TWI542542B - 碳化矽粉末及其製造方法 - Google Patents
碳化矽粉末及其製造方法 Download PDFInfo
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- TWI542542B TWI542542B TW101130654A TW101130654A TWI542542B TW I542542 B TWI542542 B TW I542542B TW 101130654 A TW101130654 A TW 101130654A TW 101130654 A TW101130654 A TW 101130654A TW I542542 B TWI542542 B TW I542542B
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- Prior art keywords
- raw material
- carbide powder
- niobium carbide
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- 238000004519 manufacturing process Methods 0.000 title claims description 40
- 238000000034 method Methods 0.000 title description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title 1
- 239000002994 raw material Substances 0.000 claims description 79
- 239000000843 powder Substances 0.000 claims description 61
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 59
- 239000012535 impurity Substances 0.000 claims description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 24
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 19
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 239000003575 carbonaceous material Substances 0.000 claims description 10
- 239000006229 carbon black Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052715 tantalum Inorganic materials 0.000 claims description 7
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 5
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 5
- 238000004804 winding Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 9
- 229910052796 boron Inorganic materials 0.000 description 8
- 239000010936 titanium Substances 0.000 description 8
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 7
- 229910052684 Cerium Inorganic materials 0.000 description 7
- 239000001263 FEMA 3042 Substances 0.000 description 7
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 7
- 229940033123 tannic acid Drugs 0.000 description 7
- 235000015523 tannic acid Nutrition 0.000 description 7
- 229920002258 tannic acid Polymers 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000011575 calcium Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 5
