EP4168372A1 - Verfahren zur herstellung eines sic-precursormaterials - Google Patents
Verfahren zur herstellung eines sic-precursormaterialsInfo
- Publication number
- EP4168372A1 EP4168372A1 EP20753909.9A EP20753909A EP4168372A1 EP 4168372 A1 EP4168372 A1 EP 4168372A1 EP 20753909 A EP20753909 A EP 20753909A EP 4168372 A1 EP4168372 A1 EP 4168372A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- silicon carbide
- precursor material
- precursor
- sic
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000000463 material Substances 0.000 title claims abstract description 200
- 239000002243 precursor Substances 0.000 title claims abstract description 198
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 95
- 230000008569 process Effects 0.000 claims abstract description 49
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 323
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 310
- 229910052710 silicon Inorganic materials 0.000 claims description 76
- 239000010703 silicon Substances 0.000 claims description 76
- 239000000843 powder Substances 0.000 claims description 59
- 150000001722 carbon compounds Chemical class 0.000 claims description 50
- 239000006185 dispersion Substances 0.000 claims description 50
- 239000000203 mixture Substances 0.000 claims description 42
- 239000000178 monomer Substances 0.000 claims description 41
- 229920000642 polymer Polymers 0.000 claims description 31
- 239000002245 particle Substances 0.000 claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims description 22
- 239000011246 composite particle Substances 0.000 claims description 20
- 238000002425 crystallisation Methods 0.000 claims description 20
- 230000008025 crystallization Effects 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 18
- 150000001720 carbohydrates Chemical class 0.000 claims description 17
- 239000011258 core-shell material Substances 0.000 claims description 15
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 12
- 239000008103 glucose Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 229930091371 Fructose Natural products 0.000 claims description 10
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 10
- 239000005715 Fructose Substances 0.000 claims description 10
- 239000002105 nanoparticle Substances 0.000 claims description 10
- 235000020357 syrup Nutrition 0.000 claims description 9
- 239000006188 syrup Substances 0.000 claims description 9
- 150000004676 glycans Chemical class 0.000 claims description 8
- 239000012705 liquid precursor Substances 0.000 claims description 8
- 229920001282 polysaccharide Polymers 0.000 claims description 8
- 239000005017 polysaccharide Substances 0.000 claims description 8
- 239000011859 microparticle Substances 0.000 claims description 7
- 239000008241 heterogeneous mixture Substances 0.000 claims description 6
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 239000004417 polycarbonate Substances 0.000 claims description 4
- 229920000515 polycarbonate Polymers 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims description 2
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims description 2
- 150000002016 disaccharides Chemical class 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 229920001542 oligosaccharide Polymers 0.000 claims description 2
- 150000002482 oligosaccharides Chemical class 0.000 claims description 2
- 229920001643 poly(ether ketone) Polymers 0.000 claims description 2
- 239000005014 poly(hydroxyalkanoate) Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000903 polyhydroxyalkanoate Polymers 0.000 claims description 2
- 229920001470 polyketone Polymers 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 74
- 229910045601 alloy Inorganic materials 0.000 description 21
- 239000000956 alloy Substances 0.000 description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- 239000002270 dispersing agent Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 13
- 239000000758 substrate Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 230000009471 action Effects 0.000 description 9
- 238000009826 distribution Methods 0.000 description 9
- -1 for example Chemical compound 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000007858 starting material Substances 0.000 description 9
- 229910000676 Si alloy Inorganic materials 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 229960004903 invert sugar Drugs 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
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- 235000020374 simple syrup Nutrition 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 230000005855 radiation Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000007641 inkjet printing Methods 0.000 description 4
- 150000001247 metal acetylides Chemical class 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 235000012431 wafers Nutrition 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 229910052698 phosphorus Chemical group 0.000 description 3
- 239000011574 phosphorus Chemical group 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 238000000859 sublimation Methods 0.000 description 3
- 230000008022 sublimation Effects 0.000 description 3
- 235000000346 sugar Nutrition 0.000 description 3
- 238000007669 thermal treatment Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 150000001298 alcohols Chemical group 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 229920000140 heteropolymer Polymers 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000000110 selective laser sintering Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- 150000008163 sugars Chemical class 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 235000010338 boric acid Nutrition 0.000 description 1
- 125000005619 boric acid group Chemical class 0.000 description 1
- 150000001638 boron Chemical class 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 150000002402 hexoses Chemical class 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002471 indium Chemical class 0.000 description 1
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical group 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 235000021190 leftovers Nutrition 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- ZLANVVMKMCTKMT-UHFFFAOYSA-N methanidylidynevanadium(1+) Chemical class [V+]#[C-] ZLANVVMKMCTKMT-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000013386 optimize process Methods 0.000 description 1
- 150000002972 pentoses Chemical class 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 239000011593 sulfur Chemical group 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- 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
- C01B32/984—Preparation from elemental silicon
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6346—Polyesters
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63464—Polycarbonates
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Definitions
- the present invention relates to the technical field of the production of silicon carbide, in particular by means of high-energy processes.
- the present invention relates to a method for producing a SiC precursor material which is suitable for producing silicon carbide-containing materials, in particular silicon carbide, preferably in high-energy processes such as selective synthetic crystallization.
- the present invention further relates to an SiC precursor material for producing silicon carbide-containing materials, in particular silicon carbide.
- the present invention relates to the use of an SiC precursor material in high-energy processes.
- the present invention also relates to a method for producing silicon carbide-containing materials, in particular silicon carbide, from an SiC precursor material.
- the present invention relates to materials containing silicon carbide, in particular silicon carbide, obtainable from an SiC precursor material.
- Silicon carbide with the chemical formula SiC also known under the name “Carborundum” is a non-oxidic ceramic solid that has outstanding properties.
- the properties of silicon carbide have a high level of constancy up to temperatures of around 1,400 ° C.
