WO2021193046A1 - 六方晶窒化ホウ素粉末の製造方法 - Google Patents
六方晶窒化ホウ素粉末の製造方法 Download PDFInfo
- Publication number
- WO2021193046A1 WO2021193046A1 PCT/JP2021/009425 JP2021009425W WO2021193046A1 WO 2021193046 A1 WO2021193046 A1 WO 2021193046A1 JP 2021009425 W JP2021009425 W JP 2021009425W WO 2021193046 A1 WO2021193046 A1 WO 2021193046A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- boron nitride
- hexagonal boron
- lithium
- nitride powder
- alkali metal
- Prior art date
Links
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 239000011812 mixed powder Substances 0.000 claims abstract description 72
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 67
- 238000010438 heat treatment Methods 0.000 claims abstract description 66
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 59
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 51
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052796 boron Inorganic materials 0.000 claims abstract description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 28
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 19
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 12
- 150000002641 lithium Chemical group 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 71
- 229910052582 BN Inorganic materials 0.000 abstract description 58
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 description 50
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 37
- 239000007789 gas Substances 0.000 description 26
- 229920005989 resin Polymers 0.000 description 24
- 239000011347 resin Substances 0.000 description 24
- 238000000034 method Methods 0.000 description 21
- 239000011342 resin composition Substances 0.000 description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 18
- -1 nitrogen-containing organic compound Chemical class 0.000 description 18
- 229920000877 Melamine resin Polymers 0.000 description 16
- 239000003822 epoxy resin Substances 0.000 description 16
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 16
- 229920000647 polyepoxide Polymers 0.000 description 16
- 239000002253 acid Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 238000011156 evaluation Methods 0.000 description 13
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 12
- 229910052808 lithium carbonate Inorganic materials 0.000 description 12
- 238000001000 micrograph Methods 0.000 description 12
- 238000002156 mixing Methods 0.000 description 12
- 229910003002 lithium salt Inorganic materials 0.000 description 10
- 159000000002 lithium salts Chemical class 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 229910052810 boron oxide Inorganic materials 0.000 description 8
- 238000010304 firing Methods 0.000 description 8
- 239000011261 inert gas Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000012299 nitrogen atmosphere Substances 0.000 description 8
- 230000004907 flux Effects 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000005755 formation reaction Methods 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229920002050 silicone resin Polymers 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000007716 flux method Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000007259 addition reaction Methods 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
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 1
- 208000019901 Anxiety disease Diseases 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 244000241257 Cucumis melo Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- YSKUZVBSHIWEFK-UHFFFAOYSA-N ammelide Chemical compound NC1=NC(O)=NC(O)=N1 YSKUZVBSHIWEFK-UHFFFAOYSA-N 0.000 description 1
- MASBWURJQFFLOO-UHFFFAOYSA-N ammeline Chemical compound NC1=NC(N)=NC(O)=N1 MASBWURJQFFLOO-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000036506 anxiety Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 150000001649 bromium compounds Chemical class 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- STIAPHVBRDNOAJ-UHFFFAOYSA-N carbamimidoylazanium;carbonate Chemical compound NC(N)=N.NC(N)=N.OC(O)=O STIAPHVBRDNOAJ-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 125000005388 dimethylhydrogensiloxy group Chemical group 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 125000006038 hexenyl group Chemical group 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000002648 laminated material Substances 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- MTKRXXSLFWZJTB-UHFFFAOYSA-N oxo(oxoboranyl)borane Chemical compound O=BB=O MTKRXXSLFWZJTB-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon 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
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 238000010333 wet classification Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
-
- 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
- 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
- C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/40—Particle morphology extending in three dimensions prism-like
Definitions
- the present invention relates to a novel method for producing hexagonal boron nitride powder.
- Hexagonal boron nitride has high thermal conductivity, and a resin composition in which hexagonal boron nitride powder is filled in a resin as a heat dissipation filler is used for heat dissipation of electronic parts.
- Known methods for producing hexagonal boron nitride include a flux method in which boron nitride is dissolved in an inorganic compound as a flux and precipitated, and a melamine method in which boron nitride is nitrided using a nitrogen-containing organic compound as a nitrogen source. ing.
- Hexagonal boron nitride particles have a significantly smaller thermal conductivity in the c-axis direction of the crystal than the thermal conductivity in the ab-axis direction of the crystal.
- they are hexagonal composed of hexagonal boron nitride particles.
- the resin composition filled with crystallization boron nitride powder has a problem of thermal conductivity anisotropy, in which hexagonal boron nitride particles are oriented in the molding process and the thermal conductivity greatly differs depending on the orientation of the resin composition. rice field.
- This thermal conduction anisotropy can be improved by bringing the aspect ratio represented by the ratio of the major axis to the thickness (major axis / thickness) of the hexagonal boron nitride particles close to 1.
- the aspect ratio represented by the ratio of the major axis to the thickness (major axis / thickness) of the hexagonal boron nitride particles close to 1.
- Patent Document 1 in the flux method, boron nitride powder and lithium carbonate are mixed so that lithium carbonate is 50 mol%. Therefore, a method of heating this has been proposed.
- thick hexagonal boron nitride particles grown in the c-axis direction can be obtained by crystal growth driven by the decomposition and evaporation of lithium carbonate.
- hexagonal boron nitride powder containing thick hexagonal boron nitride particles can be obtained by using lithium in the flux method.
- the present inventors in the melamine method, as raw materials, a boron source and a nitrogen source. And proposed a method using a mixed powder containing lithium.
- the present inventors conducted diligent research. As a result, when the amount of lithium used is reduced, the aspect ratio tends to increase, and it is not possible to obtain thick hexagonal boron nitride particles, and even if an alkali metal similar to lithium is used, the wall thickness is high. It was confirmed that hexagonal boron nitride could not be obtained. Then, as a result of further studies, surprisingly, in the melamine method, a part of lithium in the mixed powder containing the raw materials boron source, nitrogen source and lithium was replaced with an alkali metal other than lithium, and lithium was used. The present invention has been completed based on the finding that hexagonal boron nitride particles having a low aspect ratio equivalent to that when a considerable amount of lithium is used can be produced even if the amount used is reduced.
- the present invention contains an organic compound containing a nitrogen atom and a boron source in which the molar ratio of the boron atom to the nitrogen atom is adjusted to 0.26 or more and 0.67 or less, and the lithium atom is 30 mol.
- the alkali metal adjusted to the range of% or more and less than 100 mol% was allowed to exist so that the molar ratio of the boron atom to the alkali metal atom contained in the alkali metal was 0.75 or more and 3.35 or less.