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- 239000011163 secondary particle Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000011164 primary particle Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- WXANAQMHYPHTGY-UHFFFAOYSA-N cerium;ethyne Chemical compound [Ce].[C-]#[C] WXANAQMHYPHTGY-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000002006 petroleum coke Substances 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000010455 vermiculite Substances 0.000 description 3
- 229910052902 vermiculite Inorganic materials 0.000 description 3
- 235000019354 vermiculite Nutrition 0.000 description 3
- GYSCBCSGKXNZRH-UHFFFAOYSA-N 1-benzothiophene-2-carboxamide Chemical compound C1=CC=C2SC(C(=O)N)=CC2=C1 GYSCBCSGKXNZRH-UHFFFAOYSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N Decanoic acid Natural products CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-PWCQTSIFSA-N Tritiated water Chemical compound [3H]O[3H] XLYOFNOQVPJJNP-PWCQTSIFSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000011304 carbon pitch Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011874 heated mixture Substances 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B35/515—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
- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
- C04B35/573—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 carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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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
- C04B35/626—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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/424—Carbon black
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
- C04B2235/727—Phosphorus or phosphorus compound content
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Structural Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Description
本發明係關於使用艾其遜(Acheson)爐獲得之高純度碳化矽粉末、及其製造方法。
碳化矽(SiC)係作為研磨或研削材、陶瓷燒結體及導電性材料等之工業用材料，自過去以來即被廣泛使用。尤其，最近，由於省能源趨勢增強或因非核能(nuclear power free)而對自然再生能源之活用之期待等社會背景，而要求純度高之碳化矽粉末作為功率半導體等所使用之單結晶材料。
工業上量產碳化矽之技術已知有藉由以含矽(Si)之矽酸質原料(例如矽砂)與含碳之碳質原料(例如石油焦炭)作為原料，在艾其遜爐中於1600℃以上加熱，利用直接還原反應製造碳化矽之方法。
過去以來進行之由艾其遜爐之製造，由於原料中之雜質含有率高，雜質之控制困難，故無法製造高純度之碳化矽粉末。
因此，提案有使純度低之碳化矽粉末高純度化之方法。例如，專利文獻1中記載將含較多雜質之碳化矽粉末置於真空容器中，使真空度在9×10-5~1×10-2托耳(torr)之範圍，且在1,500~1,700℃之溫度範圍內加熱，而去除碳化矽粉末中之雜質，製造高純度碳化矽粉末之方法。