- silicon carbide is characterized by low density and thermal expansion, high hardness and thermal conductivity, good corrosion and wear resistance, which are also given at high temperatures and are accordingly expressed in the excellent dimensional stability of silicon carbide ceramics and components.
- silicon carbide is toxicologically harmless and therefore, unlike many oxidic or metal-containing materials, not harmful to humans.
- Silicon carbide offers itself as a construction material and is traditionally used as an abrasive or is used in semiconductor technology, preferably in semiconductor electronics.
- the properties of silicon carbide can be aligned and, in particular, optimized for the intended application by alloying or doping.
- silicon carbide ceramics are ideal for demanding areas of application and challenging conditions, such as in chemical production.
- silicon carbide is also used as an insulator in high-temperature reactors.
- Silicon carbide-containing materials are usually obtained by sintering processes from starting materials or starting material mixtures which contain silicon carbide particles.
- the properties of these porous silicon carbide structures or bodies do not correspond to those of compact crystalline silicon carbide, so that the advantageous properties of silicon carbide in particular are not fully exploited by sintering processes.
- Structures made of inorganic materials can also be produced by means of high-energy processes, such as selective synthetic crystallization, in which the starting materials or precursors used react or sublime due to a high input of energy.
- the selective synthetic crystallization processes enable rapid implementation and the production of inorganically based structures or bodies.
- the use of the corresponding high-energy processes is associated with a number of challenges for both the precursor and the product materials.
- Precursor materials have to react in a predetermined manner when exposed to energy and in particular disruptive side reactions have to be excluded.
- it must be possible to rule out segregation or phase separation or decomposition of the resulting products due to the high energy exposure.
- silicon carbide In the case of silicon carbide, this is made more difficult by the fact that silicon carbide is in the range at high temperatures, depending on the respective crystal type between 2,300 and 2,700 ° C does not melt, but sublimates, ie changes from the solid directly to the gaseous state of aggregation.
- Silicon carbide is therefore not suitable, or only suitable to a very limited extent, as a starting material in high-energy processes for the efficient production of corresponding inorganically based structures or bodies. Because of the versatility of silicon carbide and the large number of positive application properties, approaches that overcome this disadvantage are of great interest.
- An efficient possibility of producing silicon carbide-containing materials or bodies consists in the use of suitable precursor compounds or materials which react to silicon carbide or silicon carbide-containing materials under the action of energy.
- DE 10 2015 100 062 A1 describes a method for producing silicon carbide-containing materials, in particular silicon carbide crystals or fibers, which are obtained by deposition from the gas phase. For this purpose, a precursor granulate is used as the starting material, which is obtained by a sol-gel process and then subjected to a thermal treatment at over 1,000 ° C.
- additive manufacturing processes for the direct manufacture of objects containing silicon carbide from suitable precursor materials are known, for example from DE 10 2015 105 085 A1, DE 10 2017 110 362 A1, DE 10 2017 110 361 A1 or also DE 10 2018 127 877.2
- DE 102015 105 085 A1 describes a method for producing bodies from silicon carbide crystals, the silicon carbide being obtained in particular by laser irradiation of precursor materials containing suitable carbon and silicon. Under the action of the laser beam, the precursor materials decompose selectively and silicon carbide is formed without sublimation processes occurring.
- DE 102018 127877.2 describes an optimized process that allows a defined, uniformly composed SiC precursor granulate to be obtained reproducibly by first homogenizing or dissolving the individual components or starting materials of the granulate composition in a preferably colloidal solution or dispersion. This is followed by the rapid removal of the solvent or dispersant, since it has been shown that aging of the colloidal solution to form a gel, as described in DE 102015 105085 A1, is not necessary.
- the complex thermal treatment at temperatures of over 1,000 ° C. can be dispensed with and in this way a significant saving in time and energy can be achieved, which reduces the costs for the production of an SiC precursor granulate , can be significantly reduced.
- DE 10 2017 110 362 A1 relates to the production of objects containing silicon carbide, in particular from silicon carbide alloys, starting from powdered precursor materials by means of what is known as selective synthetic crystallization.
- the selective synthetic crystallization relates in detail to high-energy processes for the production of silicon carbide and silicon carbide alloys, preferably by means of additive manufacturing.
- Selective synthetic crystallization includes processes which are based on laser deposition welding, as described in DE 10 2018 128 434.9, for example, selective laser melting, such as in the
- DE 10 2017 110 362 A1 or inkjet printing methods, as known, for example, from DE 10 2017 110 361 A1, are based and in which a silicon carbide-containing material is successively produced from an SiC precursor material through a targeted energy input, in particular a location-selective energy input Object is created.
- the prior art lacks a simple process that provides suitable compositions, in particular suitable SiC precursor materials, which can be used to produce silicon carbide, in particular silicon carbide-containing materials, in high-energy processes based on selective synthetic crystallization.
- the present invention is therefore based on the object of eliminating the aforementioned disadvantages associated with the prior art, or at least reducing them.
- one object of the present invention is to provide a simplified, efficient method for producing an SiC precursor material which can be used to produce silicon carbide-containing materials, in particular silicon carbide.
- a further object of the present invention is to provide a SiC precursor material which can be produced reproducibly with controllable quality.
- a further object of the present invention is to provide a method for producing silicon carbide-containing materials, in particular silicon carbide, from an SiC precursor material which is advantageous in terms of its implementation compared to the methods described in the prior art.
- silicon carbide-containing materials, in particular silicon carbide obtainable from an SiC precursor material.
- the subject matter of the present invention according to a first aspect of the present invention is thus a method for producing an SiC precursor material according to claim 1; further advantageous refinements of this aspect of the invention are the subject matter of the relevant subclaims.
- Another object of the present invention according to a second aspect of the present invention is an SiC precursor material according to claim 13; further advantageous refinements of this aspect of the invention are the subject matter of the relevant subclaims.
- the present invention further relates to the use of an SiC precursor material according to claim 17.