- a method for producing a hexagonal boron nitride powder which comprises a step of preparing a mixed powder and a heating step of heating the mixed powder at a maximum temperature of 1200 ° C. or higher and 1500 ° C. or lower.
- a hexagonal boron nitride powder containing thick hexagonal boron nitride particles capable of reducing the thermal conduction anisotropy of the resin composition can be produced with a smaller amount of lithium than before. Is possible. This makes it possible to provide a process for producing hexagonal boron nitride powder containing thick hexagonal boron nitride particles, which is inexpensive and has less concern about the supply of raw materials, which is industrially advantageous.
- the mixed powder of the present invention contains an organic compound containing a nitrogen atom and a boron source in which the molar ratio of the boron atom to the nitrogen atom is adjusted to 0.26 or more and 0.67 or less, and the lithium atom is 30. It is a mixed powder in which an alkali metal adjusted in the range of mol% to less than 100 mol% is present so that the molar ratio of boron atoms to the alkali metal atoms is 0.75 or more and 3.35 or less.
- Examples of the boron source contained in the mixed powder of the present invention include diboron trioxide (boron oxide), diboron dioxide, tetraboron trioxide, tetraboron pentoxide, borax, and anhydrous borax.
- diboron trioxide is preferable from the viewpoint of being industrially beneficial because it uses an inexpensive raw material.
- borax or anhydrous borax from the viewpoint that it is a relatively inexpensive raw material and that fluctuations in the particle size and the like of the hexagonal boron nitride particles produced so that the reaction can proceed substantially uniformly are easily suppressed. ..
- Two or more types may be used in combination as the boron source.
- Examples of the nitrogen-containing organic compound contained in the mixed powder of the present invention include melamine, ammeline, ammelide, melamine, melon, dicyandiamide, guanidine, guanidine carbonate, and urea, and melamine and urea are preferable.
- Melamine is particularly preferred. By using melamine as an organic compound containing nitrogen, it is industrially beneficial because an inexpensive raw material is used. Two or more kinds of organic compounds containing nitrogen may be used in combination.
- the mixed powder of the present invention contains an alkali metal, and the alkali metal contains both lithium in the range of 30 mol% or more and less than 100 mol% and an alkali metal other than lithium.
- Alkali metals are generally added to the mixed powder as alkali metal salts. When the alkali metal salt melts, it becomes a flux that acts as an auxiliary agent for growing hexagonal boron nitride particles.
- the aspect ratio of the hexagonal boron nitride particles tended to increase, but even if the amount of lithium was reduced by allowing an alkali metal other than lithium to exist. It is possible to suppress an increase in the aspect ratio.
- thick hexagonal boron nitride particles cannot be obtained.
- the alkali metal salt is not particularly limited as long as it melts during heating and acts as a flux.
- the lithium salt include lithium carbonate, lithium hydroxide, lithium chloride, lithium iodide, lithium fluoride, lithium nitrate, lithium sulfate, lithium borate, and lithium molybdenate.
- lithium carbonate when lithium carbonate is used, it tends to be easy to obtain the above-mentioned thick hexagonal boron nitride particles, which is preferable.
- Two or more kinds of lithium salts may be used in combination.
- the proportion of lithium in the alkali metal is preferably 45 mol% or more, more preferably 55 mol% or more.
- the proportion of lithium is large, there is no particular problem in the physical properties of the obtained hexagonal boron nitride powder, but the effect of reducing the amount of lithium used is limited, so lithium in alkali metals.
- the ratio of is preferably 90 mol% or less, more preferably 70 mol% or less.
- the alkali metal other than lithium is preferably sodium or potassium because it is inexpensive and easily available, and it is easy to prevent excessive volatilization of flux that causes deterioration of the heating furnace body. Therefore, sodium is more preferable. Two or more kinds of alkali metals other than lithium may be used in combination.
- alkali metal salts other than lithium examples include carbonates, nitrates, borates, hydroxides, fluorides, chlorides, bromides, and iodides.
- the alkali metal borate can also serve as a boron source and an alkali metal salt other than lithium.
- the molar ratio (B / N) of boron atoms to nitrogen atoms in the mixed powder of the present invention is 0.26 or more and 0.67 or less, and preferably 0.32 or more and 0.45 or less.
- B / N is 0.26 or more
- a high yield can be ensured.
- B / N is 0.67 or less
- a sufficient nitrogen source for nitriding can be secured.
- the nitrogen atom in the mixed powder heated in the heating step is derived from an organic compound containing nitrogen
- the boron atom in the mixed powder heated in the heating step is derived from a boron source.
- the molar ratio (B / AM) of boron atoms to alkali metal atoms in the mixed powder of the present invention is 0.75 or more and 3.35 or less, and preferably 0.82 or more and 2.70 or less.
- B / AM is 0.75 or more
- hexagonal boron nitride having a sufficient wall thickness can be obtained in order to improve the thermal conduction anisotropy.
- B / AM is 3.35 or less, a sufficient amount of flux can be formed, so that thick hexagonal boron nitride particles can be uniformly obtained.
- the mixed powder may contain a boron source, an organic compound containing nitrogen, and a substance other than an alkali metal as long as the effects of the present invention are not impaired.
- the mixed powder may be prepared by mixing a boron source, an organic compound containing nitrogen, an alkali metal, etc. by a known method. By mixing before the heating step, the reaction proceeds substantially uniformly, so that fluctuations in the particle size and the like of the hexagonal boron nitride particles in the produced hexagonal boron nitride powder are suppressed.
- the mixed powder is heated at a maximum temperature of 1200 ° C. or higher and 1500 ° C. or lower.
- the maximum temperature is more preferably 1250 ° C. or higher.
- the maximum temperature is more preferably 1450 ° C. or lower.
- the maximum temperature it is possible to control the particle size of the obtained hexagonal boron nitride powder. Therefore, for example, by setting the maximum temperature to 1350 ° C. or lower, a hexagonal boron nitride powder having a small particle size of about 0.1 ⁇ m to 0.4 ⁇ m can be obtained, and the maximum temperature is about 1400 ° C. to 1500 ° C. Therefore, a hexagonal boron nitride powder having a particle size of about 0.5 ⁇ m to 2.0 ⁇ m can be obtained.
- the heating step is preferably under an inert gas atmosphere and under normal pressure or reduced pressure environment to heat the mixed powder.
- an inert gas atmosphere is a state in which the inert gas is allowed to flow into a container for heating the mixed powder, and the gas inside the container is replaced with the inert gas.
