CN101555387A - Rare-earth polishing material with a core shell structure and preparation method thereof - Google Patents
Rare-earth polishing material with a core shell structure and preparation method thereof Download PDFInfo
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- CN101555387A CN101555387A CNA2008101034870A CN200810103487A CN101555387A CN 101555387 A CN101555387 A CN 101555387A CN A2008101034870 A CNA2008101034870 A CN A2008101034870A CN 200810103487 A CN200810103487 A CN 200810103487A CN 101555387 A CN101555387 A CN 101555387A
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- polishing material
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- ammonium
- oxide
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- 238000005498 polishing Methods 0.000 title claims abstract description 104
- 239000000463 material Substances 0.000 title claims abstract description 67
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 50
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011258 core-shell material Substances 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 54
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 238000001556 precipitation Methods 0.000 claims description 20
- 229910052684 Cerium Inorganic materials 0.000 claims description 17
- 239000011257 shell material Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 11
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 11
- 239000011707 mineral Substances 0.000 claims description 11
- 235000010755 mineral Nutrition 0.000 claims description 11
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 9
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- -1 polyoxyethylene Polymers 0.000 claims description 8
- 238000003483 aging Methods 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims description 6
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 229910052772 Samarium Inorganic materials 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 4
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 4
- 150000003863 ammonium salts Chemical class 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 4
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 4
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- WMOHXRDWCVHXGS-UHFFFAOYSA-N [La].[Ce] Chemical compound [La].[Ce] WMOHXRDWCVHXGS-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- ONLCZUHLGCEKRZ-UHFFFAOYSA-N cerium(3+) lanthanum(3+) oxygen(2-) Chemical compound [O--].[O--].[O--].[La+3].[Ce+3] ONLCZUHLGCEKRZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- AOSFMYBATFLTAQ-UHFFFAOYSA-N 1-amino-3-(benzimidazol-1-yl)propan-2-ol Chemical compound C1=CC=C2N(CC(O)CN)C=NC2=C1 AOSFMYBATFLTAQ-UHFFFAOYSA-N 0.000 claims description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004160 Ammonium persulphate Substances 0.000 claims description 2
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- 241000282326 Felis catus Species 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229920004890 Triton X-100 Polymers 0.000 claims description 2
- 239000013504 Triton X-100 Substances 0.000 claims description 2
- OZZOVSQSDIWNIP-UHFFFAOYSA-N acetic acid;azane Chemical compound [NH4+].[NH4+].CC([O-])=O.CC([O-])=O OZZOVSQSDIWNIP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 238000000975 co-precipitation Methods 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 239000006012 monoammonium phosphate Substances 0.000 claims description 2
- 230000006911 nucleation Effects 0.000 claims description 2
- 238000010899 nucleation Methods 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims 5
- 238000005520 cutting process Methods 0.000 abstract description 12
- 238000007517 polishing process Methods 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract 2
- 150000002484 inorganic compounds Chemical class 0.000 abstract 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000000227 grinding Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CNERRGRDMYRHEV-UHFFFAOYSA-H [Cl-].[La+3].[Ce+3].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] Chemical compound [Cl-].[La+3].[Ce+3].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] CNERRGRDMYRHEV-UHFFFAOYSA-H 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- AAINJZRFCSHHJI-UHFFFAOYSA-H trifluorocerium trifluorolanthanum Chemical compound F[La](F)(F)[Ce](F)(F)F AAINJZRFCSHHJI-UHFFFAOYSA-H 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 239000012702 metal oxide precursor Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- TZBAVQKIEKDGFH-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-1-benzothiophene-2-carboxamide;hydrochloride Chemical compound [Cl-].C1=CC=C2SC(C(=O)NCC[NH+](CC)CC)=CC2=C1 TZBAVQKIEKDGFH-UHFFFAOYSA-N 0.000 description 1
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention provides a polishing material with a nuclear shell structure and a preparation method thereof. The rare-earth polishing material is powder granules, the inner core of the rare-earth polishing material is an inorganic compound taking rare-earth oxide as a main body, and the shell is an inorganic compound containing the rare-earth oxide or/and fluoride. The polishing material comprises the following components according to the weight percentage: 50-99 of rare earth, 0.9-50 of other components and less than 0.1 of unavoidable impurities. The rare-earth polishing material has mean granule size of 0.1um-2.0um, the specific surface area after calcination at 900 DEG C of less than 15m<2>/g, and the dispersity of less than 1.5. The obtained rare-earth polishing material has a positive cooperative function in the polishing process, a greater cutting function on a material with high hardness, an elastic buffer function on a material with lower hardness and higher cutting capability and does not generate scratches. The preparation method of the rare-earth polishing material is simple and is easy to realize industrialization.