- Yet another subject matter of the present invention according to a fourth aspect of the present invention is a method for producing silicon carbide, in particular silicon carbide-containing materials, from an SiC precursor material according to claim 18; further advantageous refinements of this aspect of the invention are the subject of the related sub-claim.
- the present invention further provides silicon carbide, in particular silicon carbide-containing materials, obtainable from an SiC precursor material according to claim 20.
- the subject of the present invention - according to a first aspect of the present invention - is thus a method for Fier ein a SiC- Precursor materials, where elemental silicon is mixed with at least one organic carbon compound.
- SiC precursor materials can be produced from elementary silicon and at least one organic carbon compound efficiently and reproducibly with constant quality, which allow the production of silicon carbide in high-energy processes.
- a combination of silicon powder and saccharides, in particular sugars makes it possible to produce inexpensive and highly pure precursor materials in a particularly simple and easily reproducible manner.
- composite particles with a core-shell structure, in particular a silicon core and a shell made of sugar are also accessible in this way.
- the method according to the invention allows the provision of a large number of SiC precursor materials from which a wide variety of silicon carbide-containing materials can then be produced.
- a silicon carbide-containing material is to be understood as meaning a binary, ternary or quaternary inorganic compound or alloy whose empirical formula contains silicon and carbon.
- a silicon carbide-containing compound does not contain any molecularly bound carbon, such as, for example, carbon monoxide or carbon dioxide; rather, the carbon is in a solid structure.
- the method according to the invention also ensures that silicon carbide-containing material or silicon carbide can be reliably obtained from the SiC precursor material by means of methods that can be carried out efficiently.
- the composition of the SiC precursor material allows a method to be carried out which provides temperatures in the context of silicon carbide production which are safely below the sublimation limit of silicon carbide.
- silicon carbide can be obtained reliably and with little effort for a variety of purposes from an SiC precursor material that can be produced in an uncomplicated manner.
- a significant advantage of the method according to the invention is that the elemental silicon used can be obtained from easily accessible sources.
- the preparation of the elemental silicon for the method for producing the SiC precursor material can be carried out particularly easily.
- the quality of the elemental silicon used can also be traced and ensured, so that the SiC precursor material can be produced in a reproducible manner and with constant quality.
- the purity of the silicon and thus ultimately also of the silicon carbide-containing materials obtained with the precursor materials can be determined by the selection of the respective reference source, whereby silicon carbide-containing materials can be provided for a wide variety of applications under respectively optional economic conditions.
- the method according to the invention in that it starts from reusable raw material sources and / or excess material residues, represents an advantageous, since value-adding, further use of elemental silicon.
- elemental silicon can be used for the production of the SiC precursor material from the production of silicon wafers or Solar cells are purchased, ie the material leftovers can easily be removed from the respective manufacturers.
- This aspect of the further use of a raw material that is qualitatively flawless, but initially in excess, is a particular example of a value-adding further use of material residues and also has a positive effect on the cost efficiency of the method according to the invention.
- the elemental silicon is used in the form of a powder, in particular in the form of a microscale powder, preferably in the form of a nanoscale powder.
- the elemental silicon is used in the form of particles, in particular in the form of microparticles, preferably in the form of nanoparticles.
- the elementary silicon is used in the form of monocrystalline particles, in particular in the form of monocrystalline microparticles, preferably in the form of monocrystalline nanoparticles.
- the use of the elemental silicon in the powdery, in particular particulate, nature mentioned favors the homogeneous distribution of the elemental silicon in the SiC precursor material according to the invention.
- a homogeneous distribution of the material components enables the efficient implementation of the SiC precursor material in high-energy processes, in particular also with brief exposure to high temperatures, as is the case with laser-based processes.
- the elementary silicon is obtained from reusable raw material sources and / or comes from excess material residues from silicon processing.
- the elemental silicon in particular the elemental silicon from reusable raw material sources and / or excess material residues from silicon processing, is comminuted, in particular crushed, preferably ground.
- Reusable raw material sources and / or excess material residues from silicon processing are understood in the context of the present invention to mean, for example, excess material from silicon wafer production or solar cell production.
- These excess materials can then advantageously be collected and processed in the context of a flomogenization process for use in producing the SiC precursor material.
- elemental silicon from the sources described has the great advantage that the quality of the elemental silicon used is reliably ensured. At the same time, it can be assumed that both the SiC precursor material and the silicon carbide produced therefrom are largely free of undesirable impurities and by-products. In the context of the present invention, it is now further preferred if elemental silicon with a degree of purity of at least 95%, in particular at least 98%, preferably at least 99%, preferably at least 99.5%, is used. This makes it possible on the one hand to obtain highly pure and defined silicon carbide ceramics, on the other hand it is also possible to produce silicon carbides with specific and preselected electrical properties.
- the elemental silicon is mixed with at least one organic carbon compound.
- an organic carbon compound is understood to be a compound that is composed predominantly of the elements carbon, hydrogen and oxygen.
- other heteroatoms such as nitrogen, sulfur or phosphorus can also be contained in the organic carbon compound, these heteroatoms only being desirable if doping of the silicon carbide is to be achieved.
- organic carbon compound it is preferably provided within the scope of the present invention that it is used in liquid form.
- the organic carbon compound if it is present as a solid, is first brought into solution and then used for the method for producing the SiC precursor material. If the organic carbon compound is already present as a liquid or at least essentially in liquid form, it is used as such directly for the production process.
- the organic carbon compound can in particular be present in a liquid or in the form of a liquid solution or dispersion which contain the organic carbon compound, as explained below.
- the organic carbon compound in liquid form is preferably suitable for forming a homogeneous dispersion with the elemental silicon, in particular in the form of a nano- or microscale powder.
- the organic carbon compound is a polymer or an oligomer or monomer.
- a monomer is generally understood to be a low molecular weight, reactive molecular unit which can be converted in polyreactions to form higher molecular weight compounds such as oligomers or polymers.