- the inflow amount of the inert gas is not particularly limited, but the inflow amount of the inert gas is 5 L / min. That may be the above.
- the inert gas may be, for example, nitrogen gas, carbon dioxide gas, argon gas or the like.
- the heating step arranging the mixed powder inside the reaction vessel where gas exchange does not occur during the heating step can be exemplified as a preferable method.
- the boron source contained in the mixed powder is used in the hexagonal boron nitride formation reaction, but part of it is volatilized by heating and is not used in the hexagonal boron nitride formation reaction.
- volatilization of the boron source from the mixed powder can be suppressed.
- the amount of the boron source used in the reaction for producing hexagonal boron nitride can be increased, and the yield of hexagonal boron nitride can be improved.
- gas exchange does not occur means that the gas inside the reaction vessel and the gas outside the reaction vessel are not exchanged.
- gas is generated inside the reaction vessel due to the progress of the hexagonal boron nitride formation reaction and the volatilization or decomposition of the mixed powder. Therefore, it is not necessary to intentionally take in the gas from the outside into the reaction vessel, and it is not necessary to completely prevent the gas inside the reaction vessel from being released to the outside of the reaction vessel.
- the structure, size, shape, material, etc. of the reaction vessel are not particularly limited, and the reaction vessel should have sufficient durability, heat resistance, pressure resistance, corrosion resistance, etc. in consideration of the manufacturing conditions such as heating temperature and raw materials. Can be decided.
- reaction vessel with a lid As a mechanism for preventing gas exchange, for example, using a reaction vessel with a lid as a reaction vessel can be mentioned.
- a reaction vessel with a lid since it is separated from the outside by a lid, the inflow of gas from the outside of the reaction vessel can be suppressed and gas exchange does not occur.
- the inside of the vessel is caused by the progress of the hexagonal boron nitride formation reaction, the generation of gas by volatilization or decomposition of the mixed powder, or the expansion of the gas in the reaction vessel by heating. Pressure increases.
- the reaction vessel may be damaged, or the material and shape of the reaction vessel may be restricted because the reaction vessel has a pressure-resistant structure. Therefore, it is preferable to appropriately release the excess gas inside the reaction vessel within a range that does not significantly affect the yield of hexagonal boron nitride.
- Examples of the method of releasing the excess gas inside the reaction vessel include a method of attaching a pressure control valve to the reaction vessel and a method of making a small hole in the reaction vessel.
- the reaction vessel is a container with a lid
- the lid is placed on the upper part of the reaction vessel, and the reaction vessel is sealed by the weight of the lid when the internal pressure is low.
- the internal pressure rises, the lid is lifted and the gas inside the reaction vessel is discharged to the outside. Therefore, by using a container with a lid, it is possible to release excess gas inside the reaction vessel while preventing gas exchange from occurring easily, which is a preferable form.
- the weight of the lid per unit area is preferably in the range of 5 kg / m 2 to 20 kg / m 2.
- the weight of the lid per unit area is a value obtained by dividing the weight of the lid by the area of the lid facing the internal space of the reaction vessel.
- the shape of the reaction vessel is not particularly limited, and any shape such as a cylindrical shape or a square shape can be used.
- the shape of the reaction vessel is preferably cylindrical from the viewpoint of preventing damage to the reaction vessel due to repeated heating and cooling, and from the viewpoint of effectively utilizing space when installing in the heating furnace to improve production efficiency.
- a square shape is preferable.
- the material of the reaction vessel is not particularly limited as long as it can withstand the heating temperature of 1200 ° C. or higher and 1500 ° C. or lower in the heating step, and the main components are alumina, titania, zirconia, silica, magnesia and calcia, and silica and alumina. Examples thereof include various ceramic sintered bodies such as Kojilite and Mullite. Further, from the viewpoint of preventing contamination of hexagonal boron nitride, which is a reaction product, it is also preferable to use boron nitride as the material of the reaction vessel, and the inner surface (mixed powder) of the reaction vessel manufactured of a material other than boron nitride. It is also possible to mention as a preferable mode that the surface to which the generated hexagonal boron nitride is in contact) is coated with boron nitride.
- the amount of the mixed powder to be placed inside the reaction vessel is not particularly limited, but if it is too small, the volatilization of the boron source is not sufficiently suppressed because there are many vapor phases in the reaction vessel, and the effect of improving the yield is limited. Become. On the other hand, if the amount of the mixed powder is too large, the pressure in the reaction vessel tends to increase because the gas phase portion is small. Therefore, the volume occupied by the mixed powder in the reaction vessel is preferably in the range of 50% to 90% of the volume of the reaction vessel, and more preferably 60% to 80%. In the present specification, the volume occupied by the mixed powder is the volume of the portion occupied by the mixed powder including the voids between the particles of the mixed powder when placed in the reaction vessel.
- the method of heating the mixed powder arranged inside the reaction vessel in which gas exchange does not occur is not particularly limited, but it is preferable to install the reaction vessel in the heating furnace and heat it to a desired temperature because it can be easily carried out. It is a form.
- a batch type heating furnace such as a shuttle kiln or a continuous type heating furnace such as a tunnel kiln can also be used.
- a continuous heating furnace capable of heating while moving a reaction vessel such as a tunnel kiln in the furnace is a particularly preferable form with high production efficiency.
- the heating source may be an electric heater, but it is more convenient to heat with hot air obtained by burning fuel such as butane gas or kerosene, which is more preferable. It is a form.
- the method for producing hexagonal boron nitride powder of the present invention may include steps other than the step of preparing the mixed powder and the step of heating. Such steps are referred to herein as "other steps”. Other steps included in the method for producing hexagonal boron nitride powder include, for example, an acid washing step, a water washing step, a drying step, and a classification step.
- the acid cleaning step is a step of removing reaction by-products such as boron sources, alkali metal salts, and composite oxides adhering to the hexagonal boron nitride powder by cleaning the hexagonal boron nitride powder with an acid. ..
- a dilute acid such as hydrochloric acid.
- the acid cleaning method is not particularly limited, and may be acid cleaning by showering, acid cleaning by soaking, or acid cleaning by stirring.
- the water cleaning step is a step of washing the hexagonal boron nitride powder with water in order to remove the acid adhering to the hexagonal boron nitride powder in the acid cleaning step.
- the water washing method is not particularly limited, and the hexagonal boron nitride powder may be washed with water by showering after filtering, or may be washed with water by soaking.
- the drying step is a step of drying the produced hexagonal boron nitride powder.
