CN118103343A - 含铝氮化物陶瓷基质复合物及其制造方法和使用方法 - Google Patents
含铝氮化物陶瓷基质复合物及其制造方法和使用方法 Download PDFInfo
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- CN118103343A CN118103343A CN202280068661.0A CN202280068661A CN118103343A CN 118103343 A CN118103343 A CN 118103343A CN 202280068661 A CN202280068661 A CN 202280068661A CN 118103343 A CN118103343 A CN 118103343A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 139
- 238000000034 method Methods 0.000 title claims abstract description 75
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 41
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 34
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 106
- 239000000203 mixture Substances 0.000 claims abstract description 103
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000002245 particle Substances 0.000 claims abstract description 88
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 4
- 239000011574 phosphorus Substances 0.000 claims abstract description 4
- 239000002775 capsule Substances 0.000 claims description 31
- 239000011248 coating agent Substances 0.000 claims description 31
- 238000000576 coating method Methods 0.000 claims description 31
- 239000011575 calcium Substances 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 25
- -1 amidimide Chemical class 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 229910052712 strontium Inorganic materials 0.000 claims description 18
- 239000008188 pellet Substances 0.000 claims description 17
- 229910052791 calcium Inorganic materials 0.000 claims description 16
- 239000011777 magnesium Substances 0.000 claims description 16
- 229910052727 yttrium Inorganic materials 0.000 claims description 14
- 229910003564 SiAlON Inorganic materials 0.000 claims description 11
- 150000001540 azides Chemical class 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 229910052706 scandium Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- 229910052790 beryllium Inorganic materials 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 7
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 7
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 7
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 150000001408 amides Chemical class 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 6
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 6
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000010937 tungsten Substances 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 238000007606 doctor blade method Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 150000003949 imides Chemical class 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- 241000894007 species Species 0.000 claims description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 238000007650 screen-printing Methods 0.000 claims description 3
- 229910004412 SrSi2 Inorganic materials 0.000 claims description 2
- PQLAYKMGZDUDLQ-UHFFFAOYSA-K aluminium bromide Chemical compound Br[Al](Br)Br PQLAYKMGZDUDLQ-UHFFFAOYSA-K 0.000 claims description 2
- CECABOMBVQNBEC-UHFFFAOYSA-K aluminium iodide Chemical compound I[Al](I)I CECABOMBVQNBEC-UHFFFAOYSA-K 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims 2
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims 2
- 241000237858 Gastropoda Species 0.000 claims 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims 1
- UKFWSNCTAHXBQN-UHFFFAOYSA-N ammonium iodide Chemical compound [NH4+].[I-] UKFWSNCTAHXBQN-UHFFFAOYSA-N 0.000 claims 1
- 150000004678 hydrides Chemical class 0.000 claims 1
- 238000005453 pelletization Methods 0.000 claims 1
- TZLVRPLSVNESQC-UHFFFAOYSA-N potassium azide Chemical compound [K+].[N-]=[N+]=[N-] TZLVRPLSVNESQC-UHFFFAOYSA-N 0.000 claims 1
- 239000002002 slurry Substances 0.000 description 24
- 239000000919 ceramic Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 19
- 239000002131 composite material Substances 0.000 description 18
- 239000011159 matrix material Substances 0.000 description 14
- 238000012545 processing Methods 0.000 description 14
- 229910001220 stainless steel Inorganic materials 0.000 description 14
- 239000010935 stainless steel Substances 0.000 description 14
- 229910045601 alloy Inorganic materials 0.000 description 13
- 239000000956 alloy Substances 0.000 description 13