- structurally identical or structurally similar, at least similarly reactive, monomers are linked to one another via reactive groups such as multiple bonds or functional groups and thus form the basic units of an oligomer or polymer.
- Exemplary polyreactions can be polycondensations, polyadditions and radical or coordinative polymerizations, without wishing to limit the type of possible polyreactions by this list.
- an oligomer is understood to mean a molecule that results from monomers reacted with one another in a polyreaction.
- an oligomer is composed of at least two monomer units. These monomer units can be the same or different, so that homooligomers or heterooligomers are obtained.
- oligomers have a definable number of repeating units, in particular between two and 50 repeating units.
- polymers are understood as meaning macromolecular compounds which are built up in a polyreaction from one or more different monomers.
- the term polymer therefore includes both homopolymers and heteropolymers; Homopolymers are obtained by reacting the same monomers and heteropolymers are obtained by reacting different monomers.
- polymers can have a relatively broad distribution of the monomeric repeating units. Overall, polymers within the meaning of the invention are characterized by a number of monomer units that is difficult to define and have high average molecular weights.
- the organic carbon compound is a polymer or oligomer
- the organic carbon compound is preferably characterized in that the polymer or oligomer is selected from the group of polyethers, polyethylene glycols, polysaccharides, polyketones, polyether ketones, polyesters, polycarbonates, polyhydroxyalkanoates and mixtures thereof , in particular polyethers, polysaccharides, polyesters, polycarbonates and their mixtures, is preferably a polysaccharide.
- the organic carbon compound is a monomer
- the monomer is a monomer for producing the aforementioned polymers or oligomers, in particular selected from the group of ethers, saccharides, esters, carbonates, carboxylic acids and mixtures thereof, preferably a saccharide is.
- the organic carbon compound in particular the polymer or oligomer, has ether, carbonyl, acetal, ester and / or carbonate repeat units.
- Organic carbon compounds of the aforementioned nature and composition show in the context of the present invention an advantageous mixing behavior with the elemental silicon in the course of the production of the SiC precursor material and excellent properties in the production of silicon carbide in the context of high-energy processes from the SiC precursor material , since they contain in particular carbon, hydrogen and oxygen and thus possibly form by-products which are preferably highly volatile and do not reduce the quality of the silicon carbide produced.
- the one organic carbon compound, in particular the polymer or oligomer or monomer is linear and / or branched and / or cyclic. Branched or cyclic monomers can occur in particular when using sugars or other substances that can react to form oligomers or polymers.
- the organic carbon compound in particular the polymer or oligomer or monomer, has functional groups, in particular hydroxyl groups, in addition to the repeating units.
- the organic carbon compound is present as a heterogeneous mixture, in particular as a heterogeneous mixture of monomers and monomer condensate, preferably as a heterogeneous mixture of monomer and dimeric, oligomeric or polymeric monomer condensate.
- the organic carbon compound, in particular the polymer or oligomer or monomer is a polyalcohol.
- the polyalcohol is a saccharide.
- the saccharide is selected from the group of hexoses or pentoses or mixtures thereof.
- saccharides as a special form of the organic carbon compound is characterized in particular by the fact that saccharides have an advantageously balanced ratio between carbon, hydrogen and oxygen in the context of the present invention and thus in the context of the production of silicon carbide from the SiC precursor according to the invention - show ideal reaction behavior. Above all, it should be emphasized here that saccharides enable the formation of particularly pure silicon carbide, since apart from carbon only volatile by-products are released, in particular water.
- the saccharide is selected from the group of glucose and its stereoisomers, fructose and its stereoisomers, xylose and its stereoisomers, the disaccharides of the aforementioned compounds, in particular glucose and / or fructose, preferably the glucose and fructose, the oligosaccharides of the aforementioned compounds, in particular glucose and / or fructose, the polysaccharides of the aforementioned compounds, in particular glucose or mixtures thereof.
- the saccharide is in the form of a liquid, in particular in the form of a syrup, preferably in the form of a highly concentrated syrup.
- a highly concentrated syrup is understood to mean an aqueous solution of the saccharide with a water content of less than 25% by weight, based on the total amount of the syrup. Watery Saccharide solutions with a water content equal to or greater than 25% by weight are regarded as syrup.
- the saccharide is invert sugar syrup.
- Invert sugar syrup in the context of the invention means an aqueous solution of sucrose or starch which has been partially inverted by hydrolysis.
- the invert sugar syrup in this connection can contain varying proportions of the glucose and fructose obtained by partial hydrolysis. These proportions are preferably between 5 to 95% for glucose and accordingly between 95 to 5% for fructose, based on the total amount of monosaccharides in the invert sugar syrup. This is because it has been found for this special embodiment that elemental silicon can be mixed so well with invert sugar syrup that a particularly homogeneous distribution of elemental silicon in powder or particle form can be achieved. This forms the ideal prerequisites for the production of a uniformly composed, reproducible and controllable high-quality SiC precursor material from which silicon carbide can subsequently be produced efficiently and reliably.
- the mixture of elemental silicon and organic carbon compound is in the form of a dispersion.
- a dispersion is to be understood as an at least two-phase system, a first phase, namely the dispersed phase, being present in a distributed manner in a second phase, the continuous phase.
- the dispersion contains a dispersant.
- the dispersant is selected from water, organic solvents and / or mixtures thereof.
- the organic solvent is selected from alcohols, esters, ketones, amines, amides, sulfoxides and mixtures thereof, in particular methanol, ethanol, 2-propanol, acetone, ethyl acetate, / V, / V-dimethylformamide, dimethyl sulfoxide and mixtures thereof.
- both components are mixed, in particular mixed, preferably stirred, in the presence of a dispersant.
- a dispersant it has preferably proven useful if the mixture or dispersion of elemental silicon and organic carbon compound, in particular polymer or oligomer or monomer, is homogeneously distributed.
