JP2023532002A - アルミン酸マグネシウムスピネルを含むセラミック焼結体 - Google Patents
アルミン酸マグネシウムスピネルを含むセラミック焼結体 Download PDFInfo
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- JP2023532002A JP2023532002A JP2022579883A JP2022579883A JP2023532002A JP 2023532002 A JP2023532002 A JP 2023532002A JP 2022579883 A JP2022579883 A JP 2022579883A JP 2022579883 A JP2022579883 A JP 2022579883A JP 2023532002 A JP2023532002 A JP 2023532002A
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- sintered body
- ceramic sintered
- ceramic
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- powder mixture
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- 239000000919 ceramic Substances 0.000 title claims abstract description 257
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 94
- 239000011029 spinel Substances 0.000 title claims abstract description 85
- 239000011777 magnesium Substances 0.000 title claims abstract description 33
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 31
- -1 magnesium aluminate Chemical class 0.000 title claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 146
- 238000005245 sintering Methods 0.000 claims abstract description 124
- 239000013078 crystal Substances 0.000 claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims description 209
- 238000000034 method Methods 0.000 claims description 166
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 81
- 239000000395 magnesium oxide Substances 0.000 claims description 52
- 238000000137 annealing Methods 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 33
- 238000001354 calcination Methods 0.000 claims description 27
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 26
- 239000004065 semiconductor Substances 0.000 claims description 26
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 23
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 21
- 239000012535 impurity Substances 0.000 claims description 19
- 229910020068 MgAl Inorganic materials 0.000 claims description 17
- 238000009826 distribution Methods 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 238000003754 machining Methods 0.000 claims description 9
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 150000002642 lithium compounds Chemical class 0.000 claims description 5
- 230000008569 process Effects 0.000 description 49
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 37
- 238000012545 processing Methods 0.000 description 31
- 239000000463 material Substances 0.000 description 29
- 239000012071 phase Substances 0.000 description 29
- 239000002245 particle Substances 0.000 description 28
- 210000002381 plasma Anatomy 0.000 description 28
- 238000005530 etching Methods 0.000 description 25
- 230000007797 corrosion Effects 0.000 description 20
- 238000005260 corrosion Methods 0.000 description 20
- 239000007789 gas Substances 0.000 description 19
- 239000000126 substance Substances 0.000 description 19
- 230000003628 erosive effect Effects 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 14
- 230000003746 surface roughness Effects 0.000 description 14