- 238000010586 diagram Methods 0.000 description 13
- 239000003826 tablet Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 11
- 239000008187 granular material Substances 0.000 description 11
- 239000012212 insulator Substances 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 239000012071 phase Substances 0.000 description 11
- 229910000831 Steel Inorganic materials 0.000 description 10
- 238000009826 distribution Methods 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 9
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- 239000001301 oxygen Substances 0.000 description 9
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000004014 plasticizer Substances 0.000 description 8
- 238000010926 purge Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 235000011089 carbon dioxide Nutrition 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
- 238000003801 milling Methods 0.000 description 6
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 5
- 238000000429 assembly Methods 0.000 description 5
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- 238000002844 melting Methods 0.000 description 5
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- 229910052709 silver Inorganic materials 0.000 description 5
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- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 4
- 150000001342 alkaline earth metals Chemical class 0.000 description 4
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- KCXZNSGUUQJJTR-UHFFFAOYSA-N Di-n-hexyl phthalate Chemical compound CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCC KCXZNSGUUQJJTR-UHFFFAOYSA-N 0.000 description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Chemical compound CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 description 1
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- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- WEAPVABOECTMGR-UHFFFAOYSA-N triethyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCOC(=O)CC(C(=O)OCC)(OC(C)=O)CC(=O)OCC WEAPVABOECTMGR-UHFFFAOYSA-N 0.000 description 1
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- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 1
- 235000013769 triethyl citrate Nutrition 0.000 description 1
- TUUQISRYLMFKOG-UHFFFAOYSA-N trihexyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCOC(=O)CC(C(=O)OCCCCCC)(OC(C)=O)CC(=O)OCCCCCC TUUQISRYLMFKOG-UHFFFAOYSA-N 0.000 description 1
- AMMPRZCMKXDUNE-UHFFFAOYSA-N trihexyl 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCOC(=O)CC(O)(C(=O)OCCCCCC)CC(=O)OCCCCCC AMMPRZCMKXDUNE-UHFFFAOYSA-N 0.000 description 1
- APVVRLGIFCYZHJ-UHFFFAOYSA-N trioctyl 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCCCOC(=O)CC(O)(C(=O)OCCCCCCCC)CC(=O)OCCCCCCCC APVVRLGIFCYZHJ-UHFFFAOYSA-N 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
-
- 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
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本公开的实施方式可以提供一种用于形成含铝的氮化物陶瓷基质复合物的方法,所述方法包括:将生坯、含铝组合物、氨和矿化剂组合物在可密封的容器中加热至在约400摄氏度与约800摄氏度之间的温度和约10MPa与约1000MPa之间的压力,以形成含铝的氮化物陶瓷基质复合物,其特征在于,磷与氮化铝(AlN)的体积比在约1%与约99%之间,孔隙率在约1%与约50%之间,并且热导率在约1瓦/米‑开尔文与约320瓦/米‑开尔文之间。所述生坯体包含磷光体粉末,所述磷光体粉末包含至少一种磷光体组合物,其中所述磷光体粉末粒子的特征在于D50直径在约100纳米与约500微米之间,并且所述生坯的孔隙率在约10%与约80%之间。含铝组合物基于金属计的纯度为约90%至约99.9999%。在所述可密封的容器中加热所述生坯、所述含铝组合物、氨和所述矿化剂组合物之前,所述可密封的容器内的自由体积分数含有在约10%与约95%之间的液氨。
Description
背景技术
技术领域
本公开一般而言涉及用于处理用于制造多晶陶瓷复合物(包括含铝氮化物基质复合物)的材料的技术。更具体地,本公开的实施方式包括用于使用处理技术的组合来制造在含铝氮化物基质中掺入了一种或多种磷光体组合物的陶瓷基质复合物的技术。此类陶瓷基质复合物可用于多种应用,包括用于强光源(例如激光二极管等)的磷光体构件。
背景技术
固态照明在过去二十年中已经取得了巨大的发展,并广泛应用于许多住宅、商业和工业环境中。通常,(例如由发光二极管(LED)发射的)来自蓝色和/或紫色激发源的光被一种或多种磷光体组合物吸收,所述一种或多种磷光体组合物进而发射蓝色、绿色、黄色和/或红色光,从而产生整体白光,所述白光的色温和其他特性(例如显色指数(colorrendition index,CRI))可以控制。最近,激光二极管已被用作激发源,所述激发源提供极高亮度和照度以及非常窄的射束角、更长的投射距离和更高的对比度的能力的优点。然而,为了充分实现基于激光的照明的优点,需要具有非常高的热导率的磷光体组合物,使得由磷光体内的光转换过程生成的热量可以被带走,而不降低磷光体或包装的性能。对于LED,磷光体通常分散在有机硅、环氧树脂或其他具有非常低的热导率的聚合物组合物中。许多小组已经证明玻璃磷光体(phosphor-in-glass,PiG)组合物具有良好的磷光体性能,但这些组合物的热导率仍然相当低。
至少在原则上,陶瓷磷光体组合物对于基于激光的照明来说是理想的。理想地,它应具有高热导率和高内量子效率和外量子效率。然而,目前,发黄光的Ce掺杂的钇铝石榴石(YAG:Ce+3)是唯一广泛商购可得的陶瓷磷光体组合物,而蓝色+YAG白光具有低CRI。几个小组已经展示了陶瓷形式的其他磷光体组合物,其中烧结和致密化已经通过传统方法(例如热压、热等静压和放电等离子体烧结)实现。然而,与这些传统陶瓷处理方法相关联的高温常常会降低磷光体的性能。此外,对于许多应用来说,需要具有彼此紧密接近的多种磷光体组合物,例如绿色磷光体和红色磷光体,并且共烧结涉及除了简单组合物的烧结之外的附加挑战。使用基质可以潜在地克服共烧结中的一些困难,但迄今为止已展示的基质材料在所得陶瓷基质复合物的光学和热性质方面具有重大的局限性。