- the homogeneous distribution of components in a mixture or dispersion is understood to mean that these components are present within the mixture or dispersion in such a way that a very similar, preferably identical, composition of the components is found throughout the mixture or dispersion becomes.
- the term homogeneous particles is understood to mean that particles are present which are characterized by at least essentially the same properties such as size, density, nature or chemical composition.
- the dispersion of elemental silicon and organic carbon compound, in particular polymer or oligomer or monomer is converted into a powder, in particular a precursor powder, by drying, in particular afterwards.
- This procedure is characterized by the fact that, as part of the conversion into a powder, a particularly homogeneous distribution and thorough mixing of the Components, ie of elemental silicon and the at least one organic carbon compound, is achieved.
- the dispersion of elemental silicon and organic carbon compound in particular polymer or oligomer or monomer, is carried out
- (ii) is optionally converted downstream into a powder, in particular a precursor powder, by drying.
- the dispersion of elemental silicon and organic carbon compound in particular polymer or oligomer or monomer, is carried out
- the SiC precursor material into a powder, in particular a microscale powder, preferably a nanoscale powder, by comminuting, in particular crushing, preferably grinding, preferably grinding.
- the SiC precursor material is available as a precursor powder, in particular as a granular precursor powder, or as a precursor dispersion, in particular as a solid-in-liquid precursor dispersion.
- the precursor powder or the precursor dispersion consists of homogeneous particles, in particular microparticles, preferably consists of or contains nanoparticles, preferably consists of them.
- the precursor powder or the precursor dispersion consists of composite particles, in particular homogeneous composite particles, preferably composite particles with a core-shell structure (core-shell structure), or contains these , preferably consists of this.
- composite particles with a core-shell structure are generally understood to mean particles which have an inner core and an outer shell.
- the inner core can for example be formed by the elementary silicon, so that the outer shell is formed by the at least one organic carbon compound.
- the SiC precursor material according to the invention when present as a precursor powder, in particular as a granular precursor powder, a particularly preferred embodiment of the present invention provides for the SiC precursor material to be composed of homogeneous particles, in particular microparticles, preferably nanoparticles , and these particles are preferably composite particles, in particular homogeneous composite particles, preferably composite particles with a core-shell structure (core-shell structure), or contain them.
- SiC precursor materials composed in this way are characterized by an overall high level of homogeneity.
- this circumstance allows particularly good conversions and the formation of silicon carbide with a particularly uniform composition in relation to the quantitative ratio between carbon and silicon.
- particularly good results are now obtained for the powdery, in particular particulate, SiC precursor material if the powder has particle sizes in the range from 0.1 ⁇ m to 1,500 ⁇ m, in particular 0.1 ⁇ m to 1,000 ⁇ m, preferably 0, 5 pm to 800 pm, preferably 1 pm to 600 pm.
- SiC precursor materials which are present in the form of precursor powders, in particular particles, preferably in the form of composite particles, preferably composite particles with a core-fill structure, also make it possible to control the composition of the silicon carbide produced in advance by simply the quantitative ratio between elemental silicon and the at least one organic carbon compound is varied.
- the SiC precursor material is obtainable in the form of a precursor dispersion, in particular in the form of a solid-in-liquid precursor dispersion. It is very particularly preferred if the precursor dispersion is in the form of an SiC precursor sol, for the production of silicon carbide-containing materials, in particular silicon carbide of the aforementioned nature.
- the solvent or dispersant for the SiC precursor material in the form of a solution or dispersion in particular in the form of an SiC precursor sol, this can be selected from all suitable solvents or dispersants.
- the dispersant is selected from water and organic solvents and their mixtures.
- the organic carbon compounds used and the elemental silicon should have sufficiently high solubilities or high dispersibility in the solvents used, in particular in ethanol and / or water, in order to be able to form finely divided dispersions or solutions, especially sols.
- the SiC precursor components should also not react with other constituents of the dispersion, in particular the sol, to form insoluble compounds during the production process. About that In addition, the individual components should be distributed as homogeneously as possible in the dispersion.
- the organic dispersant is selected from alcohols, in particular methanol, ethanol, 2-propanol, acetone, ethyl acetate and mixtures thereof. It is particularly preferred in this context if the organic dispersant is selected from methanol, ethanol, 2-propanol and mixtures thereof, with ethanol being particularly preferred.
- organic dispersants are miscible with water over a wide range and in particular are also suitable for dispersing polar inorganic substances.
- mixtures of water and at least one organic dispersant in particular mixture of water and ethanol, are preferably used as the dispersant.
- the dispersant has a weight ratio of water to organic solvent of 1:10 to 20: 1, in particular 1: 5 to 15: 1, preferably 1: 2 to 10: 1, preferably 1: 1 to 5: 1, particularly preferably 1: 3.
- the amount in which the composition contains the dispersant can vary within a wide range depending on the particular application conditions and the type of silicon carbide-containing compound to be produced.
- the composition usually has dispersants in amounts of 10 to 80% by weight, in particular 15 to 75% by weight, preferably 20 to 70% by weight, preferably 20 to 65% by weight, based on the composition.
- the viscosity of the SiC precursor material in the form of a precursor dispersion in particular in the form of a solid-in-liquid precursor dispersion, preferably in the form of an SiC precursor sol, this can vary within wide ranges in view of the respective application conditions and the structures to be produced .
- the SiC precursor material is in the form of a precursor dispersion, in particular in the form of a solid-in-liquid precursor dispersion, preferably in the form of an SiC precursor sol, has a dynamic Brookfield viscosity at 25 ° C. in the range from 3 to 500 mPas, in particular 4 to 200 mPas, preferably 5 to 100 mPas.
- SiC precursor materials in the form of a precursor dispersion in particular in the form of a solid-in-liquid precursor dispersion, preferably in the form of an SiC precursor sol, which are suitable for spray or print application, can be used, as in this way even towering structures are accessible to a certain extent without support structures.