- 238000005259 measurement Methods 0.000 description 13
- 239000007858 starting material Substances 0.000 description 13
- 238000002156 mixing Methods 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 11
- 229910052566 spinel group Inorganic materials 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 230000000875 corresponding effect Effects 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 238000001878 scanning electron micrograph Methods 0.000 description 10
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 229910052736 halogen Inorganic materials 0.000 description 8
- 150000002367 halogens Chemical class 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 7
- 238000007654 immersion Methods 0.000 description 7
- 238000003801 milling Methods 0.000 description 7
- 239000002019 doping agent Substances 0.000 description 6
- 238000004439 roughness measurement Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000000280 densification Methods 0.000 description 5
- 239000011858 nanopowder Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910001610 cryolite Inorganic materials 0.000 description 4
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 4
- 238000010587 phase diagram Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- BHHYHSUAOQUXJK-UHFFFAOYSA-L zinc fluoride Chemical compound F[Zn]F BHHYHSUAOQUXJK-UHFFFAOYSA-L 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229910021582 Cobalt(II) fluoride Inorganic materials 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910021570 Manganese(II) fluoride Inorganic materials 0.000 description 2
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910001632 barium fluoride Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000010216 calcium carbonate Nutrition 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 235000011148 calcium chloride Nutrition 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000001739 density measurement Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- CTNMMTCXUUFYAP-UHFFFAOYSA-L difluoromanganese Chemical compound F[Mn]F CTNMMTCXUUFYAP-UHFFFAOYSA-L 0.000 description 2
- 238000001312 dry etching Methods 0.000 description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000007542 hardness measurement Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000010849 ion bombardment Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Inorganic materials [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- 229910015844 BCl3 Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000012777 commercial manufacturing Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 description 1
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
- C04B35/443—Magnesium aluminate spinel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/162—Magnesium aluminates
-
- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
-
- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
-
- 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