由于至少上述问题,需要一种具有优异的磷光体性能和高热导率的含磷光体的陶瓷基质复合物。
发明内容
根据本公开,提供了与处理用于制造含铝陶瓷基质复合物的材料的技术相关的另外技术。更具体地,本公开的实施方式包括。
本公开的实施方式还可以提供一种用于形成含铝的氮化物陶瓷基质复合物的方法。所述方法可包括:形成至少一种生坯,所述至少一种生坯包含磷光体粉末和含铝组合物,其中所述至少一种生坯的特征在于孔隙率在约10%与约80%之间;以及将可密封的容器加热至在约400摄氏度与约800摄氏度之间的温度和在约10MPa与约1000MPa之间的压力。在对可密封的容器进行加热和加压之前,将至少一种生坯、氨、和矿化剂组合物设置在所述可密封的容器内。所述磷光体粉末包含至少一种磷光体组合物,所述磷光体粉末粒子的D50直径在约100纳米与约500微米之间。含铝组合物基于金属计的纯度为约90%至约99.9999%。在对可密封的容器进行加热和加压之前,填充有液氨的可密封的容器内的自由体积分数在约10%与约95%之间。加热可密封的容器包括将所述可密封的容器加热达第一时间段以形成含铝的氮化物陶瓷基质复合物,所述含铝的氮化物陶瓷基质复合物的特征在于,磷与AlN的体积比在约1%与约99%之间,孔隙率在约1%与约50%之间,并且热导率在约1瓦/米-开尔文与约320瓦/米-开尔文之间。
本公开的实施方式还可以提供一种含铝组合物。所述含铝组合物包含含铝的氮化物基质材料和多个二次陶瓷相粒子。所述多个二次陶瓷相粒子的特征在于具有在约1微米与约10微米之间的D10值和在约10微米与约100微米之间的D90值的粒径分布。所述含铝组合物还包括:与含铝基质材料结合的多个二次陶瓷相粒子的边界的至少50%;在约1%与约99%之间的多个二次陶瓷相粒子与含铝基质材料的比率;并且所述含铝组合物的特征在于孔隙率在约1%与约50%之间并且热导率在约1瓦/米-开尔文与约320瓦/米-开尔文之间。所述多个二次陶瓷相粒子还可包含至少一种磷光体组合物。所述多个二次陶瓷相粒子还可包含至少两种磷光体组合物。在一些实施方式中,所述含铝组合物的特征还可在于,所述多个二次陶瓷相粒子与所述含铝基质材料的比率在约5%与约95%之间,孔隙率在约2%与约50%之间,并且热导率在约5瓦/米-开尔文与约260瓦/米-开尔文之间。所述磷光体组合物还可包含以下中的至少一者:Y3Al5O12:Ce3+、Lu3Al5O12:Ce3+、(Y,Gd,Tb,Sc,Lu,La)3(Al,Ga,In)5O12:Ce3+、β-SiAlON:Eu2+、α-SiAlON:Eu2+和CaAlSiN3:Eu2+。在一些实施方式中,所述含铝组合物的经抛光区段的二次电子显微照片揭露在所述多个二次陶瓷相粒子与所述含铝基质材料之间的边界的至少50%内没有可观察到的间隙。
本公开的本质和优点的进一步理解可通过参考说明书和附图来进一步理解。
附图说明
以能够详细理解本公开的上述特征的方式,以上简要概括的本公开的更具体描述可以通过参考实施方式来获得,所述实施方式中一些实施方式在附图中示出。然而,要注意的是,附图仅示出示例性实施方式,因此不应被视为对实施方式的范围的限制,并且可以承认其他同等有效的实施方式。
图1A是示出根据本公开的实施方式的多个具有涂层的磷光体粒子的简化图。
图1B是示出磷光体粒子和含铝粒子的混合物的简化图。
图2A是示出根据本公开的实施方式的用于对浆料组合物进行流延成型的工艺流程的简化图。
图2B是示出根据本公开的实施方式的使用刮刀刀片和镂空掩模来对浆料组合物进行流延成型的工艺流程的简化图。
图2C是根据本公开的实施方式的图2A所示的流延成型装置的刮刀刀片部分和镂空掩模部分的平面图。
图3A和图3B是示出根据本公开的实施方式的形成经浸润的复合物组合物的方法的简化图。
图4A和图4B是示出根据本公开的实施方式的形成经浸润的复合物组合物的替代方法的简化图。
图5A是示出根据本公开的实施方式的用于通过压片方法形成生坯的工艺流程的简化图。
图5B是示出根据本公开的实施方式的使用喷雾干燥机由浆料形成混合干粉组合物的工艺流程的简化图。
图5C是根据本公开的实施方式的用于形成片剂的输送机系统的简化图。
图6是示出根据本公开的实施方式的容纳有颗粒体、丸粒、片剂或其他生坯形式的可密封的容器的剖视图的简化图。
图7是示出根据本公开的实施方式的压力容器设备的示意图。
图8是示出根据本公开的实施方式的内热式压力容器、设备的示意图。
图9是示出根据本公开的实施方式的矿化剂容器及其使用方法的示意图。
为了便于理解,在可能的情况下已经使用相同的附图标记来表示附图中共有的相同元件。可以设想,一个实施方案的元件和特征可以有益地结合到其他实施方案中而无需进一步叙述。
具体实施方式
根据本公开,提供了与处理用于制造含铝的氮化物陶瓷基质复合物的材料的技术相关的技术。所述含铝的氮化物陶瓷基质复合物将掺入的粒子(例如磷光体粒子)的功能性与半透明光学性状和高热导率相结合。
图1A和图1B是示出克服上述限制的含铝的氮化物陶瓷基质复合物制造方法内的工艺步骤的示意性剖视图。参考图1A和图1B,提供了多个磷光体粒子101。在某些实施方式中,磷光体粒子101选自一种或多种具有在蓝色区域(430-490nm)、绿色区域(490-560nm)、黄色区域(560-600nm)、或红色区域(600-750nm)中的发射波长的组合物。
在一个具体实施方式中,所述磷光体粒子101包含一种或多种材料组合物,所述一种或多种材料组合物可包含Y3Al5O12:Ce3+、Lu3Al5O12:Ce3+、(Y,Gd,Tb,Sc,Lu,La)3(Al,Ga,In)5O12:Ce3+、β-SiAlON:Eu2+、α-SiAlON:Eu2+、SrSi2O2N2:Eu2+、SrGa2S4:Eu2+、SrS:Eu2+和CaAlSiN3:Eu2+。
在某些实施方式中,所述多个磷光体粒子101可包含能够发射基本上红光的磷光体。这种磷光体可以选自可包含:以下中的一者或多者的材料组合物:CaAlSiN3:Eu2+、(Gd,Y,Lu,La)2O3:Eu3+,Bi3+;(Gd,Y,Lu,La)2O2S:Eu3+,Bi3+;(Gd,Y,Lu,La)VO4:Eu3+,Bi3+;Y2(O,S)3:Eu3 +;Ca1-xMo1-ySiyO4:其中0.05≦x≦0.5,0≦y≦0.1;(Li,Na,K)5Eu(W,Mo)O4;(Ca,Sr)S:Eu2+;SrY2S4:Eu2+;CaLa2S4:Ce3+;(Ca,Sr)S:Eu2+;3.5MgO*0.5MgF2*GeO2:Mn4+(MFG);(Ba,Sr,Ca)MgxP2O7:Eu2+,Mn2+;(Y,Lu)2WO6:Eu3+,Mo6+;(Ba,Sr,Ca)3MgxSi2O8:Eu2+,Mn2+,其中1<x≦2;(RE1-yCey)Mg2-xLixSi3-xPxO12,其中RE是Sc、Lu、Gd、Y、和Tb中的至少一者,0.0001<x<0.1并且0.001<y<0.1;(Y,Gd,Lu,La)2-xEuxW1-yMoyO6,其中0.5≦x≦1.0,0.01≦y≦1.0;(SrCa)1- xEuxSi5N8,其中0.01≦x≦0.3;SrZnO2:Sm+3;MmOnX,其中M选自由以下组成的组:Sc、Y、镧系元素、碱土金属以及它们的混合物;X是卤素;1≦m≦3;并且1≦n≦4,并且其中镧系元素掺杂水平的范围可以在0.1%至40%光谱权重的范围内;以及Eu3+活化的磷酸盐或硼酸盐磷光体;以及它们的混合物。
在某些实施方式中,磷光体粒子101包含蓝色磷光体组合物,所述蓝色磷光体组合物包含以下中的一者或多者:α-SiAlON:Eu2+、(Ba,Sr,Ca)5(PO4)3(Cl,F,Br,OH):Eu2+,Mn2+;Sb3+,(Ba,Sr,Ca)MgAl10O17:Eu2+,Mn2+;(Ba,Sr,Ca)BPO5:Eu2+,Mn2+;(Sr,Ca)10(PO4)6*nB2O3:Eu2+;2SrO*0.84P2O5*0.16B2O3:Eu2+;Sr2Si3O8*2SrCl2:Eu2+;(Ba,Sr,Ca)MgxP2O7:Eu2+,Mn2+;Sr4Al14O25:Eu2+(SAE);BaAl8O13:Eu2+;以及它们的混合物。
在某些实施方式中,磷光体粒子101包含绿色磷光体组合物,所述绿色磷光体组合物包含以下中的一者或多者:β-SiAlON:Eu2+、(Ba,Sr,Ca)MgAl10O17:Eu2+,Mn2+(BAMn);(Ba,Sr,Ca)Al2O4:Eu2+;(Y,Gd,Lu,Sc,La)BO3:Ce3+,Tb3+;Ca8Mg(SiO4)4Cl2:Eu2+,Mn2+;(Ba,Sr,Ca)2SiO4:Eu2+;(Ba,Sr,Ca)2(Mg,Zn)Si2O7:Eu2+;(Sr,Ca,Ba)(Al,Ga,In)2S4:Eu2+;(Y,Gd,Tb,La,Sm,Pr,Lu)3(Al,Ga)5O12:Ce3+;(Ca,Sr)8(Mg,Zn)(SiO4)4Cl2:Eu2+,Mn2+(CASI);Na2Gd2B2O7:Ce3 +,Tb3+;(Ba,Sr)2(Ca,Mg,Zn)B2O6:K,Ce,Tb;以及它们的混合物。
在某些实施方式中,磷光体粒子101的直径或大小在约1纳米与约1毫米之间、在约100纳米与约500微米之间、在约1微米与约200微米之间、在约1.5微米与约100微米之间,或在约2微米与约50微米之间。通常,粒子将不是球形的,并且如本文所用的术语“直径”是指与粒子具有相同体积的球体的直径。在某些实施方式中,磷光体粒子101的特征在于具有在约1微米与约10微米之间的D10值和在约10微米与约100微米之间的D90值的粒径分布。粒径分布可以通过本领域已知的各种方法测量,所述方法为例如激光衍射、动态光散射、动态图像分析、筛分分析、光学计数、电阻计数、沉降、声谱学、激光遮蔽时间等。就累积粒径分布而言,量D10、D50和D90分别是指这样的直径,在所述直径时10%的粒子体积、50%的粒子体积或90%的粒子体积的直径小于或等于规定值。在这个术语中,我们称为D10、D50和D90的量有时分别称为Dv10、Dv50和Dv90。