然而，在真空中升溫之專利文獻1的方法之裝置複雜、昂貴，且工業上無法一次大量生產。
另外，在專利文獻2記載將含較多雜質之碳化矽粉與氫氟酸之混合物導入於密閉容器中，在加壓下加熱處理之高純度碳化矽粉之製造方法。
然而，氫氟酸對人體有害且危險性高，在操作上困難，且會有工業上無法大量處理碳化矽粉之問題。
[專利文獻1]特開昭64-61308號公報
[專利文獻2]專利第4006716號公報
本發明之目的係提供一種高純度之碳化矽粉末，及可便宜且大量而且安全地製造高純度碳化矽粉末之方法。
本發明人等為解決上述課題而積極檢討之結果，發現使用艾其遜爐，燒成使矽酸質原料與碳質原料混合而成之碳化矽製造用原料所獲得之特定碳化矽粉末，以及藉由該製造方法，可達成上述目的，因而完成本發明。
亦即，本發明為提供以下之[1]~[6]者。
[1]一種碳化矽粉末，其係使用艾其遜爐使混合矽酸質原料與碳質原料而成之碳化矽製造用原料燒成所獲得之碳化矽粉末，其特徵為前述碳化矽粉末中之雜質含有率為500ppm以下。
[2]一種碳化矽粉末之製造方法，其為製造前述[1]所記載之碳化矽粉末之方法，該方法係使用碳質原料與矽酸質原料之混合莫耳比(C/SiO2)為2.5~4.0，且雜質含有率為120ppm以下者作為前述碳化矽製造用原料。
[3]如前述[2]所記載之碳化矽粉末之製造方法，其中在作為艾其遜爐加熱手段之由碳所組成的發熱體中，其雜質含有率為前述碳化矽製造用原料中之雜質含有率以下。
[4]如前述[2]或[3]所記載之碳化矽粉末之製造方法，其中前述矽酸質原料係雜質含有率為50ppm以下之非晶質二氧化矽。
[5]如前述[2]~[4]中任一項所記載之碳化矽粉末之製造方法，其中前述碳質原料係雜質含有率為300ppm以下之碳黑。
[6]如前述[2]~[5]中任一項所記載之碳化矽粉末之製造方法，其中前述碳化矽製造用原料經預先顆粒化。
本發明之碳化矽粉末為高純度且便宜，除可使用作為功率半導體方面之單結晶用原料及治具以外，亦可使用作
為要求高純度之用途之陶瓷燒結體之原料。
依據本發明之製造方法，可便宜且大量而且安全地製造高純度之碳化矽粉末。
以下針對本發明詳細說明。
本發明之碳化矽粉末為使用艾其遜爐，燒成使矽酸質原料與碳質原料混合而成之碳化矽製造用原料所獲得之碳化矽粉末，該碳化矽粉末中之雜質之含有率為500ppm以下，較好為300ppm以下，更好為200ppm以下，又更好為150ppm以下，再更好為100ppm以下，最好為50ppm以下者。該含有率超過500ppm時，難以使用作為功率半導體方面之單結晶用原料及治具、以及要求高純度之用途之陶瓷燒結體之原料。
此處，所謂碳化矽粉末中之雜質意指除矽(Si)、碳(C)、氧(O)及氮(N)以外之成分。矽(Si)及碳(C)為碳化矽本身之成分，不包含在雜質中。氧(O)及氮(N)亦不包含在雜質中。
雜質之例列舉為硼(B)、磷(P)、鋁(Al)、鐵(Fe)、鈦(Ti)、鎳(Ni)、銅(Cu)、鈣(Ca)、鋅(Zn)等。
尤其，使用本發明之碳化矽粉末作為功率半導體之單結晶用原料時，碳化矽粉末中之硼(B)及磷(P)之各別的含有率較好為1ppm以下。又，該情況下，碳化矽粉
末中之鋁(Al)、鐵(Fe)及鈦(Ti)之各別的含有率較好為100ppm以下，更好為5ppm以下，最好為2ppm以下。
本發明之製造方法中使用之碳化矽製造用原料為碳質原料與矽酸質原料之混合莫耳比(C/SiO2)為2.5~4.0，且雜質含有率為120ppm以下者。
本說明書中，所謂「碳質原料與矽酸質原料之混合莫耳比」係指混合碳質原料與矽酸質原料，調製碳化矽製造用原料時之碳質原料中之碳(C)之莫耳與矽酸質原料中之矽酸(SiO2)之莫耳比(C/SiO2)。
碳質原料與矽酸質原料之混合莫耳比之範圍為2.5~4.0，較好為2.8~3.8，更好為3.0~3.6。該混合莫耳比未達2.5時或超過4.0時，製品之碳化矽粉末中會殘留較多未反應之矽酸質原料或碳質原料。因此，該混合莫耳比對碳化矽粉末之組成造成影響。
碳化矽製造用原料中之雜質含有率為120ppm以下，較好為100ppm以下，更好為70ppm以下，又更好為50ppm以下，再更好為40ppm以下，最好為20ppm以下。該含有率超過120ppm時，難以滿足與製造之碳化矽粉末有關之可使用作為半導體用單結晶原料之純度。
此處，所謂碳化矽製造用原料中之雜質係與上述之碳化矽粉末中之雜質相同，意指除矽(Si)、碳(C)、氧(O)及氮(N)以外之成分。
又，碳化矽製造用原料中之氧(O)在碳化矽粉末之
製造過程中幾乎被去除。
本發明之碳化矽製造用原料可使用使矽酸質原料與碳質原料經粉體混合獲得之混合原料預先顆粒化而成者。顆粒化之碳化矽製造用原料可藉由例如使二氧化矽與有機樹脂之混合物顆粒化而獲得者。
顆粒之粒度(最長尺寸；例如剖面為橢圓時為長徑之尺寸)，就操作容易性、燒成效率等觀點而言，較好為0.3~10 mm，更好為0.5~5mm，最好為1~4mm。
本發明之製造法中使用之矽酸質原料列舉為例如天然矽砂及矽石粉，人造矽石粉、發煙二氧化矽、非晶質二氧化矽等。該等可單獨使用一種或組合兩種以上使用。另外。就反應性之觀點而言以非晶質二氧化矽較佳。