Description
Technical field
The present invention relates to rare-earth polishing material of a kind of nucleocapsid structure and preparation method thereof, belong to the chemical preparation technical field of rare earth powder body material.
Background technology
From 1940, polishing powder from rare earth began to replace ferric oxide and is used for glass polishing, becomes one of critical process material in the glass polishing course of processing.Compare with traditional polishing powder, polishing powder from rare earth has the advantage of fast, the highly polished and long service life of polishing velocity, and can change quality of finish and operating environment.Two the important performance characteristic polishing velocities in the polishing process and the quality (being roughness) of glazed surface are all relevant by the structure (monocrystalline, polycrystalline) and the pattern (size distributes and shape) of polishing powder.The researchist does not stop has developed various polishing powder, as silicon-dioxide, aluminum oxide, cerium oxide, zirconium white, stannic oxide and manganese oxide etc.Wherein the Mohs' hardness of cerium rouge is 6 to receive much concern less than other several polishing powders.A kind of preparation method of synthetic cerium oxide particle is disclosed as United States Patent (USP) 5543216, the pH value of this method conditioned reaction thing is 8～9, and under pressure, be warming up to 100～200 ℃, the particle size that obtains is between 0.03～5um, this method more complicated, apparatus expensive, size-grade distribution is wide, and polishing effect is not good.Chinese patent CN1821314 discloses a kind of preparation method of fine cerium oxide, after adopting cerium solution to add tensio-active agent, allow solution contact with alkaline matter earlier, the control reaction pH value, generate throw out, this suspension transforms with oxalic acid then, the pH value of control reaction end, filter at last, wash, dry this throw out, the fine cerium oxide that obtains after the calcination can be used for polishing, but also more complicated of preparation process in this method, the Granularity Distribution of system also than broad between 10nm～30um, specific surface area has reached 50m
2/ g, it is poor as the polishing powder reusability.
In the use of polishing powder, there is following problem: the dispersion of particles stability problem, because interparticle interaction force, scattered particle is in depositing process, can take place inevitably to assemble to some extent, generate macroparticle, cause polishing cut ground to produce.On the other hand when reducing the scuffing of polishing powder, the cutting power of polished surface has been reduced at glazed surface.Having software engineering researchers invent to go out mixture uses as polishing powder, Chinese patent 03812996.6 discloses a kind of metal oxide powder that can be used for the high degree of accuracy polishing and preparation method thereof, this metal oxide powder mixes thinner for passing through with metal oxide precursor, grinding mixture, the mixture of the metal oxide that obtains after the calcining, its invention is a kind of improved polishing metal oxide powder, and need produce the aggregate of the one-level spheroidal particle with irregular particle shape by careful control preparation technology.This metal oxide or its mixture use it to wear no resistance as polishing powder, and be broken easily, the irregularly shaped easy scuffing polished surface after the fragmentation.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, rare-earth polishing material of a kind of nucleocapsid structure and preparation method thereof is provided.The rare-earth polishing material of this nucleocapsid structure is a powder, particulate state, and its kernel is the mineral compound based on rare earth oxide, shell is to contain rare earth oxide/and or mineral compound of fluorochemical.
The shell of nucleocapsid rare-earth polishing material is fluorine-containing mineral compound, and fluorine content is more than 2 times of fluorine content in the kernel, and the thickness of shell is 2nm-1 μ m.
The shell of this nucleocapsid rare-earth polishing material can contain rare earth oxide/or fluorochemical, comprises the oxide compound of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium and in the fluorochemical one or more.Particularly cerium or lanthanum cerium oxide are or/and the mineral compound of fluorochemical.
The mineral compound main body of the kernel of nucleocapsid rare-earth polishing material of the present invention is a rare earth oxide, comprises in the oxide compound of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium one or more.Be preferably cerium or lanthanum cerium mixed oxide.