再次参考图1A,在某些实施方式中,磷光体粒子101可以涂覆有含铝涂层103。在某些实施方式中,含铝涂层103的厚度在约10纳米与约100微米之间、在约100纳米与约25微米之间、在约150纳米与约10微米之间、或在约0.25微米与约5微米之间。在某些实施方式中,含铝涂层103通过物理气相沉积(physical vapor deposition,PVD)方法(例如热蒸发、电子束蒸发、或溅射)沉积。在某些实施方式中,含铝涂层103通过化学气相沉积(chemicalvapor deposition,CVD)沉积。在某些实施方式中,含铝涂层103还包含其他组分,例如吸气剂组合物,所述吸气剂组合物包含以下中的一者或多者:铍、镁、钙、锶、钡、钪、钛、钒、铬、钇、锆、铌、稀土金属、铪、钽、和钨。在具体实施方式中,含铝涂层103还包含铍、镁、钪或钇中的一者或多者。在此上下文中,吸气剂是指对氧的亲和力高于对铝的亲和力的组合物。氧化铝在铝金属的表面上形成高度稳定的钝化膜,所述钝化膜可对氮化铝的形成有害,并且吸气剂的存在可以通过优先与可用氧结合并由此减少在处理期间在铝金属的表面上形成的氧化物的浓度来抑制氧化铝的形成。在优选的实施方式中,吸气剂材料的氧化物具有高热导率,氧化铍是突出的示例。
在某些实施方式中,在正在例如振动台上沉积含铝涂层103的同时,在表面上搅动磷光体粒子101。在某些实施方式中,在正在沉积含铝涂层103的同时,磷光体粒子101处于流化床中。在某些实施方式中,含氮气体在含铝涂层103的沉积期间存在。在某些实施方式中,含氮气体包含或由氨或N2组成。
再次参考图1B,在某些实施方式中,将磷光体粒子101与含铝粒子105混合。可用于形成下文进一步讨论的含铝生坯的粒子的混合可促进在磷光体粒子周围形成具有高热导率的含铝氮化物基质。含铝粒子105可包含或由以下物质组成:氮化铝粉末、氮化铝砂粒、铝粉、铝片、铝丸粒、铝刨花、铝砂粒、铝蒸发料块(aluminum evaporation slug)等。含铝粒子105的最小尺寸可在约10毫米与约1微米之间、在约5毫米与约2微米之间、在约2毫米与约5微米之间、在约1毫米与约10微米之间、或在约500微米与约20微米之间。较大大小的含铝粒子105可能更难以与磷光体粒子101混合,但可能具有与降低的氧含量相关联的优点,这可以使得能够在最终陶瓷基质复合物中实现更高的热导率和改善的半透明度。磷光体粒子101与含铝粒子105的体积比可以在约1%与约99%之间、在约5%与约95%之间、在约10%与约90%之间、或在约20%与约80%之间。在某些实施方式中,将磷光体粒子101与含铝粒子105在球磨机、磨碎机、气流粉碎机等中混合。在某些实施方式中,研磨介质(例如Si3N4、SiC、ZrO2、或AlN)在混合操作期间存在,并且可以在研磨已经完成时从混合物中分离。在某些实施方式中,研磨过程在干燥氮气气氛下执行。在某些实施方式中,采用保护气体。在某些实施方式中,研磨操作期间存在的气氛包括或由氨组成。在研磨过程期间,磷光体粒子101的至少一部分与含铝粒子105之间可能发生机械结合。
在某些实施方式中,将附加的粉末组分与磷光体粒子101混合。在某些实施方式中,可将吸气剂组合物与磷光体粒子101混合,所述磷光体粒子为例如以下中的一者或多者:铍、镁、钙、锶、钡、钪、钛、钒、铬、钇、锆、铌、稀土金属、铪、钽和钨,以及它们的氮化物、氮氧化物、酰胺、酰亚胺、酰胺基酰亚胺、卤化物或卤氧化物。在具体实施方式中,吸气剂组合物包含铍、镁、钪和钇中的一者或多者。在某些实施方式中,吸气剂组合物作为杂质包含在含铝粒子105中。在某些实施方式中,含铝粒子105包含或由合金组成,所述合金具有在约0.1%与约20%之间或在约1%与约10%之间的吸气剂组合物以及在约80%与约99.9%之间或在约90%与99%之间的铝。
在某些实施方式中,将磷光体粒子101混合并分散在浆料201中作为处理系统200的一部分,如图2A中示意性所示。所述处理系统200包括混合部件251和生坯形成组件255。所述混合部件251可以包括混合装置253、浆料罐254、均质化装置259和泵260。生坯形成组件255可以包括载体膜进给组件261,所述载体膜进给组件具有载体膜进给卷盘211、输入罐265、刮刀刀片266、加热装置267、生坯卷取卷盘213、和载体膜卷取卷盘212。在一些实施方式中,所述浆料包含水。在某些实施方式中,所述浆料包含极性非质子溶剂。在某些实施方式中,浆料基本上不含水并且包含脂肪族溶剂(例如二乙胺)或芳族溶剂(例如苯胺)。避免水和质子溶剂可能有助于最小化磷光体粒子101、含铝涂层103、和含铝粒子105(如果存在的话)的表面上Al2O3和其他氧化物的形成。在某些实施方式中,所述浆料包含本领域已知的粘合剂、润滑剂、润湿剂、增塑剂、分散剂、抗絮凝剂、其他添加剂等中的一者或多者。在某些实施方式中,所述浆料包含蜡组合物和尿素中的一者或多者。
可作为浆料或干混粉末的组分用于制造含铝的氮化物陶瓷基质复合物的有机粘合剂包括但不限于乙烯基聚合物,例如但不限于聚乙烯醇缩丁醛(PVB)、聚乙烯醇(PVA)、聚氯乙烯(PVC)、聚乙酸乙烯酯(PVAc)、聚丙烯腈、它们的混合物和它们的共聚物、聚乙烯亚胺、聚甲基丙烯酸甲酯(PMMA)、氯乙烯-乙酸酯以及它们的混合物,优选地PVB。可用于制造含铝的陶瓷基质复合物的增塑剂包括但不限于邻苯二甲酸丁基苄酯、基于二羧酸/三羧酸酯的增塑剂,例如但不限于基于邻苯二甲酸酯的增塑剂,例如但不限于邻苯二甲酸双(2-乙基己基)酯、邻苯二甲酸二异壬酯、邻苯二甲酸双(正丁基)酯、邻苯二甲酸丁基苄酯、邻苯二甲酸二异癸酯、邻苯二甲酸二正辛酯、邻苯二甲酸二异辛酯、邻苯二甲酸二乙酯、邻苯二甲酸二异丁酯、邻苯二甲酸二正己酯以及它们的混合物;基于己二酸酯的增塑剂,例如但不限于己二酸双(2-乙基己基)酯、己二酸二甲酯、己二酸单甲酯、己二酸二辛酯以及它们的混合物;基于癸二酸酯的增塑剂,例如但不限于癸二酸二丁酯;和马来酸酯型增塑剂,例如但不限于马来酸二丁酯、马来酸二异丁酯以及它们的混合物;聚亚烷基二醇类,例如但不限于聚乙二醇、聚丙二醇以及它们的混合物。可以使用的其他增塑剂包括但不限于苯甲酸盐;环氧化植物油;磺酰胺类,例如但不限于N-乙基甲苯磺酰胺、N-(2-羟丙基)苯磺酰胺、和N-(正丁基)苯磺酰胺;有机磷酸酯,例如但不限于磷酸三甲苯酯和磷酸三丁酯;二醇/聚醚,例如但不限于三甘醇二己酸酯、四甘醇二庚酸酯以及它们的混合物;柠檬酸烷基酯,例如但不限于柠檬酸三乙酯、乙酰基柠檬酸三乙酯、柠檬酸三丁酯、乙酰基柠檬酸三丁酯、柠檬酸三辛酯、乙酰基柠檬酸三辛酯、柠檬酸三己酯、乙酰基柠檬酸三己酯、丁酰基柠檬酸三己酯、和柠檬酸三甲酯;以及烷基磺酸苯酯,以及它们的混合物。
可用于形成浆料或干混粉末的分散剂包括但不限于氧化鲱鱼油(Menhaden fishoil,MFO)、二羧酸(例如琥珀酸、乙二酸、丙二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸)、脱水山梨糖醇单油酸酯、邻苯二甲酸、对苯二甲酸,以及它们的混合物。
在某些实施方式中,如图2A、图2B和图2C所示,使用流延成型或刮刀刀片技术将包含磷光体粒子101和/或含铝粒子105的浆料201流延成型到柔性载体膜上,以通过使用处理系统200内的部件在载体膜202上形成生坯290。在一个示例中,所述生坯290可以形成为接收在卷取卷盘213上的连续材料卷,所述连续材料卷在本文中被称为生坯290A;或者形成为多个生坯盘290B,如图2B和图2C所示。载体膜202从载体膜进给组件261的进给卷盘211进给到卷取卷盘212。在某些实施方式中,载体膜202包含或由MylarTM组成。在某些实施方式中,载体膜202包含或由不锈钢或熔点高于约600摄氏度或高于约660摄氏度的金属组合物组成。在某些实施方式中,载体膜202包括含铝箔或涂层。在某些实施方式中,含铝箔或涂层还包含浓度在约0.1%与约20%之间或约1%与约10%之间的吸气剂组合物。
在某些实施方式中,具有施加的浆料层的载体膜经历干燥过程以形成生坯290。在某些实施方式中,用已干燥的所施加的浆料层302将含铝层303沉积在载体膜202上,如图3A示意性所示。在某些实施方式中,将具有含铝涂层303和/或包含含铝粒子105的干燥浆料层加热至高于660摄氏度的温度,例如加热至在约660摄氏度与约900摄氏度之间,或在约675摄氏度与约750摄氏度之间的温度,从而导致含铝层303和/或含铝涂层103和/或含铝粒子105熔化并通过毛细作用被吸入并遍及干燥浆料层,从而形成含铝涂层355和含铝复合物359,如图3B示意性所示。在某些实施方式中,熔化和浸润过程在真空中,在低于约10-2托、低于约10-3托、低于约10-4托、低于约10-5托、低于约10-6托、低于约10-7托或低于约10-8托的压力下执行。在某些实施方式中,熔化和浸润过程在含氮气氛(例如N2或NH3)下或在基本上不含氧气和水的惰性气氛(例如Ar)下执行。在某些实施方式中,孔隙357存在于复合主体内。孔隙357的存在可以通过以下方式来促进复合主体的后续氮化过程:提供孔隙网络,所述孔隙网络允许含氮物质(例如,氨)在处理期间到达复合主体内暴露的含铝表面。
在某些实施方式中,含铝箔或涂层402存在于载体膜202上且位于干燥浆料层403下方,如图4A中示意性所示。在某些实施方式中,将载体膜202和干燥浆料层403加热至高于600摄氏度的温度,例如,加热至在约660摄氏度与约900摄氏度之间、或在约675摄氏度与约750摄氏度之间的温度,从而使含铝箔或涂层402熔化并通过毛细作用被吸入干燥浆料层中,从而形成含铝涂层355和含铝复合物359,如图4B示意性所示。在某些实施方式中,熔化和浸润过程在真空中,在低于约10-2托、低于约10-3托、低于约10-4托、低于约10-5托、低于约10-6托、低于约10-7托或低于约10-8托的压力下执行。在某些实施方式中,熔化和浸润过程在含氮气氛(例如N2或NH3)下或在基本上不含氧气和水的惰性气氛(例如Ar)下执行。在某些实施方式中,孔隙357存在于复合主体内。