- the drying method is not particularly limited, such as high temperature drying or vacuum drying.
- the classification step is a step of dividing hexagonal boron nitride particles according to the size and / or shape of the particles.
- the classification operation may be sieving, and may be wet classification or air flow classification.
- the hexagonal boron nitride powder obtained by the production method of the present invention has an aspect ratio of 1.0 or more and 5.0 or less.
- the fact that the aspect ratio is in this range means that the hexagonal boron nitride powder contains thick hexagonal boron nitride particles, and the thermal conduction anisotropy can be reduced.
- a hexagonal boron nitride particle means a single particle of hexagonal boron nitride.
- the hexagonal boron nitride particles are usually plate-shaped particles, and in the present specification, the maximum diameter of the plate-shaped particles on the plate surface is referred to as the major axis, and the length perpendicular to the plate surface is referred to as the thickness. .. Then, the value obtained by dividing this major axis by the thickness is referred to as an aspect ratio.
- the aspect ratio of the hexagonal boron nitride powder was obtained by randomly selecting 100 different hexagonal boron nitride particles from a scanning electron microscope observation image at a magnification of 5000 times and measuring the length and thickness of the major axis of each primary particle. It is the average value of the aspect ratio of each particle.
- the particle size of the hexagonal boron nitride powder may be appropriately selected depending on the intended use, but is preferably in the range of 0.1 ⁇ m to 2.0 ⁇ m, and more preferably in the range of 0.1 ⁇ m to 0.4 ⁇ m. ..
- the particle size is 0.1 ⁇ m or more, a heat conduction path in the resin composition can be sufficiently formed, and a resin composition having high thermal conductivity can be easily obtained. In addition, it is easy to fill the resin, and the handleability of the resin composition is improved.
- the particle size is 2.0 ⁇ m or less, the filling property of the hexagonal boron nitride powder into the resin becomes high, and it becomes easy to obtain a resin composition having good handleability and high thermal conductivity.
- the particle size of the hexagonal boron nitride powder in the present invention 100 different hexagonal boron nitride particles were randomly selected from a scanning electron microscope observation image at a magnification of 5000 times, and the length of the major axis of each particle was measured. It is a calculated average value.
- the hexagonal boron nitride powder preferably has a specific surface area of 1.5 m 2 / g or more and 12.0 m 2 / g or less, and preferably 1.8 m 2 / g or more and 11.0 m 2 / g or less. More preferably, it is 2.0 m 2 / g or more and 10.0 m 2 / g or less. Further, the fact that the specific surface area of the hexagonal boron nitride powder is 1.5 m 2 / g or more indicates that there are many hexagonal boron nitride particles having a small particle size.
- the specific surface area of the hexagonal boron nitride powder is 12.0 m 2 / g or less, which means that the hexagonal boron nitride powder contains a small amount of fine powder and a large number of thick hexagonal boron nitride particles. Represents. If the content of the fine powder is small, an increase in the viscosity of the resin composition is suppressed when the hexagonal boron nitride powder is kneaded with the resin.
- the hexagonal boron nitride powder can be easily filled in the resin, and the handleability of the resin composition is improved.
- the specific surface area of the hexagonal boron nitride powder can be measured with a BET specific surface area meter.
- the hexagonal boron nitride powder produced by the production method of the present invention can be blended with a resin composition and used as a heat radiating filler.
- the resin used in the resin composition is not particularly limited, and may be, for example, a silicone-based resin or an epoxy-based resin.
- the epoxy resin include bisphenol A type epoxy resin, bisphenol S type epoxy resin, bisphenol F type epoxy resin, bisphenol A type hydrogenated epoxy resin, polypropylene glycol type epoxy resin, polytetramethylene glycol type epoxy resin, and naphthalene type.
- examples thereof include epoxy resin, phenylmethane type epoxy resin, tetrakisphenol methane type epoxy resin, biphenyl type epoxy resin, epoxy resin having a triazine nucleus as a skeleton, and bisphenol A alkylene oxide adduct type epoxy resin.
- epoxy resins may be used alone, or two or more thereof may be mixed and used.
- a curing agent an amine resin, an acid anhydride resin, a phenol resin, imidazoles and the like may be used. These curing agents may be used alone or in combination of two or more.
- the blending amount of these curing agents with respect to the epoxy resin is an equivalent ratio of 0.5 to 1.5 equivalents, preferably 0.7 to 1.3 equivalents with respect to the epoxy resin. In the present specification, these curing agents are also included in the resin.
- silicone-based resin a known curable silicone resin, which is a mixture of an addition reaction type silicone resin and a silicone-based cross-linking agent, can be used without limitation.
- addition reaction type silicone resin include polyorganosiloxane such as polydimethylsiloxane having an alkenyl group such as a vinyl group or a hexenyl group in the molecule as a functional group.
- silicone-based cross-linking agent examples include dimethylhydrogensiloxy group-terminated blocking dimethylsiloxane-methylhydrogensiloxane copolymer, trimethylsiloxy group-terminated blocking dimethylsiloxane-methylhydrogensiloxane copolymer, and trimethylsiloxane group-terminated blocking poly ( Examples thereof include polyorganosiloxane having a silicon atom-bonded hydrogen atom such as methylhydrogensiloxane) and poly (hydrogencil sesquioxane).
- the curing catalyst a known platinum-based catalyst or the like used for curing the silicone resin can be used without limitation.
- fine particle platinum fine particle platinum, fine particle platinum supported on carbon powder, chloroplatinic acid, alcohol-modified chloroplatinic acid, olefin complex of chloroplatinic acid, palladium, rhodium catalyst and the like can be mentioned.
- the blending ratio of the resin and the hexagonal boron nitride powder in the resin composition may be appropriately determined depending on the intended use.
- the above-mentioned hexagonal boron nitride powder is preferably 30 to 90% by volume in the total resin composition. , More preferably 40 to 80% by volume, still more preferably 50 to 70% by volume.
- the resin composition may contain components other than hexagonal boron nitride and the resin.
- the resin composition may replace a part of the hexagonal boron nitride powder with an inorganic filler.
- the inorganic filler include aluminum oxide, silicon oxide, zinc oxide, magnesium oxide, titanium oxide, silicon nitride, aluminum nitride, aluminum hydroxide, magnesium hydroxide, silicon carbide, calcium carbonate, barium sulfate, talc and the like.
- the resin composition may appropriately contain a curing accelerator, a discoloration inhibitor, a surfactant, a dispersant, a coupling agent, a colorant, a plasticizer, a viscosity modifier, an antibacterial agent and the like.