Rare-earth polishing material with nucleocapsid structure of the present invention, kernel are CeO
2, shell is CeF
3, CeOF.
Content with rare-earth polishing material middle-weight rare earths of nucleocapsid structure of the present invention is weight percentage 50～99%, and the content of other compositions is weight percentage 0.9～50%, and other are unavoidable impurities＜0.1%.Median size is between 0.02～3.0um, and calcining back specific surface area is less than 20m under 900 degree
2/ g, dispersity is less than 2.0.Especially, median size is between 0.1～2.0um, and calcining back specific surface area is less than 15m under 900 degree
2/ g, dispersity is less than 1.5.
The content of rare-earth polishing material middle-weight rare earths is weight percentage 50～99%, and the content of other compositions is weight percentage 0.9～50%, and other are unavoidable impurities＜0.1%.
Prepare the method with rare-earth polishing material of nucleocapsid structure of the present invention, adopt coprecipitation method, concrete steps are:
1) nitrate, muriate, vitriol or their composite solution with nuclear matter is made into the solution that concentration is 0.05～2mol/L;
2) get precipitation agent: the mixture of one or more in ammoniacal liquor, bicarbonate of ammonia, the volatile salt, precipitation agent total concn are 0.1～2.0mol/L;
3) stirring joins precipitation agent in the salts solution of nuclear matter down, and stirring is continued in the reinforced back that finishes;
4) will form nitrate, muriate, vitriol or their composite solution of shell material and Neutral ammonium fluoride that concentration is 0.01～1.0mol/L or hydrofluoric acid joins above-mentioned solution simultaneously and makes and mix;
5) mixed solution is incubated ageing 0.5～48 hour down at 30 ℃～100 ℃, filters or centrifugation, obtain the presoma of polishing material after the drying; The presoma powder 600 ℃～1100 ℃ following calcinations, through dispersion, sorting or sieve, is obtained polishing powder from rare earth again, obtain having the polishing material of nucleocapsid structure.
In above-mentioned preparation process, can add ammonium salt, in the tensio-active agent one or more are as additive and stir, add-on is the 0.01-10% of polishing powder gross weight, ammonium salt comprises ammonium chloride, ammonium nitrate, Neutral ammonium fluoride, ammonium sulfate, ammonium persulphate, monoammonium phosphate, ammonium bifluoride, ammonium molybdate, Tetrabutyl amonium bromide, the ammonium acetate ammonium formiate, ammonium sulfide, the sulphur ammonium, primary ammonium phosphate, Tetramethylammonium hydroxide, monoammonium sulfate, ammonium oxalate, ammonium polyphosphate, ammonium phosphomolybdate, ammonium phosphate, ammonium bisulfite, ammonium polyphosphate, tensio-active agent comprises anion surfactant, cats product, nonionogenic tenside, preferred polyoxyethylene glycol, polyethylene, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, Witconol AL 69-66, polyethylene anhydrous sorbitol Stearinsaeure, cetyl trimethylammonium bromide, Triton X-100.；
A kind of preparation method of rare-earth polishing material of nucleocapsid structure, with the cerium oxide is nucleus, the mode that coats nucleation prepares the polishing powder of nucleocapsid structure, its concrete steps are: ceria oxide powder is dispersed in the salts solution that contains rare earth or other components, add an amount of Neutral ammonium fluoride or hydrofluoric acid again, make it form the fluorochemical precipitation, fully react after-filtration or centrifugation, obtain the presoma of polishing material after the drying on the cerium oxide surface; Obtain having the powder of nucleocapsid structure after the calcination, through dispersion, sorting or sieve, obtain the polishing material of nucleocapsid structure again.
A kind of preparation method of rare-earth polishing material of nucleocapsid structure, the oxide compound of cerium, carbonate, oxalate, Citrate trianion, stearate are added in hydrofluoric acid and the fluorochemical one or several put into High Temperature Furnaces Heating Apparatus, under oxidizing atmosphere/no atmosphere, calcining temperature was calcined 1-20 hour under the 700-1200 degree, obtained the rare-earth polishing material of nucleocapsid structure through aftertreatment.