再次参考图2A,在一些实施方式中,在形成生坯290A(例如经铝浸润的复合生坯)之后,可以将生坯从载体膜202剥离并收集在卷取卷盘212上以用于进一步处理。生坯290的特征可在于孔隙率在约10%与约80%之间、或在约20%与约60%之间。较低水平的孔隙率可能有助于提高氮化后含铝的氮化物基质复合物的热导率,但是较高水平的孔隙率可借助于在后续处理期间更易获得氨而促进氮化过程本身。
在某些实施方式中,如图2B所示,使用流延成型或刮刀刀片技术将浆料201丝网印刷或流延成型到覆盖有镂空掩模271的柔性载体膜202上。在某些实施方式中,镂空掩模271由聚合物(例如MylarTM或有机硅)制成。在其他实施方式中,镂空掩模271由金属或金属合金(例如不锈钢)制成。在某些实施方式中,镂空掩模271具有在镂空掩模271的表面上布置成正方形或六边形阵列的开口272。在某些实施方式中,镂空掩模271中的开口272是圆形的并且直径在约50微米与约100毫米之间、在约200微米与约50毫米之间、在约500微米与约20毫米之间、或在约1毫米与约10毫米之间。在某些实施方式中,镂空掩模271的厚度(即,图2B中的竖直方向)在约10微米与约1毫米之间、在约20微米与约500微米之间、或在约50微米与约200微米之间。在某些实施方式中,提供固定件,使得在刮刀刀片266已将浆料201的组合物施加到镂空掩模271中的开口272中之后,镂空掩模271与载体膜202分离,从而在载体膜202上留下离散的生坯盘290B,如图2B的左侧示意性所示。
在某些实施方式中,不是如图2A、图2B和图2C中示意性所示通过流延成型形成生坯290,例如连续生坯膜290A(图2A)或生坯盘290B(图2B),而是包含磷光体粒子101的生坯可以通过使用利用压片系统500的造粒和/或压片工艺来形成,如图5A示意性所示。具有或不具有含铝涂层103和/或含铝粒子105的磷光体粒子101可以通过使用材料进料器501并使用如本领域已知的一个或多个混合和压实部件505来与粘合剂、润滑剂、润湿剂、分散剂、抗絮凝剂、其他添加剂等中的一者或多者一起混合。在某些实施方式中,所述混合物包含蜡组合物和尿素中的一者或多者。在某些实施方式中,所述混合物还可包括一些液体组分。在某些实施方式中,避免质子组分,例如聚乙烯醇和乙二醇,可能有助于最小化磷光体粒子101和含铝涂层103和含铝粒子105的表面上Al2O3和其他氧化物的形成。在某些实施方式中,使用V型掺混机、粉末混合机等执行混合过程。混合粉末可以通过辊压形成颗粒体,从而形成带状物,或者通过使用压片装置551形成近似球形的颗粒体。在某些实施方式中,通过研磨工艺将带状物研磨成颗粒体。
在某些实施方式中,如图5B示意性所示,将含有磷光体粒子101的浆料以浆料形式混合,然后通过使用喷雾干燥工艺干燥成粉末(即,粉末产品)。可以将混合粉末压实成颗粒体等,所述混合粉末中可能添加附加的组分,例如粘合剂、润滑剂、润湿剂、分散剂、抗絮凝剂、其他添加剂等中的一者或多者。
可将颗粒体549进给到压片机551中,并通过本领域中已知的方法单轴压制成片剂,如图5C中示意性所示。一片或多片刮刀刀片266可将颗粒体549引导到模腔547中。上活塞533可以由上凸轮543向下推动,并且下活塞531可以由下凸轮541向上推动,从而导致片剂535的形成,然后所述片剂可以被喷射出。
在某些实施方式中,如本领域中已知,通过使用盘式造粒机将混合粉末形成为丸粒。所述丸粒可以或可以不通过压片工艺进一步致密化。在某些实施方式中,通过干燥操作去除颗粒体、丸粒或片剂中的挥发性组分。
在某些实施方式中,通过蒸发和加热用含铝组合物浸润颗粒体、丸粒或片剂,如图3A和图3B中示意性所示。在某些实施方式中,通过以下方式用含铝组合物浸润颗粒体、丸粒或片剂:放置成与箔或涂层接触并加热,如图4A和图4B中示意性所示。
其他方法也可以用于将磷光体粒子101掺入到含铝生坯中,包括注浆成型、单轴压制、等静压制、和丝网印刷。
在某些实施方式中,颗粒体、丸粒、片剂、或流延成型生坯内的含铝涂层或粒子组合物的纯度基于金属计在99.9999%与90%之间、在99.9%与95%之间、在99.8%与97%之间、或在99.5%与98%之间。在某些实施方式中,含铝涂层或粒子组合物含有Fe和/或Si作为杂质,例如浓度在按重量计约1ppm(part per million)与约10%之间、或约10ppm与约1%之间。
含铝生坯609,无论是颗粒体、丸粒、片剂、轧制膜还是其他形式,都然后放置在可密封的容器600的内部621内,如图6所示。可密封的容器600可包括或由胶囊、高压釜或高压釜内的衬里组成。所述胶囊或内衬可以由以下组成或包含以下中的至少一者:银、基于银的合金、铜、基于铜的合金、金、钯、铂、铱、钌、铑、钛、铁、基于铁的合金、不锈钢、镍、基于镍的合金、锆、铌、钼、钽、它们的组合等。可密封的容器可以包括填充导管或上入口623和下入口625中的一者或多者。
可以将至少一种矿化剂组合物添加到可密封的容器中。所述矿化剂组合物可以由以下物质组成或包含以下物质:碱金属(例如Li、Na、K、Rb、或Cs)、碱土金属(例如Be、Mg、Ca、Sr、或Ba)、或碱金属或碱土金属的氢化物、酰胺、酰亚胺、酰胺-酰亚胺、氮化物、或叠氮化物。矿化剂可以由以下物质组成或包含以下物质:卤化铵(例如NH4F、NH4Cl、NH4Br、或NH4I)、卤化铝(例如AlF3、AlCl3、AlBr3、AlI3)、或任何可以通过F、Cl、Br、I、HF、HCl、HBr、HI、Al、AlN和NH3中的两者或更多者的反应形成的化合物。矿化剂可以由以下物质组成或包含以下物质:其他碱金属盐、碱土金属盐或铵盐、其他卤化物、尿素、硫或硫化物盐、或者磷或含磷盐。在具体实施方式中,矿化剂包含或由KN3和NaN3中的至少一者组成,并且基本上不含水分。
在矿化剂基本上不含卤素Cl、Br和I的情况下,银可以很好地用作可密封的容器600的构造材料。然而,当Cl、Br和I中至少一者以显著浓度存在时,金、铂或铂/铱可能是更好的选择。
也可以将吸气剂添加到可密封的容器600中。吸气剂优先与处理区域621中存在的残余或外来氧或湿气(包括可能存在于磷光体粒子和/或含铝涂料组合物的表面处的氧)反应,从而改善含铝的氮化物陶瓷基质复合物的纯度、热导率和半透明度。合适的吸气剂的示例包含铍、镁、钙、锶、钡、钪、钛、钒、铬、钇、锆、铌、稀土金属、铪、钽和钨,以及它们的氮化物、氮氧化物、酰胺、酰亚胺、酰胺基酰亚胺、卤化物、或卤氧化物。在具体实施方式中,吸气剂包含Be、Mg、Ca、Ba、Y或它们的氮化物中的至少一者。在优选实施方式中,在吸气过程期间形成的吸气剂氧化物(例如BeO、MgO、CaO、或Y2O3)的特征在于高热导率,例如高于约10W/m-K、高于约20W/m-K、高于约40W/m-K、或高于约100W/m-K。
在具体实施方式中,以预定比率提供叠氮化物矿化剂和含铝涂层或粒子组合物加任选的附加金属(例如金属形式的吸气剂)例如作为含铝合金的组分,使得由叠氮化物矿化剂分解生成的氮气与由至少金属与超临界氨反应生成的氢气物质的比率为约1:3。例如,在氨热反应条件下,铝和其他金属(如果存在的话)将经历以下反应中的一者或多者:
Al+NH3=AlN+3/2H2
Na+NH3=NaNH2+1/2H2
K+NH3=KNH2+1/2H2
3Be+2NH3=Be3N2+3/2H2
3Mg+2NH3=Mg3N2+3/2H2
3Ca+2NH3=Ca3N2+3/2H2
Ca+2NH3=Ca(NH2)2+H2
Y+3NH3=Y(NH2)3+3/2H2
Y+NH3=YN+3/2H2
使用叠氮化物作为矿化剂是方便的,因为它们往往以高纯度商购可得,可以进一步纯化,并且比例如碱金属或酰胺或碱土金属氮化物吸湿性低得多。然而,叠氮化物通常在反应条件下分解,从而产生氮气:
3KN3+2NH3=3KNH2+4N2。
在优选实施方式中,这两种效应,即通过金属与氨反应形成氢和通过叠氮化物分解形成氮气,经组合以相互抵消。将包括含铝涂层和/或粒子组合物、矿化剂和吸气剂在内的金属与叠氮化物矿化剂前体一起添加,使得以大约3:1的比率生成H2和N2。可密封的容器可进一步包括用于催化由H2和N2形成NH3的装置。催化金属与氨的反应和叠氮化物的分解中分别释放的H2与N2之间的反应以重新形成氨可以通过可密封的容器的壁或通过也提供在可密封的容器内的催化剂来执行。所添加的催化剂可以包括粉末、颗粒体、箔、涂层、散装材料、或多孔丸粒。所添加的催化剂可包含或由以下中的至少一者组成:铁、钴、镍、钛、钼、钨、铝、钾、铯、钙、镁、钡、锆、锇、铀或镧、钌、铂、钯、或铑。在具体示例中,所添加的催化剂包含或由海绵状钌组成。例如,一摩尔所添加的KN3矿化剂将生成4/3摩尔的N2,与此同时转化为KNH2。氮气生成可以通过以下方式来抗衡:还添加8/3摩尔的Al和/或另一种金属,这将生成8/3×3/2摩尔=4摩尔的H2,即来自KN3的N2的摩尔数的三倍。
然后除了与流体歧管的一个或多个连接部之外,封闭并密封可密封的容器600,所述流体歧管包括气体、液体或真空歧管中的至少一者。然后可将可密封的容器抽真空,以去除空气、湿气、和其他挥发性污染物。在一些实施方式中,将可密封的容器600在抽空期间加热至在约25摄氏度与约500摄氏度之间的温度。在一些实施方式中,使可密封的容器经历至少两次、至少三次、至少给定或至少十次抽空循环,然后用惰性气体(例如氩气或氮气)回填。在某些实施方式中,再次参考图6,可密封的容器设置有至少一个可用作气相入口的下部入口625和可用作气相出口的上部入口623,使得可密封的容器可以通过连续的气流吹扫。由于通过管道到可密封的容器的内部的传导性有限,所以相对于抽空,吹扫可提供空气、湿气和其他挥发性污染物的更好去除。可以通过使吹扫气体从可密封的容器的内部体积的一个端部流到另一端部来增强吹扫效率。根据具体实施方式,可密封的容器可借助于至少一根填充导管或净化导管联接至流体歧管内的气体源,优选地不将可密封的容器的内容物暴露于空气。气体源可尤其包含氮气、氩气、氢气、氦气和氨中的至少一者。用于吹扫可密封的容器的布置的进一步细节在美国专利8,444,765中描述,该专利据此全文以引用方式并入。