- resin sheets such as adhesive films and prepregs, circuit boards (laminated boards, multilayer printed wiring boards), solder resists, underfill materials, thermal adhesives, and dies.
- bonding materials semiconductor encapsulants, hole-filling resins, component-embedded resins, thermal interface materials (sheets, gels, greases, etc.), power module substrates, heat-dissipating members for electronic components, and the like.
- the hexagonal boron nitride powder produced by the production method of the present invention is particularly preferably blended in a resin sheet.
- the resin sheet is a sheet formed from the above-mentioned resin composition, and has a form in which hexagonal boron nitride tends to be oriented when formed into a sheet, and thermal conduction anisotropy is particularly likely to be a problem.
- the thickness of the resin sheet can be appropriately set according to the intended use, and may be, for example, 10 to 200 ⁇ m, 10 to 100 ⁇ m, or 10 to 50 ⁇ m.
- the present invention includes an organic compound containing a nitrogen atom and a boron source in which the molar ratio of the boron atom to the nitrogen atom is adjusted to 0.26 or more and 0.67 or less, and the lithium atom is 30 mol% or more.
- a method for producing a hexagonal boron nitride powder which comprises a heating step of heating the mixed powder at a maximum temperature of 1200 ° C. or higher and 1500 ° C. or lower.
- the alkali metal is preferably lithium and sodium or potassium. Further, in one embodiment of the present invention, the maximum temperature is 1200 ° C. or higher and 1350 ° C. or lower.
- ⁇ Measurement of particle size and aspect ratio of hexagonal boron nitride powder The particle size and aspect ratio of the hexagonal boron nitride powder were measured using FE-SEM (manufactured by Hitachi High-Technologies Corporation: S5500). 100 different hexagonal boron nitride particles were randomly selected from a scanning electron microscope observation image at a magnification of 5000 times, and the length and thickness of the major axis of the hexagonal boron nitride particles were measured and the aspect ratios (length of major axis / major axis /) were measured. The length of the thickness) was calculated, and the average value was used as the aspect ratio. The particle size was determined by calculating the average value of the measured major axis values.
- Example 1 By mixing 0.20 mol of boron oxide as a boron source, 0.20 mol of melamine as an organic compound containing nitrogen, 0.06 mol of lithium carbonate as a lithium salt, and 0.06 mol of sodium carbonate as an alkali metal salt other than lithium. A mixed powder was prepared. In the prepared mixed powder, B / N was 0.33, B / AM was 1.67, and the ratio of lithium in the alkali metal was 50 mol%.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- FIG. 1 shows a scanning electron microscope image taken at a magnification of 2000 times in (a), 5000 times in (b), and 10000 times in (c).
- a mixed powder was prepared by mixing 0.20 mol of borosand as an alkali metal salt other than the boron source and lithium, 0.40 mol of melamine as an organic compound containing nitrogen, and 0.26 mol of lithium carbonate as a lithium salt.
- B / N was 0.33
- B / AM was 0.87
- the ratio of lithium in the alkali metal was 58 mol%.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- FIG. 2 shows a scanning electron microscope image taken at a magnification of 2000 times in (a), 5000 times in (b), and 10000 times in (c).
- Example 3 Hexagonal boron nitride powder was produced in the same manner as in Example 2 except that the maximum temperature in the heating step was set to 1300 ° C., and the particle size, aspect ratio, and specific surface area were measured. Table 1 shows the manufacturing conditions and evaluation results.
- FIG. 3 shows a scanning electron microscope image taken at a magnification of 2000 times in (a), 5000 times in (b), and 10000 times in (c).
- Example 4 Mix 0.20 mol of boron oxide as a boron source, 0.06 mol of borosand as an alkali metal salt other than the boron source and lithium, 0.20 mol of melamine as an organic compound containing nitrogen, and 0.06 mol of lithium carbonate as a lithium salt. This produced a mixed powder.
- B / N was 0.53
- B / AM was 2.67
- the ratio of lithium in the alkali metal was 50 mol%.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- Table 1 shows the manufacturing conditions and evaluation results.
- Hexagonal boron nitride powder was produced in the same manner as in Example 1 except that potassium carbonate was used as an alkali metal salt other than lithium, and the particle size, aspect ratio, and specific surface area were measured. Table 1 shows the manufacturing conditions and evaluation results.
- Hexagonal boron nitride powder was produced in the same manner as in Example 1 except that 0.40 mol of boric acid was used as a boron source, and the particle size, aspect ratio, and specific surface area were measured. Table 1 shows the manufacturing conditions and evaluation results.
- a mixed powder was prepared by mixing 0.20 mol of boron oxide as a boron source, 0.20 mol of melamine as an organic compound containing nitrogen, and 0.12 mol of lithium carbonate as a lithium salt.
- B / N was 0.33
- B / AM was 1.67
- the ratio of lithium in the alkali metal was 100 mol%. This is an example in which B / AM is the same as in Examples 1 and 5 and does not contain an alkali metal other than lithium.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- FIG. 4 shows a scanning electron microscope image taken by magnifying 2000 times in (a), 5000 times in (b), and 10000 times in (c).
- a mixed powder was prepared by mixing 0.20 mol of boron oxide as a boron source, 0.20 mol of melamine as an organic compound containing nitrogen, and 0.23 mol of lithium carbonate as a lithium salt.
- B / N was 0.33
- B / AM was 0.87
- the ratio of lithium in the alkali metal was 100 mol%. This is an example in which the B / AM is the same as that of Example 2 and does not contain an alkali metal other than lithium.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- Table 1 shows the manufacturing conditions and evaluation results.
- Hexagonal boron nitride powder was produced in the same manner as in Reference Example 2 except that the maximum temperature in the heating step was set to 1300 ° C., and the particle size, aspect ratio, and specific surface area were measured.
- Table 1 shows the manufacturing conditions and evaluation results.
- a mixed powder was prepared by mixing 0.19 mol of boron oxide as a boron source, 0.12 mol of melamine as an organic compound containing nitrogen, and 0.07 mol of lithium carbonate as a lithium salt.
- B / N was 0.53
- B / AM was 2.71
- the ratio of lithium in the alkali metal was 100 mol%. This is an example in which the B / AM is almost the same as that of Example 4 and does not contain an alkali metal other than lithium.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- Table 1 shows the manufacturing conditions and evaluation results.
- Hexagonal boron nitride powder was produced in the same manner as in Reference Example 1 except that 0.40 mol of boric acid was used as a boron source, and the particle size, aspect ratio, and specific surface area were measured.