- a very particularly preferred embodiment of the present invention provides, in particular, a precursor dispersion which is composed of elemental silicon and a carbon compound which is in the form of a liquid, in particular in the form of a syrup, preferably in the form of a boiling-centered syrup.
- a precursor dispersion which is composed of elemental silicon and a carbon compound which is in the form of a liquid, in particular in the form of a syrup, preferably in the form of a boiling-centered syrup.
- an advantageous since it is easy to adjust and stable, homogeneous distribution of the components in the precursor dispersion is achieved.
- the elemental silicon is mixed with invert sugar syrup.
- a stable, highly viscous precursor dispersion is obtained from Flieraus, which can be processed easily, safely and specifically in the selective synthetic crystallization, applied as an inket process.
- stoichiometric silicon carbide For the production of stoichiometric silicon carbide, it has now proven itself within the scope of the present invention if there is an at least essentially stoichiometric silicon-to-carbon ratio between the elemental silicon and the organic carbon compound, in particular polymer or oligomer or monomer, in the SiC precursor material, in particular a silicon-to-carbon ratio in the range from 35:65% by weight to 65:35% by weight, preferably 40:60% by weight to 60:40% by weight, preferably 45:55% by weight to 55:45% by weight, particularly preferably 50:50 % By weight, based on the SiC precursor material.
- a stoichiometric silicon carbide or silicon carbide-containing material is to be understood as a material which contains carbon and silicon at least essentially in a molar silicon-to-carbon ratio in a range around 1: 1.
- non-stoichiometric silicon carbide can also be easily produced.
- a non-stoichiometric silicon carbide is to be understood as meaning a silicon carbide which does not contain carbon and silicon in a molar ratio of 1: 1.
- a non-stoichiometric silicon carbide usually has a molar excess of silicon.
- the non-stoichiometric silicon carbide is usually a silicon carbide of the general formula (I)
- SiC-i- x (I) with x 0.05 to 0.8, in particular 0.07 to 0.5, preferably 0.09 to 0.4, preferred
- Such silicon-rich silicon carbides have a particularly high mechanical strength and are suitable for a large number of applications as ceramics.
- the SiC precursor material usually contains (A) the silicon source in amounts of 60 to 90% by weight, in particular 65 to 85
- the carbon source in amounts of 10 to 40% by weight, in particular 15 to 35% by weight, preferably 20 to 30% by weight, each based on the SiC precursor material.
- SiC precursor materials which are intended to be used to produce non-stoichiometric silicon carbide or material containing silicon carbide, have a comparatively higher proportion of elemental silicon than the organic carbon compound.
- a silicon-to-carbon ratio between the elemental silicon and the organic carbon compound, in particular polymer or oligomer or monomer in the range of 65:35% by weight to 85:15% by weight in the SiC precursor material.
- % preferably 70:30% by weight to 80:20% by weight, preferably 72:28% by weight to 78:22% by weight, based on the SiC precursor material.
- the SiC precursor material in such a way that the silicon carbide-containing compound produced contains a silicon carbide alloy or is a silicon carbide alloy.
- the silicon carbide alloy is usually selected from MAX phases, alloys of silicon carbide with elements, in particular metals, and alloys of silicon carbide with metal carbides and / or metal nitrides.
- Such silicon carbide alloys contain silicon carbide in varying and strongly fluctuating proportions.
- silicon carbide is the main component of the alloys.
- the silicon carbide alloy contains silicon carbide only in small amounts.
- the silicon carbide alloy usually contains the silicon carbide, in particular the elements silicon and carbon, in amounts of 10 to 95% by weight, in particular 15 to 90% by weight, preferably 20 to 80% by weight, based on the silicon carbide alloy.
- M stands for an early transition metal from the third to sixth group of the periodic table of the elements, while A stands for an element of the 13th to 16th group of the periodic table of the elements.
- X is either carbon or nitrogen.
- MAX phases have unusual combinations of chemical, physical, electrical and mechanical properties, as they show both metallic and ceramic behavior depending on the conditions. This includes, for example, high electrical and thermal conductivity, high resistance to thermal shock, very high levels of hardness and low coefficients of thermal expansion.
- the silicon carbide alloy is a MAX phase
- the MAX phase is selected from TUSiC3 and T SiC.
- the silicon carbide-containing compound is an alloy of silicon carbide
- the alloy is an alloy of silicon carbide with metals
- the alloy is selected from alloys of silicon carbide with metals from the group of Al, Ti, V, Cr, Mn, Co, Ni, Zn, Zr and their mixtures.
- the alloy of silicon carbide is selected from alloys of silicon carbide with metal carbides and / or nitrides, it has proven useful if the alloys of silicon carbide with metal carbides and / or nitrides is selected from the group of boron carbides, in particular B4C, chromium carbides, in particular Cr2C3 , Titanium carbides, especially TiC, molybdenum carbides, especially M02C, niobearbides, especially NbC, tantalum carbides, especially TaC, vanadium carbides, especially VC, zirconium carbides, especially ZrC, tungsten carbides, especially WC, boron nitride, especially BN, and mixtures thereof.
- boron carbides in particular B4C
- chromium carbides in particular Cr2C3
- Titanium carbides especially TiC, molybdenum carbides, especially M02C, niobearbides, especially NbC
- tantalum carbides especially
- the SiC precursor material is used to produce a silicon carbide alloy, the SiC precursor material usually contains it
- a doping reagent is added to the elemental silicon or the SiC precursor material. If a doping reagent is added to the elemental silicon or the SiC precursor material, it has proven to be advantageous if the doping reagent is used in amounts of 0.000001 to 15% by weight, in particular 0.000001 to 10% by weight, preferably 0.000005 to 5% by weight, preferably 0.00001 to 1% by weight, based on the mixture, is added.
- the doping reagent can be selected from suitable doping elements.
- the doping reagent or the doping element is preferably selected from elements of the third and fifth main groups of the periodic table, which in particular are soluble in the dispersant.