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/76—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by a space-group or by other symmetry indications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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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
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Abstract
Description
本明細書で使用される場合、用語「アルミナ」は、酸化アルミニウム、Al2O3であると理解され、「マグネシア」は、酸化マグネシウム、MgOであると理解される。
開示されるセラミック焼結体は、様々な形状、サイズ、及び様々な材料組成のものであってよい。半導体ウェハ加工に加えて、自動車、航空宇宙、半導体、光学、及び医療などの他の産業、並びに本発明を利用することができる他の製品としては、光学素子、高エネルギーレーザ、極限条件での分光法、半導体チャンバ構成要素、マイクロ機械デバイス、光センサなどの様々な物品が挙げられる。
ドライエッチングプロセスは、業界の標準的装置であるPlasma-Therm Versaline DESC PDC Deep Silicon Etchを用いて行なわれた。エッチングは、2工程プロセスを用いて合計6時間の持続時間で完了した。エッチング方法は、10ミリトルの圧力、600ボルトのバイアス、及び2000ワットのICP出力を用いて行なわれた。エッチング方法は、90標準立方センチメートル/分(sccm)のCF4流量、30標準立方センチメートル/分(sccm)の酸素流量、及び20標準立方センチメートル/分(sccm)のアルゴン流量を用いる第1のエッチング工程と、100標準立方センチメートル/分(sccm)の酸素流量及び20標準立方センチメートル/分(sccm)のアルゴン流量を用いる第2のエッチング工程とを用いて行なわれ、第1及び第2のエッチング工程は、6時間の合計持続時間にわたって各々300秒間繰り返される。
Sa、Sz及びSdrの表面粗さ特徴は、エッチング前のMASセラミック焼結体の研磨された表面にわたってISO規格25178-2-2012に従って測定した。表4の試料B及びC(それぞれ実施例2及び4)に対応する2つのMAS焼結体を、上記の表面粗さ特徴について測定した。表面粗さの測定結果を表5に示す。本明細書に開示されるエッチングプロセスの前に、Saを測定したところ、30nm未満、好ましくは20nm未満、好ましくは2~20nm、好ましくは10~20nm、好ましくは15~20nmであった。Szを測定したところ、20um未満、好ましくは15um未満、好ましくは3~20um、好ましくは3~15umであり、Sdrを測定したところ、5000×10-5未満、好ましくは1000×10-5未満、好ましくは200~5000×10-5、好ましくは300~1000×10-5であった。本明細書で使用される場合、nm及びumは、それぞれ1×10-9m及び1×10-6mを意味する。
6ppmの総不純物に相当する99.9994%の総純度、4~6m2/gの表面積、及び3~4umの平均又はd50粒径を有するマグネシアの粉末を、5ppmの総不純物に相当する99.9995%の総純度、6~8m2/gの表面積、及び2.5~4.5umの平均又はd50粒径を有するアルミナの粉末と組み合わせた。焼結後に立方晶結晶構造を有するスピネルMgAl2O4を形成するために、粉末を相対量で秤量して、マグネシア粉末28.5重量%及びアルミナ粉末71.5重量%の量で粉末混合物を作製した。粉末を、高純度(99.99%)アルミナ媒体及びエタノールとそれぞれ等しい重量で混合して、スラリーを形成した。ボールミル粉砕を150rpmで12時間の持続時間にわたって行ない、ロータリーエバポレーターを用いてスラリーを乾燥させた。粉末混合物を、酸素含有環境中、850℃で4時間、か焼した。か焼された粉末混合物は、任意選択で、か焼後に、当該分野で公知の方法を使用して篩い分けされ得る。X線回折測定の検出限界内で、か焼された粉末混合物は、図2に示すように、酸化マグネシウム及び酸化アルミニウムの存在を示した。か焼された粉末混合物の特性を表2に列挙する。次いで、か焼された粉末混合物を、本明細書に開示される方法に従って、1450℃の温度、20MPaの圧力で30分間、真空下で焼結して、100mmの最大寸法を有する焼結セラミック体を形成した。アルキメデス水浸漬法を使用した密度を測定したところ、3.47g/cc又は理論密度の97%であった。図3は、立方晶結晶構造を有するスピネルを含むセラミック焼結体の形成が確認される、X線回折結果を示す。結晶粒径測定を、ASTM E112-2010に従って行ない、それぞれ4.1um、4.9um及び3.2umの、平均、最大及び最小結晶粒径が、5000倍SEM画像から取った研磨表面にわたって測定された。
出発粉末、ミル粉砕プロセス及びか焼は、実施例1に開示したように行なった。次いで、か焼された粉末混合物を、本明細書に開示される方法に従って、1500℃の温度、20MPaの圧力で30分間、真空下で焼結して、100mmの最大寸法を有する焼結セラミック体を形成した。アルキメデス水浸漬法を使用してセラミック焼結体の密度を測定したところ、3.55g/cc又は理論密度の99.2%であった。ASTM C1327に従って、0.025kgfの適用荷重を使用して、焼結セラミック体に対して硬度測定を行なった。8回の測定にわたって、15.06GPaの平均硬度が0.75の標準偏差で測定された。結晶粒径測定を、ASTM E112-2010に従って行ない、それぞれ8.1um、10.7um及び6.7umの、平均、最大及び最小粒径が、5000倍SEM画像から取った研磨表面にわたって測定された。
出発粉末、ミル粉砕プロセス及びか焼は、実施例1に開示したように行なった。次いで、か焼された粉末混合物を、本明細書に開示される方法に従って、1550℃の温度、20MPaの圧力で30分間、真空下で焼結して、100mmの最大寸法を有する焼結セラミック体を形成した。アルキメデス水浸漬法を使用してセラミック焼結体での密度を測定したところ、3.54g/cc又は理論密度の98.9%であった。
出発粉末、ミル粉砕プロセス及びか焼は、実施例1に開示したように行なった。次いで、か焼された粉末混合物を、本明細書に開示される方法に従って、1600℃の温度、30MPaの圧力で30分間、真空下で焼結して、100mmの最大寸法を有する焼結セラミック体を形成した。アルキメデス水浸漬法を使用してセラミック焼結体での密度を測定したところ、3.57g/cc又は理論密度の99.7%であった。結晶粒径測定を、ASTM E112-2010に従って行ない、それぞれ34um、54um及び32umの、平均、最大及び最小結晶粒径が、5000倍SEM画像から取った研磨表面にわたって測定された。