矽酸質原料中之雜質之含有率較好為50ppm以下，更好為25ppm以下。該含有率超過50ppm時，會有所製造之碳化矽粉末之純度變低之情況。
此處，所謂矽酸質原料中之雜質係與上述之碳化矽粉末中之雜質相同，意指除矽(Si)、碳(C)、氧(O)及氮(N)以外之成分。
另外，矽酸質原料中之B、P、Al、Fe、Ca、及Ti之各別之含有率較好為20ppm以下，更好為10ppm以下，又更好為5ppm以下，最好為1ppm以下。
矽酸質原料之粒度較好為10mm以下，更好為8mm以下，最好為6mm以下。該粒度超過10mm時，反應性顯著變差，成為生產性差之結果。
矽酸質原料之粒度之定義係與上述顆粒之粒度(最長尺寸)相同。
本發明之製造方法中使用之碳質原料可列舉為例如石油焦炭、石碳瀝青、碳黑、各種有機樹脂等。該等可單獨使用一種或組合兩種以上使用。其中，就純度之觀點而言，以碳黑較佳。
碳質原料中之雜質之含有率較好為300ppm以下，更好為200ppm以下，又更好為100ppm以下，最好為70ppm以下。該含有率超過300ppm時，會有所得碳化矽粉末之純度變低之情況。
此處，所謂碳質原料中之雜質係與上述之碳化矽粉末中之雜質相同，意指除矽(Si)、碳(C)、氧(O)及氮(N)以外之成分。
本發明之製造方法中使用之艾其遜爐之發熱體之種類為由碳所成者，只要可通電即可，並無特別限制，可列舉為例如石墨粉、碳棒。
發熱體中之雜質之含有率係上述碳化矽製造用原料中所含雜質之含有率以下為較好。
此處，所謂發熱體中之雜質係與上述之碳化矽粉末中之雜質相同，意指除矽(Si)、碳(C)、氧(O)及氮(N)以外之成分。
發熱體中之雜質之含有率較好為120ppm以下，更好為70ppm以下，又更好為50ppm以下，最好為25ppm以下。該含有率定在較佳範圍內時，可獲得更高純度之碳化
矽粉末。
發熱體之形態如上述只要可通電即可，可為粉狀亦可為棒狀。另外，棒狀之情況，該棒狀體之形態亦無特別限制，可為圓柱狀亦可為角柱狀。
針對本發明中使用之艾其遜爐，邊參照圖1及圖2邊加以說明。
圖1為艾其遜爐4之長度方向之剖面圖，圖2為與艾其遜爐4之長度方向垂直之方向之剖面圖。
艾其遜爐4為大氣開放型，為爐本體5之剖面成略U字狀之爐，且兩端具有電極蕊3、3。於長度方向之中央部以連結電極蕊3、3設置發熱體2，發熱體2之周圍填充碳化矽製造用原料1。且，碳化矽製造用原料1在爐本體5之內部空間中收容為半圓柱體狀。
電流流入電極蕊3、3之間，藉由使發熱體2通電加熱，而在發熱體2之周圍引起以下述式(1)所示之直接還原反應，生成碳化矽(SiC)之塊狀物。
SiO2+3C → SiC+2CO (1)
進行上述反應之溫度為1600~3000℃。
藉由粉碎所得之碳化矽塊狀物，可獲得高純度之碳化矽粉末。
粉碎手段可列舉為球磨機、震動粉碎機、噴射粉碎機等之一般之粉碎手段。
所得高純度之碳化矽粉末可依據成為目標之純度，以無機酸進行洗淨。無機酸可使用鹽酸、硫酸、硝酸等。
以下以實施例具體說明本發明，但本發明並不限於該等實施例。
使用以下所示之材料。
(1)矽酸質原料A；結晶質二氧化矽(共立材料(股)製造，純化矽石粉，粒度：2mm以下)
(2)矽酸質原料B；非晶質二氧化矽(太平洋水泥(股)製造，試製品，粒度：5mm以下)
(3)矽酸質原料C；結晶質二氧化矽(豪州產，天然矽石粉，粒度：2mm以下)
(4)碳質原料A；碳黑(日本Cabot(股)製造，商品名「SHOW BLACK 550」，一次粒子之平均粒徑：50nm，二次粒子之平均粒徑：724μm)
(5)碳質原料B：碳黑(東海Carbon(股)製造，商品名「SEAST 600」，一次粒子之平均粒徑：25nm，二次粒子之平均粒徑：500μm)
(6)碳質原料C：碳黑(東海Carbon(股)製造，商品名「SEAST TA」，一次粒子之平均粒徑：120nm，二次粒子之平均粒徑：900μm)
(7)碳質原料D：碳黑(AIR WATER(股)製造，商品名「BELLFINE」，一次粒子之平均粒徑：20nm，二
次粒子之平均粒徑：243μm)
(8)碳質原料E；石油焦碳(中國產)，二次粒子之平均粒徑：3000μm)
(9)發熱體之原料；發熱體用石墨粉(太平洋水泥
(股)製造之試製品)
(10)結合劑：聚乙烯醇(關東化學(股)特級)使用上述材料調製以下之材料。
(11)發熱體用石墨A；使上述發熱體用石墨粉在非氧化性環境下，以2,000℃之條件重複燒成兩次獲得。
(12)發熱體用石墨B；使上述發熱體用石墨粉在非氧化性環境下，以2,000℃之條件重複燒成四次獲得。
(13)發熱體用石墨C；使上述發熱體用石墨粉在非氧化性環境下，以2,000℃之條件重複燒成六次獲得。
(14)顆粒狀之混合原料A；混合矽酸質原料B 47質量份和碳質原料C 52質量份後，對該粉體混合原料100質量份添加30質量份之聚乙烯醇(20%)水溶液，製成顆粒狀(粒度：4mm)。
(15)顆粒狀之混合原料B；混合矽酸質原料B 62.5質量份和碳質原料D 37.5質量份後，與前述方法同樣，添加聚乙烯醇，且以造粒機製成顆粒狀(粒度：2mm)。
如下列分析上述材料之化學成分。結果示於表1。
(1)B(硼)及P(磷)之含有率之分析方法
依據土壤中之B(硼)之分析方法(參照BUNSEKI KAGAKU VOL47，No7，pp451~454)之利用鹼熔融法之ICP-AES分析進行分析。