在某些实施方式中,如图3B或图4B中示意性所示将含铝组合物浸润到含磷光体的颗粒体、丸粒、片剂或流延成型膜中可以在可密封的容器内在真空下或者在正在用惰性气体(例如氩气)或含氮气体(例如氮气或氨)吹扫可密封的容器的同时,例如在约660摄氏度与约750摄氏度之间的温度下原位执行。
在完成泵吹扫和/或流吹扫过程之后,可将可密封的容器600冷却并填充氨至指定水平。在某些实施方式中,将可密封的容器600冷却至干冰温度,例如通过浸没在干冰溶剂浴中或通过使用热交换器,并且使受控量的气态氨从流体歧管流入可密封的容器中并冷凝成液相。在其他实施方式中,使受控量的液氨在来自流体歧管中的泵送流体组件的升高的压力下(例如高于大约七个大气压下)流入可密封的容器600。
在某些实施方式中,将矿化剂与例如溶液中的液氨一起添加到可密封的容器600中。例如,参见图9,矿化剂组合物可以经称重并添加到手套箱(未示出)内的矿化剂容器951中,并且可以将矿化剂容器951密封并从手套箱中取出。矿化剂容器951和冲洗容器953可以附接至氨歧管961。当阀955和957打开时,可将矿化剂容器951冷却至干冰温度并用预定量的氨填充。然后,在阀957打开且阀955关闭时,可将冲洗容器953冷却并用预定量的氨填充。当阀957关闭时,可使冲洗容器953和矿化剂容器951与氨歧管断开连接并加热至室温,从而在矿化剂容器951内生成矿化剂的氨溶液,并将所述冲洗容器和矿化剂容器连接到已预先抽空的可密封的容器600。然后可以打开阀959以及矿化剂容器951与可密封的容器600之间的任何附加阀,从而使液氨矿化剂溶液注入可密封的容器600中。如果需要的话,可冷却可密封的容器600,或者将矿化剂容器951加热例如5摄氏度至25摄氏度以使液氨的最后残留物被转移到可密封的容器600中。然后可以关闭阀959并打开阀955,从而使氨从冲洗容器953转移到矿化剂容器951中。如果需要的话,可以将矿化剂容器951冷却,或将冲洗容器953加热例如5摄氏度至25摄氏度,以使最后残留的液氨从冲洗容器953转移至矿化剂容器951。矿化剂容器951可以加热至室温,从而使在第一次氨从矿化剂容器951至可密封的容器600的转移留下的任何痕量矿化剂重新溶解。然后可以打开阀959,以及在矿化剂容器951与可密封的容器600之间的任何附加阀(例如,V4和FV),从而导致具有痕量的溶解的矿化剂的液氨被注入可密封的容器600中。此过程可以根据需要重复附加次数。如上所述,可以将附加的氨添加到可密封的容器600中。在处理之后,任何残留的氨可以通过出口965排空。
可密封的容器600内填充有液氨的自由体积分数可以在约10%与约95%之间、在约20%与约90%之间、在约30%与约80%之间、或在约40%与约70%之间。在将所需量的氨添加到可密封的容器600中之后,可关闭并密封所述可密封的容器600。密封过程可以包括以下中的一者或多者:关闭阀门、超声波焊接填充导管(例如上入口623和/或下入口625)、以及填充导管(例如上入口623和/或下入口625)的钨惰性气体焊接。
在某些实施方式中,在可密封的容器被封闭在压力容器内(或者在可密封的容器是高压釜的情况下是压力容器)时执行氨填充过程。在某些实施方式中,可密封的容器600在用氨填充并密封之后被放置在压力容器内。
在某些实施方式中,压力容器是高压釜,并且可密封的容器600是高压釜200内的衬里或胶囊211,如图7中示意性所示。高压釜可以能够在高于约5MPa且低于约800MPa、低于约500MPa、低于约400MPa、低于约300MPa、低于约200MPa、或低于约100MPa的压力下,在约50摄氏度与约900摄氏度之间、约100摄氏度与约600摄氏度之间、约150摄氏度与约500摄氏度之间、或约200摄氏度与约400摄氏度之间的温度下处理流体中的材料。再次参考图7,高压釜200包括高压釜主体201。高压釜主体201的上部部分可以被上部加热器205围绕,并且高压釜主体的下部部分可以被下部加热器207围绕,所述上部加热器和所述下部加热器中的每一者都可包括绝缘体。上部加热器205可包括一个、两个或更多个独立可控的热区,例如,顶部尾区域205a和顶部主区域205b。下部加热器207可包括一个、两个或更多个独立可控的热区,例如,底部主区域207a和底部尾区域207b。上部加热器205和下部加热器207可以物理地接合成单一部件,但通常是独立可控的。在某些实施方式中,衬里211放置在高压釜主体201的空腔内。衬里211可以由以下物质形成或可包含以下物质:铂、钯、铱、Pt/Ir合金、金或银。衬里211还可包含或由以下物质中的一者或多者形成:钛、铼、铜、不锈钢、锆、钽、钼、铌、它们的合金等。
在某些实施方式中,高压釜200进一步包括如示意性所示的高压釜盖217和封闭固定件219,加垫圈(未示出)。如图7所示的配置是GraylocTM密封件的示意图。在其他实施方式中,高压釜200包括以下中的一者或多者:无支撑的布里奇曼密封件、O形环密封件、受限垫圈密封件、螺栓封闭件、AETM封闭件、EZE-封闭件TM、Keuntzel封闭件、ZipperClaveTM封闭件、无螺纹销封闭件、或GascheTM垫圈密封件。在某些实施方式中,除了上端上的盖、封闭固定件和密封件之外,高压釜200进一步包括下端上的盖、封闭固定件和密封件。
高压釜主体201、高压釜盖217、和封闭固定件219均可以由选自由以下项组成的组的材料制成:钢、低碳钢、SA723钢、SA266碳钢、4340钢、A-286钢、基于铁的超合金、基于镍的超合金、基于钴的超合金、Inconel 718、Rene 41、304不锈钢、310不锈钢、316不锈钢、340不锈钢、410不锈钢、和17-4沉淀硬化不锈钢、锆及其合金、钛及其合金、以及通常称为蒙乃尔合金、因科耐尔合金、哈氏合金、Udimet 500、司特来合金、Rene 41、和Rene 88的其他材料。包括高压釜主体201、高压釜盖217、和封闭固定件219部件中的一个或多个部件可以经历热处理操作。在某些实施方式中,高压釜主体201包括在底部以及顶部处的可拆卸密封件。
高压釜200可进一步包括底端加热器231,所述底端加热器热耦合至高压釜主体201的底部部分并且包括热隔离件232。底端加热器231生成围绕高压釜主体201的轴线在方位角上大致均匀的功率分布。相对于下部加热器207和上部加热器205中的功率水平的底端加热器231中的功率水平,以及对底端加热器231内的功率密度的径向依赖性经选择为维持沿着底表面215的温度分布均匀在10摄氏度内、5摄氏度内、2摄氏度内、1摄氏度内、0.5摄氏度内、或0.2摄氏度内。在某些实施方式中,相对于下部加热器207和上部加热器205中的功率水平的底端加热器231中的功率水平,以及对底端加热器231内的功率密度的径向依赖性经选择为维持底表面215的平均温度等于关于底表面215、衬里211的内表面、或高压釜主体201的内表面(如果衬里211不存在)测量的在指定高度内的平均温度,在20摄氏度内、10摄氏度内、5摄氏度内、2摄氏度内、或1摄氏度内。在某些实施方式中,指定高度为大约1厘米、5厘米、10厘米、20厘米、或25厘米。在某些实施方式中,底端加热器231配置有至少两个或至少三个独立可控的热区。
在某些实施方式中,高压釜200进一步包括顶部绝缘体/加热器209。在某些实施方式中,顶部绝缘体/加热器209包括或由以下组成:载荷热隔离体,例如氧化锆或另一种具有低热导率的陶瓷材料。在某些实施方式中,顶部绝缘体/加热器还具有生成热量,例如借助于通过高压釜盖217的电连接生成热量的能力。在某些实施方式中,顶部绝缘体/加热器209包括筒式加热器、缆线加热器、盘式加热器等中的一者或多者。顶部绝缘体/加热器209可具有精加工表面,以便所述顶部绝缘体/加热器紧贴高压釜盖217的下表面并抵靠衬里211的顶表面245并且相对于高压釜主体201的内表面有足够的径向间隙以便于插入和去除,而不会使得能够在高压操作期间将衬里211的上部部分挤压到径向间隙中。顶部绝缘体/加热器209的尺寸及其功率水平(如果存在的话),以及下部加热器207和上部加热器205(包括上部加热器205内的顶部区域)中的功率水平,,以及对顶部绝缘体/加热器209内的功率密度的径向依赖性可以经选择,以便维持沿着顶表面245的温度分布均匀在10摄氏度内、5摄氏度内、2摄氏度内、或1摄氏度内。此外,顶部绝缘体/加热器209的尺寸以及上部加热器205和下部加热器207的功率水平可经选择以维持顶表面245处于平均温度,所述平均温度等于关于顶表面245、内衬211的内表面、或高压釜主体201的内表面(如果衬里211不存在)测量的指定高度内的平均温度,在20摄氏度内、10摄氏度内、5摄氏度内、2摄氏度内,或1摄氏度内。在某些实施方式中,指定高度为大约1厘米、5厘米、10厘米、20厘米、或25厘米。在某些实施方式中,顶部绝缘体/加热器209配置有至少两个或至少三个独立可控的热区。
在某些实施方式中,可密封的容器600放置在内部加热的高压设备300内作为胶囊307,如图8中示意性所示。内部加热的高压设备300在所有方向上提供足够的围堵,所述方向对于典型的圆柱形容器可以分类为径向和轴向。此外,取决于设计参数的具体情况,所述设备能够在200摄氏度与1500摄氏度之间的温度下、约5MPa与约2000MPa之间的压力下操作达在约1小时与约180天之间。所述内部加热的高压设备300可以包括一个或多个环组件的堆叠以提供径向封堵,所述径向封堵包括高强度封闭环301和陶瓷环303。所述堆叠可包括大于2个、大于5个、大于10个、大于20个、大于30个、大于50个、或大于100个环组件。所述堆叠围绕加热器或加热构件305和胶囊307,并且可以由至少一个支撑板(未示出)机械支撑。换句话说,加热构件或加热器可定位在胶囊与一个或多个径向约束结构之间,所述径向约束结构包括高强度封闭环和陶瓷环303。所述堆叠可以为在胶囊307内生成并通过加热器305向外传递的压力提供径向封堵。加热器305包括上部加热器305a和下部加热器305b。上部加热器305a和下部加热器305b中的每一者可包括一个、两个或更多个独立可控的热区。上部加热器305a和下部加热器305b可以物理地接合成单一部件,但通常是独立可控的。加热器305的内部可以限定处理腔室,胶囊307可以放置在所述处理腔室中。在模具堆叠中的环组件由高强度封闭环301和陶瓷环303构成的情况下,在每个环组件中的两个构件之间可能存在干涉配合。可提供用于对一个或多个环组件或径向约束件进行外部冷却的装置。在某些实施方式中,胶囊307包括内部胶囊构件和外部胶囊构件(未示出)。