アルミン酸マグネシウムスピネルを含むセラミック焼結体を、以下に開示されるように製造した。焼結後にスピネル、MgAl2O4を形成するために、マグネシア及びアルミナの高純度の市販の粉末を組み合わせて、28.5重量%のマグネシア粉末及び71.5重量%のアルミナ粉末を含む粉末混合物を形成した。
Claims (40)
- 90~100体積%の立方晶結晶構造及び3.47~3.58g/ccの密度を有する組成MgAl2O4のアルミン酸マグネシウムスピネルを含むセラミック焼結体であって、焼結助剤を含まない、セラミック焼結体。
- 前記焼結助剤が、元素状リチウム及びリチウム化合物を含む、請求項1に記載のセラミック焼結体。
- 3.49~3.58g/ccの密度を有する、請求項1に記載のセラミック焼結体。
- 3.56~3.58g/ccの密度を有する、請求項3に記載のセラミック焼結体。
- 90~99.95体積%の立方晶結晶構造を有する、請求項1に記載のセラミック焼結体。
- 95~99.5体積%の立方晶結晶構造を有する、請求項5に記載のセラミック焼結体。
- 前記セラミック焼結体の99質量%以上で立方晶結晶構造を含む、請求項1に記載のセラミック焼結体。
- ICPMSで測定した99.99%以上の総純度を有する、請求項1~7のいずれか一項に記載のセラミック焼結体。
- ICPMSで測定した99.9975%以上の総純度を有する、請求項8に記載のセラミック焼結体。
- ICPMSで測定した99.9995%以上の総純度を有する、請求項9に記載のセラミック焼結体。
- ICPMSで測定した10ppm以下の総不純物含有量を有する、請求項1~10のいずれか一項に記載のセラミック焼結体。
- ICPMSで測定した5ppm以下の総不純物含有量を有する、請求項11に記載のセラミック焼結体。
- 前記セラミック焼結体が、多結晶である、請求項1~12のいずれか一項に記載のセラミック焼結体。
- 平均結晶粒径が、ASTM E112-2010に従って測定して0.5~20μmである、請求項1~13のいずれか一項に記載のセラミック焼結体。
- 平均結晶粒径が、ASTM E112-2010に従って測定して2~15μmである、請求項14に記載のセラミック焼結体。
- 平均結晶粒径が、ASTM E112-2010に従って測定して3~10μmである、請求項15に記載のセラミック焼結体。
- ASTM C1327に従って0.025kgfの適用荷重を使用して測定して、13.5~16.5GPaの硬度を有する、請求項1~16のいずれか一項に記載のセラミック焼結体。
- ASTM C1327に従って測定して、14.5~15.5GPaの硬度を有する、請求項17に記載のセラミック焼結体。
- 100mm~622mmの最大寸法を有する、請求項1~18のいずれか一項に記載のセラミック焼結体。
- 200mm~622mmの最大寸法を有する、請求項19に記載のセラミック焼結体。
- 最大寸法にわたって測定して、0.2~5%未満の密度分散を有する、請求項19に記載のセラミック焼結体。
- 最大寸法にわたって測定して、0.2~3%の密度分散を有する、請求項21に記載のセラミック焼結体。
- セラミック焼結体の作製方法であって、
a.酸化マグネシウム粉末と酸化アルミニウム粉末とを組み合わせて粉末混合物を作製する工程であって、前記粉末混合物は、99.995%超の総純度を有し、前記粉末混合物は、焼結助剤を含まない、作製する工程と、
b.加熱して前記粉末混合物の温度を600℃~1000℃の温度に上昇させることによって前記粉末混合物をか焼し、か焼温度を4~12時間維持してか焼された粉末混合物を形成する工程と、
c.焼結装置のツールセットによって画定された容積内に前記か焼された粉末混合物を入れて、前記容積内に真空条件を作り出す工程と、
d.1000℃~1700℃の焼結温度に加熱しながら、前記か焼された粉末混合物に5~60MPaの圧力を加えて焼結を行なって前記セラミック焼結体を形成する工程と、
e.前記セラミック焼結体の温度を低下させる工程であって、前記セラミック焼結体は、90~100体積%の立方晶結晶構造及び3.47~3.58g/ccの密度を有する組成MgAl2O4のアルミン酸マグネシウムスピネルを含む、低下させる工程と、
を含む、方法。 - 前記焼結助剤が、元素状リチウム及びリチウム化合物を含む、請求項23に記載の方法。
- 前記ツールセットが、ある容積、内壁、第1及び第2の開口部を有するグラファイトダイと、前記ダイと動作可能に連結された第1及び第2のパンチとを含み、前記第1及び第2のパンチの各々が、前記ダイの前記内壁の直径よりも小さい直径を画定する外壁を有し、それによって、前記第1及び第2のパンチの少なくとも1つが前記ダイの前記容積内で移動するとき、前記第1及び第2のパンチの各々と前記ダイの前記内壁との間にギャップを形成する、請求項23又は24に記載の方法。
- 前記ギャップが、前記ダイの前記内壁と前記第1及び第2のパンチの各々の前記外壁との間の10~100μmの距離である、請求項25に記載の方法。
- 前記焼結温度が、1000~1650℃である、請求項23~26のいずれか一項に記載の方法。
- 前記焼結温度が、1200~1600℃である、請求項27に記載の方法。
- 前記焼結温度に加熱しながら、5~59MPaの圧力を前記か焼された粉末混合物に加える、請求項23~28のいずれか一項に記載の方法。
- 前記圧力が、5~40MPaである、請求項29に記載の方法。
- 前記圧力が、5~20MPaである、請求項29に記載の方法。
- 前記焼結温度に加熱しながら、50MPa未満の圧力を前記か焼された粉末混合物に加える、請求項23~28のいずれか一項に記載の方法。
- 焼結セラミック体が、100mm~622mmの最大寸法を有する、請求項23~32のいずれか一項に記載の方法。
- 焼結セラミック体が、200mm~622mmの最大寸法を有する、請求項33に記載の方法。
- 前記セラミック焼結体が、前記最大寸法にわたって測定して0.2~5%未満の密度分散を有する、請求項23~34のいずれか一項に記載の方法。
- 前記セラミック焼結体が、前記最大寸法にわたって測定して0.2~3%の密度分散を有する、請求項35に記載の方法。
- 前記か焼された粉末混合物が、酸化アルミニウム及び酸化マグネシウムを含む、請求項23~36のいずれか一項に記載の方法。
- f.加熱して前記セラミック焼結体の温度を、アニールを行なうアニール温度に達するまで上昇させることによって前記セラミック焼結体をアニールする工程と、
g.前記アニールしたセラミック焼結体の温度を下げる工程と、
を更に含む、請求項23~37のいずれか一項に記載の方法。 - h.前記セラミック焼結体を機械加工して、立方体、円板、板、リング、シリンダ、湾曲板、管、ドーム、窓、リング、ノズル、チャック、シャワーヘッド、注入器の形状のセラミック焼結体構成要素を作製する工程、
を更に含む、請求項38に記載の方法。 - 請求項23~38のいずれか一項に記載の方法によって作製された、半導体製造チャンバ構成要素を製造するためのセラミック焼結体。
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