具體而言，將試料1g及Na2CO3 4g置於白金坩堝中之後，將該白金坩堝載置於電爐中且在700℃加熱1小時。接著每隔1小時，邊攪拌白金坩堝內之混合物，邊在800℃加熱4小時，進而在1000℃加熱15分鐘。於加熱後之混合物(熔成物)中添加50質量%之HCl 120ml，使用加熱板，在140℃邊粉碎熔融物10分鐘邊溶解。加水補足至100ml後進行過濾。對所得固體成分進行ICP-AES分析。所得結果示於表1。
依據「JIS R 1616」所記載之加壓酸分解法之ICP-AES分析測定。所得結果示於表1。
又，關於表1中之各原料，前述6種原料(B、P、Al、Fe、Ca、Ti)以外之雜質含有率之合計為10ppm以下。
於圖1及圖2所記載之艾其遜爐中收容表2所記載之混合原料、及發熱體用石墨後，以最大負荷70kwh通電加熱12小時，生成碳化矽之塊狀物。使用桌上型磨床(Top Grinder)粉碎所得碳化矽之塊狀物，獲得碳化矽粉末。使用上述分析方法測定所得碳化矽粉末中之雜質(B、P、Al、Fe、Ca、及Ti)之含有率。結果示於表3。
關於表2中之「混合原料」及「發熱體」，「雜質之含有率」均為表1中所記載之六種雜質之合計量。
且，關於表3中之實施例1~8之任一者，表3中所記載之六種雜質以外之雜質之合計量亦均為10ppm以下。
又，艾其遜爐加熱時之爐內溫度係在1600~3000℃之範圍內。
1‧‧‧矽酸質原料與碳質原料之混合物(碳化矽製造用原料)
2‧‧‧發熱體用石墨
3‧‧‧電極蕊
4‧‧‧艾其遜爐
5‧‧‧爐本體
圖1為艾其遜爐之長度方向之剖面圖。
圖2為與艾其遜爐之長度方向垂直之方向之剖面圖。
Claims (8)
- 一種碳化矽粉末之製造方法，其特徵係包含：將雜質之含有率為50ppm以下之矽酸質原料與雜質之含有率為300ppm以下之碳質原料以使碳質原料與矽酸質原料之混合莫耳比(C/SiO2)為2.5~4.0之方式混合，來調製碳化矽製造用原料之步驟，與在具備由碳所組成的發熱體之艾其遜爐內，將前述碳化矽製造用原料予以繞成而得雜質之含有率為120ppm以下之碳化矽粉末之步驟。
- 如申請專利範圍第1項之碳化矽粉末之製造方法，其中前述由碳所組成的發熱體中，其雜質含有率為前述碳化矽製造用原料中雜質之含有率以下。
- 如申請專利範圍第1項之碳化矽粉末之製造方法，其中前述由碳所組成的發熱體中，其雜質含有率為120ppm以下。
- 如申請專利範圍第2項之碳化矽粉末之製造方法，其中前述由碳所組成的發熱體中，其雜質含有率為120ppm以下。
- 如申請專利範圍第1~4項中任一項之碳化矽粉末之製造方法，其中前述矽酸質原料為非晶質二氧化矽。
- 如申請專利範圍第1~4項中任一項之碳化矽粉末之製造方法，其中前述碳質原料為碳黑。
- 如申請專利範圍第1~4項中任一項之碳化矽粉末之製造方法，其中前述矽酸質原料為非晶質二氧化矽，且 前述碳質原料為碳黑。
- 如申請專利範圍第1~4項中任一項之碳化矽粉末之製造方法，其中前述碳化矽製造用原料經預先顆粒化。
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| JP5797086B2 (ja) * | 2011-11-01 | 2015-10-21 | 太平洋セメント株式会社 | 高純度炭化珪素粉末の製造方法 |
| KR101349502B1 (ko) * | 2011-12-28 | 2014-01-08 | 엘지이노텍 주식회사 | 탄화규소 분말 제조 방법 |
| JP6230106B2 (ja) * | 2013-07-31 | 2017-11-15 | 太平洋セメント株式会社 | 炭化珪素単結晶の製造方法 |
| JP6270414B2 (ja) * | 2013-10-30 | 2018-01-31 | 太平洋セメント株式会社 | 炭化珪素の製造方法 |
| JP6210598B2 (ja) * | 2014-02-25 | 2017-10-11 | 太平洋セメント株式会社 | 炭化珪素粉末の製造方法 |
| CN105236410B (zh) * | 2015-09-15 | 2017-07-18 | 扬州大学 | 发光非晶碳化硅纳米颗粒的制备方法 |
| CN105858664B (zh) * | 2016-06-17 | 2017-11-28 | 大同新成新材料股份有限公司 | 可提高碳化硅质量的方法及艾奇逊炉 |
| JP6990136B2 (ja) * | 2017-07-27 | 2022-01-12 | 太平洋セメント株式会社 | 炭化ケイ素粉末 |
| CN108529630A (zh) * | 2018-07-17 | 2018-09-14 | 东北大学 | 一种采用内热法制备碳化硅的方法 |
| JP7518593B2 (ja) * | 2020-01-29 | 2024-07-18 | 太平洋セメント株式会社 | 炭化ケイ素粉末の製造方法 |
| JP7483192B2 (ja) * | 2020-03-19 | 2024-05-15 | 太平洋セメント株式会社 | 複合粒子およびその製造方法 |