- the doping reagent is suitable for n- or p-doping, in particular is selected from the group of the elements nitrogen, phosphorus, boron, aluminum and indium, and mixtures thereof.
- the solution can contain nitric acid, ammonium chloride or melanin. If doping with phosphorus is provided, for example phosphoric acid or phosphates or phosphonic acids can be used. In addition, nitrogen doping is also possible by performing the method according to the invention in a nitrogen atmosphere.
- doping with boron for example boric acids, borates or boron salts such as boron trichloride are used.
- the silicon carbide produced in particular the material containing silicon carbide, can thus be selected from silicon carbide, doped silicon carbide, non-stoichiometric silicon carbide, doped non-stoichiometric silicon carbide and silicon carbide alloys.
- silicon carbide-containing materials in particular different silicon carbide compounds, is thus accessible to the method according to the invention.
- Another object of the present invention - according to a second aspect of the present invention - is the SiC precursor material, containing elemental silicon and at least one organic carbon compound, obtainable by the process according to the invention.
- the SiC precursor material is preferably characterized in that the SiC precursor material is present as a precursor powder, in particular a microscale granular powder, preferably a nanoscale granular powder or as a precursor dispersion, in particular as a solid-in-liquid precursor dispersion.
- the precursor powder or the precursor dispersion contains or consists of homogeneous particles, in particular microparticles, preferably nanoparticles, preferably consists of them.
- the precursor powder or the precursor dispersion is composed of homogeneous composite particles, in particular composite particles with a core-shell structure.
- the composite particles in particular those with a core-shell structure (core-shell structure), have a core made of elemental silicon and a shell made of at least one organic carbon compound, in particular a polymer or oligomer or a monomer.
- Another object of the present invention - according to a third aspect of the present invention - is the use of an SiC precursor material, in particular an SiC precursor material with the aforementioned features, in high-energy processes, in particular in the context of selective synthetic crystallization processes.
- These high-energy processes are particularly suitable for applying silicon carbide-containing materials to a substrate surface, with generally gaseous, liquid or powdery precursor materials containing a silicon source and a carbon source being gasified and / or decomposed by the action of laser radiation.
- the use of the SiC precursor material according to the invention lends itself to the high-energy process for selective synthetic crystallization.
- at least some of the decomposition products generated by the action of laser radiation are deposited in a location-selective manner on the substrate surface as silicon carbide, in particular silicon carbide-containing material.
- the use of the SiC precursor material according to the invention in the high-energy process allows a very fast and inexpensive production of three-dimensional objects or coatings containing silicon carbide and, in particular, manages without the use of pressure in order to provide compact, non-porous or slightly porous materials and materials.
- both layers of silicon carbide-containing materials can be applied to a substrate surface and three-dimensional objects can be built up from silicon carbide-containing materials.
- Selective Synthetic Crystallization is - as described at the beginning - an additive manufacturing process that can be carried out with various starting materials.
- an object is manufactured in particular not from the melt but from the gas phase.
- precursor compounds are decomposed by the action of energy and converted into the gas phase, a rapid and locally sharply delimited phase Sublimation of the decomposition products to the desired silicon carbide compounds is observed.
- powdery SiC precursor materials are converted into silicon carbide-containing materials, in particular non-stoichiometric silicon-rich silicon carbides and silicon carbide alloys, by irradiation with a laser beam, for which purpose a device based on selective laser sintering (selective laser sintering) or . Selective Laser Melting (SLM) is used.
- SLM Selective Laser Melting
- the energy required to convert the precursor materials into the gas phase can be introduced into the powdery starting material through the laser radiation, whereby the precursor materials decompose into gaseous intermediate products, so that these then recombine directly to the desired products and are obtained in crystalline form.
- This method of selective synthetic crystallization is preferably carried out in several stages.
- the SiC precursor material in a first process step, is provided in the form of a layer or layer, and in a subsequent, second process step, it is converted into a silicon carbide-containing compound through the action of energy in certain areas.
- a layer of the three-dimensional object is thus produced, to which a further layer or layer of the SiC precursor material is applied in a subsequent third process step.
- the second and third process steps are repeated in total until the three-dimensional object is completed.
- a special feature of the process is that it does not require subsequent sintering steps, ie within the scope of the present invention the SiC precursors are selected and, in particular, matched to the selective synthetic crystallization process, that each is produced directly from the gas phase homogeneous, compact, three-dimensional body is obtained, which does not have to be subjected to sintering.
- the SiC precursor material according to the invention is implemented in the context of selective synthetic crystallization based on laser deposition welding according to DE 10 2018 128434.9, it is advantageous if the powdery precursor material, in finely divided and directed form, in particular in the form of a particle beam, in Direction of a substrate is moved. Before or when it hits the substrate, the SiC precursor material is gasified and decomposed by the action of laser radiation, so that the gaseous decomposition products are moved in the direction of the substrate, in particular in the form of a particle beam.
- a particle beam is to be understood here as a directed flow of particles or particles with a cross section that preferably remains constant and which preferably moves linearly.
- the SiC precursor material in particular the powdery SiC precursor material
- the SiC precursor material is gasified and decomposed by means of laser radiation, in particular in the immediate vicinity of the substrate surface, since this prevents secondary reactions and undesired agglomerations.
- the substrate is heated only extremely slightly by the energy introduced, in particular by the laser beam, so that the silicon carbide-containing material can be applied with as little tension as possible.
- crystalline silicon carbide absorbs laser energy significantly worse than the SiC precursor material.
- silicon carbide conducts heat very well, so that the defined silicon carbide compounds are deposited in a strictly localized manner. Any unwanted constituents of the SiC precursor material and any byproducts formed form stable gases such as CO2, FI2O, etc. under the high temperatures of the laser action and can therefore be removed accordingly via the gas phase.
