構造ユニット及びsp3ハイブリダイゼーションのダイヤモンド様構造ユニットのサイズ及び結晶方位関係によって変化する、
ことを特徴とする請求項1に記載のsp2-sp3ハイブリッドクリスタル窒化ホウ素。
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CN202010305181.4A CN113526475B (zh) | 2020-04-17 | 2020-04-17 | sp2-sp3杂化的晶态氮化硼及其制备方法 |
CN202010305181.4 | 2020-04-17 | ||
JP2020180784A JP7182299B2 (ja) | 2020-04-17 | 2020-10-28 | 新規sp2-sp3ハイブリッドクリスタル窒化ホウ素の調製方法 |
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