| CN112811426A (zh) * | 2020-12-31 | 2021-05-18 | 山东天岳先进科技股份有限公司 | 一种碳化硅粉料及制备方法与装置 |
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| US4419336A (en) * | 1982-03-29 | 1983-12-06 | Norton Company | Silicon carbide production and furnace |
| US4702900A (en) * | 1985-04-08 | 1987-10-27 | Bridgestone Corporation | Method of producing silicon carbide |
| US4686032A (en) * | 1985-04-10 | 1987-08-11 | Electro Minerals (Canada), Inc. | Automatic method for separating and cleaning silicon carbide furnace materials |
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| JPS6461308A (en) | 1987-09-01 | 1989-03-08 | Tokai Konetsu Kogyo Kk | Production of high-purity silicon carbide powder |
| ES2059003T3 (es) * | 1990-09-07 | 1994-11-01 | Starck H C Gmbh Co Kg | Procedimiento para la preparacion de polvo de carburo de silicio beta. |
| EP0486938B1 (en) * | 1990-11-20 | 1999-05-19 | Asahi Glass Company Ltd. | Heat treating apparatuses for semiconductors and high purity silicon carbide parts for the apparatuses and a method of making thereof |
| NO306815B1 (no) * | 1994-06-06 | 1999-12-27 | Norton As | Fremgangsmåte ved fremstilling av siliciumkarbid |
| JP4006716B2 (ja) | 1997-06-20 | 2007-11-14 | 信越石英株式会社 | 高純度炭化珪素粉およびその製造方法 |
| JP4589491B2 (ja) * | 1999-08-24 | 2010-12-01 | 株式会社ブリヂストン | 炭化ケイ素粉末、グリーン体の製造方法、及び炭化ケイ素焼結体の製造方法 |
| ITMI20081085A1 (it) * | 2008-06-16 | 2009-12-17 | N E D Silicon S P A | Metodo per la preparazione di silicio di grado metallurgico di elevata purezza. |
| DE102008042499A1 (de) * | 2008-09-30 | 2010-04-01 | Evonik Degussa Gmbh | Verfahren zur Herstellung von hochreinem Siliciumcarbid aus Kohlenhydraten und Siliciumoxid durch Kalzinierung |
| WO2012163534A1 (en) * | 2011-06-03 | 2012-12-06 | Evonik Solar Norge As | Starting materials for production of solar grade silicon feedstock |
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| EP2749531A4 (en) | 2015-05-13 |
| KR20140081784A (ko) | 2014-07-01 |
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| TW201326041A (zh) | 2013-07-01 |
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| US9382121B2 (en) | 2016-07-05 |
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| EP2749531B1 (en) | 2023-08-23 |
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