- the SiC precursor material can also be used in the context of selective synthetic crystallization on the basis of 3D printing techniques, in particular in the inkjet process, in combination with the targeted input of energy into the material Analogous to DE 10 2017 110 361 A1 can be implemented to objects containing silicon carbide.
- a solution or dispersion of the SiC precursor in particular an SiC precursor sol, is usually applied in the form of a layer to a substrate in a first process step and the layer of solution or dispersion containing SiC precursor is applied in a subsequent second process step converted into a silicon carbide-containing compound by selective energy action. These process steps are repeated until the desired silicon carbide-containing structure is obtained.
- the process is an ink jet printing process, i.e. H. the solution and dispersion containing SiC precursor material is applied to the substrate by means of ink-jet printing.
- inkjet printing processes allows, in particular, a high-resolution and locally sharply delimited application of the solution containing SiC precursor material, in particular the SiC precursor sol, while using little material at the same time, so that filigree structures are also accessible for semiconductor applications.
- drop-on-demand processes or printers are used, with only the drops of liquid being generated which are actually actually applied to the substrate.
- the SiC precursor materials can also be used in a large number of other processes for the production of silicon carbide-containing materials.
- the SiC precursor material according to the invention in particular in the form of a precursor granulate, can be used for the production of silicon carbide-containing fibers and foams, as described in DE 10 2017 114 243 A1.
- the precursor material according to the invention in particular in the form of a solution or dispersion, can be used to produce layers comprising silicon carbide, in particular nitrogen-free silicon carbide-containing layers, as disclosed in DE 10 2017 122 708 A1.
- the SiC according to the invention can also generally be used for the production of layers from silicon carbide, as disclosed in particular in DE 10 2017 112 756 A1.
- the SiC precursor material is characterized in that it enables the formation of specifically adjustable silicon carbide or materials containing silicon carbide.
- elemental silicon in particular elemental silicon, which is obtained, for example, from silicon wafer production or solar cell production, the formation of disruptive, intercalating, by-products in the silicon carbide produced can be largely excluded.
- the composition of the SiC precursor material it is rather ensured that only gaseous by-products are produced, which can easily be removed in the context of the method for producing silicon carbide. In this context, any doping, alloying or production of non-stoichiometric silicon carbide can therefore also be set in a targeted manner.
- the use of the SiC precursor material according to the invention for the production of silicon carbide-containing materials or silicon carbide in a simple and, in particular, inexpensive manner allows reliable, reproducible and controllable access to silicon carbide-containing materials or silicon carbide of constant and high quality by means of methods that are carried out with little effort can.
- Another object of the present invention - according to a fourth aspect of the present invention - is a method for producing silicon carbide-containing materials, in particular silicon carbide, from an SiC precursor material, in particular an SiC precursor material containing elemental silicon and at least one organic carbon compound, in particular at least one polymer or oligomer or monomer, the SiC precursor material being converted in high-energy processes at temperatures above 1,300 ° C, in particular above 1,600 ° C, preferably above 1,700 ° C.
- the reaction is carried out under an inert gas atmosphere, in particular under an argon atmosphere. Under inert conditions it is avoided, in particular and advantageously, that foreign elements are unwantedly incorporated into the silicon carbide produced.
- reaction takes place in a temperature range from 1,000 to 2,500.degree. C., in particular 1,300 to 2,200.degree. C., preferably 1,500 to 2,000.degree. C., preferably 1,700 to 1,900.degree .
- silicon carbide-containing materials in particular silicon carbide, are obtained as a powder, in particular as a microscale powder, preferably as a nanoscale powder.
- silicon carbide particles are obtained, in particular crystalline silicon carbide particles, preferably monocrystalline silicon carbide particles, preferably monocrystalline silicon carbide nanoparticles.
- doped silicon carbide-containing material in particular doped silicon carbide, is obtained, in particular as a powder, preferably as a nanoscale powder, preferably as a nanoscale, crystalline powder.
- a material containing silicon carbide alloy, in particular silicon carbide alloys is obtained, in particular as a powder, preferably as a nanoscale powder, preferably as a nanoscale, crystalline powder.
- the silicon carbide produced with the method according to the invention is particularly distinguished by its high purity, so that it can ideally serve as a starting material for the production of silicon carbide wafers, for example.
- the ability to be freely doped and alloyed is a decisive advantage over known silicon carbides and their production methods.
- the silicon carbide produced from the SiC precursor material has an outstanding monodispersity and its grain size can be set variably.
- Another object of the present invention - according to a fifth aspect of the present invention - are silicon carbide-containing materials, in particular silicon carbide, obtainable from an SiC precursor material, in particular an SiC precursor material containing elemental silicon and at least one organic carbon compound, in particular at least one polymer or oligomer or monomer which can be obtained by the process according to the invention.
- the silicon carbide-containing material in particular silicon carbide, is preferably characterized in that the silicon carbide is present as a powder, in particular as a nanoscale powder, preferably as a single-crystalline nanoscale powder.
- the silicon carbide is present in the form of particles, in particular nanoparticles, preferably monocrystalline nanoparticles.
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Abstract
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DE102019121062.3A DE102019121062A1 (de) | 2019-08-05 | 2019-08-05 | Verfahren zur Herstellung eines SiC-Precursormaterials |
PCT/EP2020/071973 WO2021023761A1 (de) | 2019-08-05 | 2020-08-05 | Verfahren zur herstellung eines sic-precursormaterials |
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US5925405A (en) * | 1995-02-21 | 1999-07-20 | Ali-Khan; Imran | Method of manufacturing ceramic, metallic or ceramo-metallic, shaped bodies and layers |
DE102013204799A1 (de) * | 2013-03-19 | 2014-09-25 | Wacker Chemie Ag | Si/C-Komposite als Anodenmaterialien für Lithium-Ionen-Batterien |
DE102017110362A1 (de) * | 2017-05-12 | 2018-11-15 | Psc Technologies Gmbh | Verfahren zur Herstellung von siliciumcarbidhaltigen dreidimensionalen Objekten |
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