- a mixed powder was prepared by mixing 0.20 mol of boron oxide as a boron source, 0.20 mol of melamine as an organic compound containing nitrogen, and 0.06 mol of lithium carbonate as a lithium salt.
- B / N was 0.33
- B / AM was 3.33
- the ratio of lithium in the alkali metal was 100 mol%.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- FIG. 5 shows a scanning electron microscope image taken at a magnification of 2000 times in (a), 5000 times in (b), and 10000 times in (c).
- a mixed powder was prepared by mixing 0.20 mol of boron oxide as a boron source, 0.20 mol of melamine as an organic compound containing nitrogen, and 0.12 mol of sodium carbonate as an alkali metal salt other than lithium.
- B / N was 0.33 and B / AM was 1.67. This is an example in which B / AM is the same as in Examples 1 and 5 and does not contain lithium.
- Hexagonal boron nitride powder was prepared by heating the prepared mixed powder in a batch type firing furnace at a maximum temperature of 1400 ° C. for 1 hour in a nitrogen atmosphere in a heating step.
- the prepared hexagonal boron nitride powder was acid-washed with a 5% aqueous hydrochloric acid solution, filtered, washed with water, and dried.
- FIG. 6 shows a scanning electron microscope image taken at a magnification of 2000 times in (a), 5000 times in (b), and 10000 times in (c).
- Examples 1 to 6 thick hexagonal boron nitride powder having an aspect ratio in the range of 1.0 to 5.0 could be obtained.
- a hexagonal boron nitride powder having the same aspect ratio was obtained while reducing the amount of lithium salt used. The same can be said from the comparison between Example 2 and Reference Example 2, Example 3 and Reference Example 3, Example 4 and Reference Example 4, and Example 6 and Reference Example 5.
- Reference Example 6 in which the amount of lithium with respect to the boron atom in the mixed powder was the same as in Examples 1 and 5 but no alkali metal other than lithium was used, and only alkali metal other than lithium was used without using lithium.
- a thick hexagonal boron nitride powder could not be obtained.
- the mixed powder as a raw material contains a boron source and an organic compound containing nitrogen, and has an alkali metal atom present, and the alkali metal has a lithium content of 30 mol% or more and less than 100 mol%. It was shown that a thick hexagonal boron nitride powder can be produced even with a small amount of lithium as in the case of a large amount of lithium.
- the hexagonal boron nitride powder obtained in Example 3 in which the maximum temperature in the heating step is in the range of 1200 ° C. to 1350 ° C. is found in the heating step.
- Hexagonal boron nitride powder having a smaller particle size than the hexagonal boron nitride powder obtained in Example 2 having a maximum temperature exceeding 1350 ° C. could be obtained.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Ceramic Products (AREA)
Abstract
Description
本発明の混合粉末は、窒素原子を含む有機化合物と、上記窒素原子に対するホウ素原子のモル比が0.26以上、0.67以下に調整されたホウ素源とを含み、且つ、リチウム原子が30モル%~100モル%未満の範囲に調整されたアルカリ金属を、前記アルカリ金属原子に対するホウ素原子のモル比が、0.75以上、3.35以下となるように存在せしめた混合粉末である。
本発明の加熱工程では、混合粉末を最高温度1200℃以上、1500℃以下で加熱する。1200℃以上の温度で混合粉末を加熱することにより、得られる六方晶窒化ホウ素粒子のアスペクト比が大きくなることを抑制できる。最高温度は、1250℃以上であることがより好ましい。また、1500℃以下の温度で混合粉末を加熱することにより、アルカリ金属の過剰な揮発を防ぐことができるとともに、六方晶窒化ホウ素粒子のアスペクト比が大きくなることを抑制できる。最高温度は1450℃以下であることがより好ましい。
本発明の六方晶窒化ホウ素粉末の製造方法では、混合粉末を準備する工程、加熱工程以外の工程を含んでよい。このような工程を本明細書において「その他の工程」と称する。六方晶窒化ホウ素粉末の製造方法に含まれるその他の工程としては、例えば、酸洗浄工程、水洗浄工程、乾燥工程、および分級工程が挙げられる。
本発明の製造方法により得られる六方晶窒化ホウ素粉末は、アスペクト比が1.0以上、5.0以下である。アスペクト比がこの範囲にあることは肉厚な六方晶窒化ホウ素粒子を含む六方晶窒化ホウ素粉末であり、熱伝導異方性を小さくすることが可能であることを意味する。なお、本明細書において、六方晶窒化ホウ素粒子は、六方晶窒化ホウ素の単粒子を意味する。上述のように六方晶窒化ホウ素粒子は通常板状粒子であり、本明細書では、この板状粒子の板面において最大となる径を長径とし、この板面に垂直な長さを厚さと称する。そして、この長径を厚さで除した値をアスペクト比と称する。六方晶窒化ホウ素粉末のアスペクト比は、倍率5000倍の走査電子顕微鏡観察像から異なる六方晶窒化ホウ素粒子100個を無作為に選び、各一次粒子の長径の長さ、厚みを測定して得られた各粒子のアスペクト比の平均値である。
本発明の製造方法によって製造された六方晶窒化ホウ素粉末は、樹脂組成物に配合して放熱フィラーとして使用することができる。