胶囊307内生成的压力的轴向封堵可以由端塞311、冠构件317、和拉杆或拉杆紧固件315提供。端塞311可以包含氧化锆(zirconium oxide/zirconia)。根据具体实施方式,替代端塞材料可包括氧化镁、氧化铝、氧化硅、碳化硅、碳化钨、钢、镍合金、钛合金、盐、和页硅酸盐矿物,例如氢氧化硅酸铝或叶腊石。端塞311可以被端塞护套313包围。端塞护套可以为端塞311提供机械支撑和/或径向封堵。端塞护套313还可以为加热器305提供机械支撑和/或轴向封堵。端塞护套313可包含钢、不锈钢、基于铁的合金、基于镍的合金等。在某些实施方式中,拉杆紧固件315布置成提供两个或更多个环组件的轴向负载的构造。美国专利9,724,666和10,174,438中提供了进一步的细节,这些专利的全文据此以引用方式并入。
冠构件317和拉杆紧固件315可包含选自由以下项组成的组的材料:钢、低碳钢、SA723钢、SA266碳钢、4340钢、A-286钢、基于铁的超合金、304不锈钢、310不锈钢、316不锈钢、340不锈钢、410不锈钢、17-4沉淀硬化不锈钢、锆及其合金、钛及其合金,以及通常称为蒙乃尔合金、因科耐尔合金、哈氏合金、Udimet 500、司特来合金、Rene 41、和Rene88。
根据具体实施方式,内部加热的高压设备300可以包含靠近胶囊307的轴向端部和端塞311的压力传输介质309。压力传输介质309可以包括多个部件,例如一个或多个盘。根据具体实施方式,压力传输介质可包含氯化钠、其他盐、或页硅酸盐矿物(例如氢氧化硅酸铝或叶腊石)、或其他材料。在某些实施方式中,压力传输介质309可以包括金属卤化物中的一者或多者,例如NaCl、NaBr、AgCl、AgBr、CaF2、SrF2、石墨、六方氮化硼、滑石、皂石、石膏、石灰石、雪花石膏、二硫化钼、碳酸钙、氧化镁、氧化锆、梅岭粘土(merylinite clay)、膨润土粘土、或硅酸钠。
内部加热的高压设备300可进一步包括分别热耦合至胶囊307的底部部分和顶部部分的底端加热器331和/或顶端加热器341。底端加热器331生成围绕加热器305的轴线在方位角上大致均匀的功率分布,并且相对于下部加热器305b和上部加热器305a中的功率水平的底端加热器331中的相对功率水平,以及对底端加热器331内的功率密度的径向依赖性,经选择以便维持沿着底表面215的温度分布均匀在10摄氏度内、5摄氏度内、2摄氏度内、或1摄氏度内。在某些实施方式中,相对于下部加热器305b和上部加热器305a中的功率水平的底端加热器331中的相对功率水平,以及对底端加热器331内的功率密度的径向依赖性,经选择为维持底表面215的平均温度等于关于底表面215或胶囊307的内表面测量的指定高度内的平均温度,在10摄氏度内、5摄氏度内、2摄氏度内、或1摄氏度内。在某些实施方式中,指定高度为大约1厘米、5厘米、10厘米、20厘米、或25厘米。顶端加热器341生成围绕加热器305的轴线在方位角上大致均匀的功率分布,并且相对于下部加热器305b和上部加热器305a中的功率水平的顶端加热器341中的相对功率水平,以及对顶端加热器341内的功率密度的径向依赖性,经选择为维持沿着顶表面345的温度分布均匀在10摄氏度内、5摄氏度内、2摄氏度内、或1摄氏度内。在某些实施方式中,相对于下部加热器305b和上部加热器305a中的功率水平的顶端加热器341中的相对功率水平,以及对底端加热器331内的功率密度的径向依赖性,经选择为维持顶表面345的平均温度等于关于顶表面345或胶囊307的内表面测量的指定高度内的平均温度,在10摄氏度内、5摄氏度内、2摄氏度内、或1摄氏度内。
然后关闭压力容器(例如,高压釜200(图7)或内部加热的高压设备300(图8)),然后将可密封的容器600加热至高于约400摄氏度的温度并加压至高于约10MPa,从而导致可密封的容器600内的氨变成氨超临界流体。在某些实施方式中,温度最初升高至第一中间值,例如,在约100摄氏度与约400摄氏度之间,以使铝和其他金属能够如上所述在可密封的容器600内反应以形成氢气,以及使叠氮化物矿化剂(如果存在的话)能够如上所述分解成酰胺加氮气,以及使得能够进行氢气与氮气之间的催化反应以形成氨。然后可以将温度升高至第二值,例如,在约400摄氏度与约1000摄氏度之间、在约500摄氏度与约800摄氏度之间、或在约600摄氏度与约700摄氏度之间,并且压力在约10MPa与约1000MPa之间、在约50MPa与约750MPa之间、或在约100MPa与约500MPa之间。在某些实施方式中,再次参考图8,底端加热器331、顶端加热器341、上部加热器305a和下部加热器305b中的功率水平经调节以便将胶囊307(与可密封的容器600相同)内的温度维持均匀在约20摄氏度内、约10摄氏度内、约5摄氏度内、约2摄氏度内、或约1摄氏度内。温度可以在此温度下维持在约1小时与约30天之间、或在约2小时与约7天之间、或在约3小时与约96小时之间的时段。
再次参考图6,在矿化剂存在下将可密封的容器600在超临界氨中保持在升高的温度下期间,将含铝生坯609中存在的铝转化为AlN,并且实际上,与磷光体粒子101一起烧结,从而形成具有高热导率的含铝的氮化物陶瓷基质复合物。不希望受理论束缚,本发明人相信超临界氨进入含铝生坯609中的孔隙357(参见图3B和图4B)并且还进入在铝与NH3反应形成AlN的过程中形成的裂纹中,从而导致局部体积增加约25.7%。一部分AlN借助于与矿化剂发生化学反应而溶解。例如,在碱性矿化剂的情况下,可能会发生以下可逆反应:
AlN+KNH2+2NH3=KAl(NH2)4
溶解的中间体(在具体示例中为KAl(NH2)4)可以然后跨孔隙357输送,由此可以发生逆反应,从而在不同的位置沉积AlN。以这种方式,超临界流体提供陶瓷复合物内的Al原子和AlN单元可以移动的机制,所述机制在许多方面类似于在高得多的温度下的陶瓷烧结过程期间发生的表面扩散过程。晶粒粗化和陶瓷复合物致密化的发生原因与正常烧结过程中相同,即陶瓷复合物内表面能的降低。然而,由于超临界流体溶解/再沉积过程在比烧结所需的温度低得多的温度下发生,因此更容易在磷光体粒子101内维持良好性质,例如外部量子效率,并且与传统烧结工艺的情况相比也更容易将两种或更多种不同类型的磷光体粒子彼此紧密接近地掺入到具有高热导率的单个复合构件中。然而,重要的是维持可密封的容器600内的温度大致均匀,否则溶解的中间体可能被输送到可密封的容器600内的另一更热或更冷的位置,从而在那个位置处而不是在陶瓷复合物内沉积AlN。例如,Peters[Journal of Crystal Growth 104,411(1990)]表明,AlN单晶可以通过将Al金属转化成AlN,以及超临界氨内的宏观传输和作为矿化剂存在的KNH2,而在压力容器内最热的表面上形成。在本公开中,通过维持近似等温的环境以及可密封的容器600内的有限传导性来抑制溶解的Al的宏观传输,例如通过含铝生坯609在可密封的容器600内的密集堆积或使用复合材料的轧制层(参见图2A中的生坯290A)。
另外,不希望受理论束缚,本发明人相信,通过与来自吸气金属的超临界氨反应形成的吸气金属氮化物(如果存在的话)将与含铝涂层或粒子的表面上的氧化物反应:
Be3N2+Al2O3=3BeO+2AlN
Mg3N2+Al2O3=3MgO+2AlN
2ScN+Al2O3=Sc2O3+2AlN
2YN+Al2O3=Y2O3+2AlN
在吸气金属被包含在含铝涂层或粒子内的情况下,所得吸气金属氮化物和氧化物将可能保留在所得的含铝的陶瓷基质复合物内。在相对于含铝涂层或粒子中的氧含量仅稍微过量地添加吸气金属且吸气金属氧化物具有比Al2O3(例如,BeO或MgO)更高的热导率的情况下,通过添加吸气金属可以显著增强含铝的陶瓷基质复合物的热导率。
在第二温度下达预定的时间段之后,可冷却可密封的容器,从可密封的容器中释放氨,将氨从压力容器中去除,并打开压力容器。然后可以去除含铝的陶瓷基质复合物。在某些实施方式中,陶瓷基质复合材料的个别颗粒体、丸粒或片剂是通过颚式破碎、圆锥破碎、锤式破碎、碾磨、研磨、振动和本领域已知的其他粉碎形式中的一种或多种来制备。在某些实施方式中,陶瓷基质复合材料的个别颗粒体、丸粒或片剂经历进一步处理,例如切割、锯切、研磨、双面研磨、抛光、滚揉、蚀刻等中的一种或多种,以形成成品含铝的陶瓷基质复合物零件。
成品含铝的陶瓷基质复合物零件可在基本上由AlN组成的基质内包含至少一种、至少两种或至少三种磷光体组合物,其中磷光体与AlN的体积比在约1%与约99%之间、在约5%与约95%之间、在约10%与约90%之间、或在约20%与约80%之间。成品含铝的陶瓷基质复合物零件的孔隙率可在约1%与约50%之间、在约2%与约25%之间、在约3%与约20%之间、或在约4%与约10%之间。成品含铝的陶瓷基质复合物零件的热导率可以在约1瓦/米-开尔文与约320瓦/米-开尔文之间、在约5瓦/米-开尔文与约260瓦/米-开尔文之间、在约10瓦/米-开尔文与约170瓦/米-开尔文之间、或在约20瓦/米-开尔文与约100瓦/米-开尔文之间。成品含铝的陶瓷基质复合物零件内的至少一种、至少两种或至少三种磷光体组分的内量子效率可为至少约30%、至少约50%、至少约75%,或至少约90%。成品含铝的陶瓷基质复合物零件内的至少一种、至少两种或至少三种磷光体组分的发光效率可为至少约30流明/瓦、至少约50流明/瓦、至少约100流明/瓦、或至少约150流明/瓦。氮化铝基质材料在约400纳米与约750纳米之间的波长处的光吸收系数小于约100cm-1、小于约50cm-1、小于约20cm-1、小于约10cm-1、小于约5cm-1、小于约2cm-1、或小于约1cm-1。