本発明は、窒素原子を含む有機化合物と、上記窒素原子に対するホウ素原子のモル比が0.26以上、0.67以下に調整されたホウ素源とを含み、且つ、リチウム原子が30モル%以上、100モル%未満の範囲に調整されたアルカリ金属を、前記アルカリ金属原子に対するホウ素原子のモル比が、0.75以上、3.35以下となるように存在せしめた混合粉末を準備する工程、上記混合粉末を最高温度1200℃以上、1500℃以下で加熱する加熱工程を含む、ことを特徴とする六方晶窒化ホウ素粉末の製造方法である。
六方晶窒化ホウ素粉末の粒径およびアスペクト比はFE-SEM(日立ハイテクノロジーズ株式会社製:S5500)を用いて測定した。倍率5000倍の走査電子顕微鏡観察像から異なる六方晶窒化ホウ素粒子100個を無作為に選び、六方晶窒化ホウ素粒子の長径の長さ、厚みを測定してそれぞれのアスペクト比(長径の長さ/厚みの長さ)を算出し、その平均値をアスペクト比とした。また、粒径は、測定された長径の値の平均値を算出して求めた。
六方晶窒化ホウ素粉末の比表面積は、BET比表面積計(マウンテック社製:Macsorb HM model-1201)を使用して測定した。
ホウ素源として酸化ホウ素0.20モル、窒素を含む有機化合物としてメラミン0.20モル、リチウム塩として炭酸リチウム0.06モル、リチウム以外のアルカリ金属塩として炭酸ナトリウム0.06モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは0.33、B/AMは1.67、アルカリ金属におけるリチウムの割合は50モル%であった。
ホウ素源兼リチウム以外のアルカリ金属塩として硼砂0.20モル、窒素を含む有機化合物としてメラミン0.40モル、リチウム塩として炭酸リチウム0.26モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは0.33、B/AMは0.87、アルカリ金属におけるリチウムの割合は58モル%であった。
加熱工程における最高温度を1300℃とした以外は、実施例2と同様に六方晶窒化ホウ素粉末を製造し、粒径、アスペクト比、比表面積の測定を行った。製造条件および評価結果を表1に示す。図3には、走査型電子顕微鏡画像として、(a)は2000倍、(b)は5000倍、(c)は10000倍に拡大して撮影した図を示す。
ホウ素源として酸化ホウ素0.20モル、ホウ素源兼リチウム以外のアルカリ金属塩として硼砂0.06モル、窒素を含む有機化合物としてメラミン0.20モル、リチウム塩として炭酸リチウム0.06モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは0.53、B/AMは2.67、アルカリ金属におけるリチウムの割合は50モル%であった。
リチウム以外のアルカリ金属塩として炭酸カリウムを使用した以外は実施例1と同様に六方晶窒化ホウ素粉末を製造し、粒径、アスペクト比、比表面積の測定を行った。製造条件および評価結果を表1に示す。
ホウ素源としてホウ酸0.40モルを使用した以外は実施例1と同様に六方晶窒化ホウ素粉末を製造し、粒径、アスペクト比、比表面積の測定を行った。製造条件および評価結果を表1に示す。
ホウ素源として酸化ホウ素0.20モル、窒素を含む有機化合物としてメラミン0.20モル、リチウム塩として炭酸リチウム0.12モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは0.33、B/AMは1.67、アルカリ金属におけるリチウムの割合は100モル%であった。これは、実施例1および5と、B/AMが同一で、且つリチウム以外のアルカリ金属を含まない例である。
ホウ素源として酸化ホウ素0.20モル、窒素を含む有機化合物としてメラミン0.20モル、リチウム塩として炭酸リチウム0.23モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは0.33、B/AMは0.87、アルカリ金属におけるリチウムの割合は100モル%であった。これは、実施例2と、B/AMが同一で、且つリチウム以外のアルカリ金属を含まない例である。
加熱工程における最高温度を1300℃とした以外は、参考例2と同様に六方晶窒化ホウ素粉末を製造し、粒径、アスペクト比、比表面積の測定を行った。これは、実施例3と、B/AMが同一で、且つリチウム以外のアルカリ金属を含まない例である。製造条件および評価結果を表1に示す。
ホウ素源として酸化ホウ素0.19モル、窒素を含む有機化合物としてメラミン0.12モル、リチウム塩として炭酸リチウム0.07モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは0.53、B/AMは2.71、アルカリ金属におけるリチウムの割合は100モル%であった。これは、実施例4と、B/AMがほぼ同一で、且つリチウム以外のアルカリ金属を含まない例である。
ホウ素源としてホウ酸0.40モルを使用した以外は参考例1と同様に六方晶窒化ホウ素粉末を製造し、粒径、アスペクト比、比表面積の測定を行った。これは、実施例6と、B/AMが同一で、且つリチウム以外のアルカリ金属を含まない例である。製造条件および評価結果を表1に示す。
ホウ素源として酸化ホウ素0.20モル、窒素を含む有機化合物としてメラミン0.20モル、リチウム塩として炭酸リチウム0.06モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは0.33、B/AMは3.33、アルカリ金属におけるリチウムの割合は100モル%であった。これは、実施例1および5と、ホウ素に対するリチウム量が同一で、且つリチウム以外のアルカリ金属を含まない例であり、参考例1からリチウム使用量を単に減少させた製造方法に相当する。
ホウ素源として酸化ホウ素0.20モル、窒素を含む有機化合物としてメラミン0.20モル、リチウム以外のアルカリ金属塩として炭酸ナトリウム0.12モルを混合することによって混合粉末を作製した。作製した混合粉末において、B/Nは、0.33、B/AMは1.67であった。これは、実施例1および5とB/AMが同一で、且つリチウムを含まない例である。
Claims (3)
- 窒素原子を含む有機化合物と、上記窒素原子に対するホウ素原子のモル比が0.26以上、0.67以下に調整されたホウ素源とを含み、且つ、リチウム原子が30モル%以上、100モル%未満の範囲に調整されたアルカリ金属を、前記アルカリ金属に含まれるアルカリ金属原子に対するホウ素原子のモル比が、0.75以上、3.35以下となるように存在せしめた混合粉末を準備する工程、上記混合粉末を最高温度1200℃以上、1500℃以下で加熱する加熱工程を含む、ことを特徴とする六方晶窒化ホウ素粉末の製造方法。
- 前記アルカリ金属は、リチウムと、ナトリウムまたはカリウムである、請求項1に記載の六方晶窒化ホウ素粉末の製造方法。
- 前記最高温度が、1200℃以上1350℃以下である、請求項1に記載の六方晶窒化ホウ素粉末の製造方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP21776413.3A EP4129898A4 (en) | 2020-03-27 | 2021-03-10 | METHOD FOR PRODUCING HEXAGONAL BORON NITRIDE POWDER |
KR1020227026588A KR20220158681A (ko) | 2020-03-27 | 2021-03-10 | 육방정 질화붕소 분말의 제조 방법 |
CA3167241A CA3167241A1 (en) | 2020-03-27 | 2021-03-10 | Method for producing hexagonal boron nitride powder |
US17/910,984 US20230134671A1 (en) | 2020-03-27 | 2021-03-10 | Method for producing hexagonal boron nitride powder |
CN202180012180.3A CN115038664B (zh) | 2020-03-27 | 2021-03-10 | 六方晶氮化硼粉末的制造方法 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2020-057912 | 2020-03-27 | ||
JP2020057912A JP6993455B2 (ja) | 2020-03-27 | 2020-03-27 | 六方晶窒化ホウ素粉末の製造方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2021193046A1 true WO2021193046A1 (ja) | 2021-09-30 |
Family
ID=77891491
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2021/009425 WO2021193046A1 (ja) | 2020-03-27 | 2021-03-10 | 六方晶窒化ホウ素粉末の製造方法 |
Country Status (8)
Country | Link |