在某些实施方式中,磷光体粒子101中的磷光体组合物中的一种或多种磷光体组合物可以在包含氨和矿化剂组合物的超临界流体组合物中具有显著的溶解度。在这些情况下,除了磷光体粒子与AlN基质之间的键之外,相邻磷光体粒子之间还可以形成直接键。例如,可能会发生在氮化物和氮氧化物磷光体组合物之内和之间的直接“烧结”,例如,β-SiAlON:Eu2+、α-SiAlON:Eu2+、和CaAlSiN3:Eu2+。在某些实施方式中,本公开中描述的方法可用于制造完全不含AlN的含磷光体的陶瓷复合物。例如,可以通过注浆成型(图2A)和/或压片(图5A)工艺生产包含磷光体粒子和添加剂的生坯。在放置后,可将含磷光体的生坯连同矿化剂和任选的一种或多种用于去除表面氧化物的吸气剂材料和用于将H2和N2转化为NH3的催化剂一起放置在可密封的容器中(图6)。在泵送、吹扫、添加NH3和密封之后,然后可将可密封的容器加热至第一温度(例如,在约100摄氏度与约400摄氏度之间)和第二温度(例如,在约400摄氏度与约1000摄氏度之间),如上所述。如上所述,所得磷光体陶瓷复合物可以处理成成品磷光体陶瓷复合物零件。
通过上述一种或多种方法形成的成品含铝的氮化物陶瓷基质复合物可以与激光二极管和发光二极管中一者或多者一起结合到包装中。例如,来自激光二极管或发光二极管的紫光或蓝光可以照射或聚焦在含铝的氮化物陶瓷基质复合物上,从而导致发射蓝光、绿光、黄光、橙光和/或红光。在某些实施方式中,从包装发出的总体出射光(包括来自激光二极管或发光二极管的反射光以及由磷光体发射的光)是白光。在某些实施方式中,白光的显色指数(CRI)大于约80、大于约85、大于约90、大于约95、大于约98、或大于约99。在某些实施方式中,白光的CRI R9值大于约50、大于约70、大于约80、或大于约90。含铝的氮化物陶瓷基质复合物可以结合至散热器以消散在磷光体内的光转化期间生成的热量。在某些实施方式中,一个或多个含铝的陶瓷基质复合物零件被结合到表面安装装置(surface mountdevice,SMD)内,所述表面安装装置作为紧凑的、成本有效的包装可能是有利的。
方法实施例
本文所述的方法提供了用于制造高性能陶瓷基质复合物的方法,所述高性能陶瓷基质复合物包含具有高热导率和高内量子效率的磷光体组合物。
实施例1
在氧和水浓度低于1ppm的手套箱内通过填充高纯度铝锭制备粒径在约10微米与约100微米之间的铝粉。提供粒径均在约5微米与约50微米之间的绿色β-SiAlON:Eu2+磷光体和红色CaAlSiN3:Eu2+磷光体,并且在手套箱中用研钵和杵制备重量比为5:1:2的含铝、绿色磷光体和红色磷光体的共混物。将粉末共混物在约50MPa的压力下压制成直径为6毫米并且厚度为1mm的圆盘,所述圆盘的生坯孔隙率在约10%与约40%之间。将圆盘放入手套箱内的外径为1.00英寸并且长度为5.25英寸的含银胶囊中,并使用轨道焊机来焊接封闭胶囊。在手套箱内将4.0g的KN3粉末放入类似于图9所示的不锈钢矿化剂容器中,并借助于(CF)凸缘封闭所述容器。从手套箱中取出具有类似于图9中示意性示出的冲洗容器的矿化剂容器和胶囊。将经矿化的容器冷却至干冰温度并填充10.0g的氨,并将冲洗容器冷却至干冰温度并填充9.0g的氨,然后将两个容器都升温至室温并连接至胶囊。将胶囊冷却至干冰温度,并打开矿化剂容器与胶囊之间的阀,从而将液氨矿化剂溶液转移至胶囊。然后关闭矿化剂容器的出口阀,并打开冲洗容器与矿化剂容器之间的阀,从而将液氨从冲洗容器转移至矿化剂容器。用热风枪轻轻加热冲洗容器,以将剩余的液氨驱动到矿化剂容器中。再次打开矿化剂容器与胶囊之间的阀,从而将剩余的氨转移到胶囊中。然后将胶囊上的填充导管焊接封闭并切断,并将胶囊装载到内部加热的高压设备中。
所述高压在8小时内升温至675摄氏度,在没有故意温度梯度的情况下保持在此温度24小时,并冷却。从胶囊中去除氨,将胶囊从高压设备中取出,打开,并取出圆盘。通过光学和扫描电子显微镜(scanning electron microscopy,SEM)/能量色散光谱(energydispersive spectrometry,EDS)和x射线粉末衍射检查圆盘,通过水银孔隙率法测量所述圆盘的孔隙率,通过激光闪光法测量它们的热扩散率,使用差示扫描量热计测量它们的比热容,并且将它们的热导率计算为热扩散率、比热容和堆积密度的乘积。X射线衍射显示存在AlN(磷光体组合物),并且没有高于检测限的附加相。断裂截面的SEM图像显示两种类型的磷光体粒子都被AlN润湿并且AlN形成了多孔基质。圆盘的孔隙率测量为30%。热导率测量为30W m-1K-1。
尽管以上是具体实施方式的完整描述,但是可以使用各种修改、替代构造和等同物。因此,以上描述和说明不应被视为限制由所附权利要求书限定的本公开的范围。
Claims (20)
1.一种用于形成含铝的氮化物陶瓷基质复合物的方法,所述方法包括:
形成至少一个生坯,所述至少一个生坯包含磷光体粉末和含铝组合物,其中,
所述至少一个生坯的特征在于孔隙率在约10%与约80%之间,并且
所述磷光体粉末包含至少一种磷光体组合物,并且磷光体粒子的D50直径在约100纳米与约500微米之间;并且
将可密封的容器加热至在约400摄氏度与约800摄氏度之间的温度以及在约10MPa与约1000MPa之间的压力,
其中,
在对所述可密封的容器进行加热和加压之前,将所述至少一种生坯、氨和矿化剂组合物设置在所述可密封的容器内,
所述含铝组合物的纯度基于金属计在约90%与约99.9999%之间,
在对所述可密封的容器进行加热和加压之前,填充有液氨的所述可密封的容器内的自由体积分数在约10%与约95%之间,并且
加热所述可密封的容器包括将所述可密封的容器加热达第一时间段以形成含铝的氮化物陶瓷基质复合物,所述含铝的氮化物陶瓷基质复合物的特征在于,磷与氮化铝(AlN)的体积比在约1%与约99%之间,孔隙率在约1%与约50%之间,并且热导率在约1瓦/米-开尔文与约320瓦/米-开尔文之间。
2.根据权利要求1所述的方法,其中所述磷光体组合物包含以下中的一者或多者:Y3Al5O12:Ce3+、Lu3Al5O12:Ce3+、(Y,Gd,Tb,Sc,Lu,La)3(Al,Ga,In)5O12:Ce3+、β-SiAlON:Eu2+、α-SiAlON:Eu2+、SrSi2O2N2:Eu2+、SrGa2S4:Eu2+、SrS:Eu2+和CaAlSiN3:Eu2+。
3.根据权利要求1所述的方法,其中所述粉末粒子的特征在于D50直径在约1微米与约200微米之间。
4.根据权利要求1所述的方法,其中所述含铝组合物包含涂层,所述涂层设置在所述生坯的至少一部分上并且厚度在约50纳米与约100微米之间。
5.根据权利要求1所述的方法,其中所述含铝组合物进一步包含吸气剂组合物,所述吸气剂组合物包含以下中的一者或多者:铍、镁、钙、锶、钡、钪、钛、钒、铬、钇、锆、铌、稀土金属、铪、钽或钨。
6.根据权利要求5所述的方法,其中所述吸气剂组合物包含以下中的一者或多者:铍、镁、钪或钇。
7.根据权利要求1所述的方法,其中所述生坯进一步包含含铝粒子,所述含铝粒子包含以下中的一者或多者:氮化铝粉末、氮化铝砂粒、铝粉、铝片、铝丸粒、铝刨花、铝砂粒或铝蒸发料块。
8.根据权利要求7所述的方法,其中所述含铝粒子的特征在于最大尺寸在约1微米与约10毫米之间。
9.根据权利要求1所述的方法,所述方法进一步包括通过流延成型、丝网印刷或刮刀刀片方法形成所述至少一个生坯。
10.根据权利要求9所述的方法,其中所述流延成型、丝网印刷或刮刀刀片方法进一步包括使用镂空掩模。
11.根据权利要求1所述的方法,其中所述生坯通过造粒、粒化或压片工艺中的一者或多者形成。
12.根据权利要求1所述的方法,所述方法进一步包括:
在加热所述可密封的容器的同时,在可密封胶囊中形成超临界氨;以及
在将所述生坯暴露于所述超临界氨之前,将所述生坯加热至高于约600摄氏度的温度。
13.根据权利要求1所述的方法,其中所述矿化剂包含以下中的一者或多者:Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr或Ba,或其氢化物、酰胺、酰亚胺、酰胺酰亚胺、氮化物或叠氮化物。
14.根据权利要求13所述的方法,其中所述矿化剂包括叠氮化钠和叠氮化钾中的至少一者。
15.根据权利要求13所述的方法,其中所述可密封的容器在加热所述可密封的容器之前进一步包含金属组合物,并且设置在所述可密封的容器内的所述金属组合物的组成和量使得通过叠氮化物矿化剂的分解生成氮气物质,并且通过摩尔比为约1:3的至少所述金属与所述超临界氨的反应生成氢气物质。
16.根据权利要求1所述的方法,其中所述矿化剂包含以下中的一者或多者:NH4F、NH4Cl、NH4Br、NH4I、AlF3、AlCl3、AlBr3、AlI3,或通过F、Cl、Br、I、HF、HCl、HBr、HI、Al、AlN、和NH中的两者或更多者的反应形成的任何化合物。
17.根据权利要求1所述的方法,其中所述含铝氮化物陶瓷基质复合物的特征在于,孔隙率在约3%与约20%之间。
18.根据权利要求1所述的方法,其中所述含铝的氮化物陶瓷基质复合物的特征在于,热导率在约10瓦/米-开尔文与约170瓦/米-开尔文之间。
19.根据权利要求1所述的方法,其中所述含铝的氮化物陶瓷基质复合物包含至少两种磷光体组合物。
20.根据权利要求1所述的方法,其中所述含铝的氮化物陶瓷基质复合物包含至少一种内量子效率为至少约30%的磷光体组合物。
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