---|---|
US (1) | US20230134671A1 (ja) |
EP (1) | EP4129898A4 (ja) |
JP (1) | JP6993455B2 (ja) |
KR (1) | KR20220158681A (ja) |
CN (1) | CN115038664B (ja) |
CA (1) | CA3167241A1 (ja) |
TW (1) | TW202142484A (ja) |
WO (1) | WO2021193046A1 (ja) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2023150526A (ja) * | 2022-03-31 | 2023-10-16 | 株式会社トクヤマ | 表面処理窒化ホウ素、表面処理窒化ホウ素の製造方法、樹脂組成物、放熱基板 |
CN115925428B (zh) * | 2023-01-06 | 2023-10-27 | 灵石鸿润和新材料有限公司 | 一种六方氮化硼粉体及其制备方法和应用 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1998005590A1 (fr) * | 1996-08-06 | 1998-02-12 | Otsuka Kagaku Kabushiki Kaisha | Nitrure de bore et son procede de preparation |
JP2016141600A (ja) | 2015-02-02 | 2016-08-08 | 三菱化学株式会社 | 六方晶窒化ホウ素単結晶およびその製造方法、該六方晶窒化ホウ素単結晶を配合した複合材組成物並びに該複合材組成物を成形してなる放熱部材 |
JP2018104253A (ja) * | 2016-12-28 | 2018-07-05 | デンカ株式会社 | 六方晶窒化ホウ素一次粒子凝集体及びその用途 |
JP2018108933A (ja) * | 2018-03-20 | 2018-07-12 | 株式会社トクヤマ | 窒化硼素粉末及びその製造方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0647446B2 (ja) * | 1985-09-09 | 1994-06-22 | 昭和電工株式会社 | 窒化ホウ素の製造法 |
-
2020
- 2020-03-27 JP JP2020057912A patent/JP6993455B2/ja active Active
-
2021
- 2021-03-10 WO PCT/JP2021/009425 patent/WO2021193046A1/ja active Application Filing
- 2021-03-10 CN CN202180012180.3A patent/CN115038664B/zh active Active
- 2021-03-10 CA CA3167241A patent/CA3167241A1/en active Pending
- 2021-03-10 US US17/910,984 patent/US20230134671A1/en active Pending
- 2021-03-10 KR KR1020227026588A patent/KR20220158681A/ko unknown
- 2021-03-10 EP EP21776413.3A patent/EP4129898A4/en active Pending
- 2021-03-11 TW TW110108726A patent/TW202142484A/zh unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1998005590A1 (fr) * | 1996-08-06 | 1998-02-12 | Otsuka Kagaku Kabushiki Kaisha | Nitrure de bore et son procede de preparation |
JP2016141600A (ja) | 2015-02-02 | 2016-08-08 | 三菱化学株式会社 | 六方晶窒化ホウ素単結晶およびその製造方法、該六方晶窒化ホウ素単結晶を配合した複合材組成物並びに該複合材組成物を成形してなる放熱部材 |
JP2018104253A (ja) * | 2016-12-28 | 2018-07-05 | デンカ株式会社 | 六方晶窒化ホウ素一次粒子凝集体及びその用途 |
JP2018108933A (ja) * | 2018-03-20 | 2018-07-12 | 株式会社トクヤマ | 窒化硼素粉末及びその製造方法 |
Non-Patent Citations (1)
Title |
---|
See also references of EP4129898A4 |
Also Published As
Publication number | Publication date |
---|---|
JP2021155279A (ja) | 2021-10-07 |
EP4129898A1 (en) | 2023-02-08 |
EP4129898A4 (en) | 2024-04-17 |
JP6993455B2 (ja) | 2022-01-13 |
CA3167241A1 (en) | 2021-09-30 |
KR20220158681A (ko) | 2022-12-01 |
CN115038664A (zh) | 2022-09-09 |
TW202142484A (zh) | 2021-11-16 |
CN115038664B (zh) | 2024-07-09 |
US20230134671A1 (en) | 2023-05-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP7455047B2 (ja) | 窒化ホウ素凝集粒子、窒化ホウ素凝集粒子の製造方法、該窒化ホウ素凝集粒子含有樹脂組成物、及び成形体 | |
WO2020179662A1 (ja) | 六方晶窒化ホウ素粉末、樹脂組成物、樹脂シートおよび六方晶窒化ホウ素粉末の製造方法 | |
WO2021193046A1 (ja) | 六方晶窒化ホウ素粉末の製造方法 | |
Li et al. | Synthesis of a multinary nitride, Eu-doped CaAlSiN3, from alloy at low temperatures | |
KR20160078340A (ko) | 수지 조성물, 방열 재료 및 방열 부재 | |
TW201722848A (zh) | 六方晶體氮化硼粉末、其製造方法、樹脂組成物及樹脂薄片 | |
JP5558885B2 (ja) | 樹脂複合組成物及びその用途 | |
JP6950148B2 (ja) | 窒化アルミニウム−窒化ホウ素複合凝集粒子およびその製造方法 | |
KR20150114468A (ko) | 질화알루미늄 분말 | |
JP2019019222A (ja) | 球状シリカフィラー用粉末及びその製造方法 | |
JPWO2017126608A1 (ja) | 熱伝導性フィラー組成物、その利用および製法 | |
JP6222840B2 (ja) | 高熱伝導性無機フィラー複合粒子及びその製造方法 | |
JP6519876B2 (ja) | 六方晶窒化ホウ素の製造方法、及び放熱シートの製造方法 | |
JP2013147403A (ja) | 金属化合物含有窒化ホウ素、及びそれを含有する複合材組成物 | |
JP7152003B2 (ja) | 高熱伝導性無機フィラー複合粒子及びその製造方法 | |
JP2022109032A (ja) | 六方晶窒化ホウ素粉末 | |
WO2018194117A1 (ja) | スピネル粒子の製造方法、樹脂組成物の製造方法および成形物の製造方法 | |
TW202243990A (zh) | 六方晶氮化硼粉末及其製造方法 | |
JP2017066017A (ja) | 窒化ケイ素粉末の製造方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 21776413 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 3167241 Country of ref document: CA |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2021776413 Country of ref document: EP |
|
ENP | Entry into the national phase |
Ref document number: 2021776413 Country of ref document: EP Effective date: 20221027 |
|
NENP | Non-entry into the national phase |
Ref country code: DE |