Advantage of the present invention is: the rare-earth polishing material that the present invention obtains is because the nucleocapsid structure that two kinds of materials of different hardness and crystalline structure are formed, the different properties of core-shell material has played positive cooperativity in polishing process, in the big bigger shear action of material performance of hardness, produce when scratching, the hardness materials with smaller plays the effect of an elastic buffer, when making rare-earth polishing material of the present invention promptly have high cutting power, and do not produce scuffing.Preparation method's technology of the present invention is fairly simple, realizes industrialization easily.
The said dispersity of the present invention is defined as: (d
90-d
10)/2d
50
Wherein: d
90Be that 90% particulate diameter is less than d
90Particle diameter;
d
50Be that 50% particulate diameter is less than d
50Particle diameter;
d
10Be that 10% particulate diameter is less than d
10Particle diameter.
Embodiment
Come the present invention is done further by specific embodiment, these embodiment are not in order to limiting the scope of the invention, and those skilled in the art can unlabored modification or change, all contains within the scope of the invention.
Embodiment 1
The solution of lanthanum, the cerium sulphate 1.5mol/L of being made into soluble in water is put into reactor, be heated to 40 ℃.With the concentration for preparing is the precipitation agent bicarbonate of ammonia of 1.0mol/L and the mixing solutions of ammoniacal liquor, joins in the end liquid with the speed of 2L/min; After treating reinforced finishing, neodymium nitrate solution is joined in the end liquid with the speed of 2L/min; To mix mother liquor and be warming up to 80 ℃, continue stirring reaction 5 hours, and react fully and carry out, and obtain precipitation; Be deposited in 60 ℃ of following ageings 24 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the polishing powder presoma, powder obtains mixed powder after 900 ℃ of calcinings, cross 400 mesh sieves behind the wet ball grinding, centrifugal drying obtains having the polishing material of nucleocapsid structure, and particle diameter is 1.5um, dispersity is 1.43, and specific surface area is 9.23m
2/ g.Polishing powder is made 10% slurries, liquid-crystalline glasses is polished, polishing powder product cutting force is 0.023mm/h, and the range estimation cut is 0/m
2Existing polishing powder is made 10% slurries, liquid-crystalline glasses is polished, polishing powder product cutting force is 0.013mm/h, and the range estimation cut is 0/m
2
Embodiment 2
Its step of preparation process is with example 1, and salts solution is the muriate of lanthanum, praseodymium, neodymium, and concentration is 1.0mol/L, and precipitation agent is the mixture of bicarbonate of ammonia and volatile salt, and concentration is 2.0mol/L, and the reaction back adds the Cerium II Chloride of 1.5mol/L.Add weight percent and be 8.0% polyvinyl alcohol in mixing solutions, be reflected at 95 ℃ of reactions 4 hours down, 50 ℃ of following ageings 36 hours, be deposited in 1000 ℃ of calcinings, through the airflow milling cracking and sorting, obtaining median size is 1.3um, dispersity is 1.4, and specific surface area is 4.56m
2The polishing material of/g with nucleocapsid structure.Polishing powder is made 16% slurries, high-accuracy opticglass is polished, polishing powder product cutting force is 0.031mm/h, and the range estimation cut is 1/m
2Existing polishing powder is made 16% slurries, high-accuracy opticglass is polished, polishing powder product cutting force is 0.027mm/h, and the range estimation cut is 2/m
2
Embodiment 3
Its step of preparation process is with example 1, and rare earths salt is the muriate of cerium, lanthanum nitrate, and concentration is 0.9mol/L, and precipitation agent is a solid bicarbonate of ammonia.Adding is 4% Neutral ammonium fluoride by the polishing powder weight percent, be reflected at 75 ℃ and reacted 6 hours down,, be deposited in 800 ℃ of calcinings 50 ℃ of following ageings 30 hours, cross 300 mesh sieves behind the wet ball grinding, obtaining behind the centrifugal drying with the cerium lanthanum oxide is that core is the polishing material of shell with the lanthanum fluoride cerium.
Embodiment 4
With the cerium oxide that the prepares concentration that is made into soluble in water is 5% slurry, with salt acid for adjusting pH value to 3, it is 5: 1 that the adding lanthanum-cerium chloride makes the mol ratio of Ce-La/Ce, adding hydrofluoric acid stirred 3 hours as precipitation agent, with sedimentation and filtration, washing, drying, carry out after the roasting crossing 300 mesh sieves behind the wet ball grinding, obtaining shell lanthanum fluoride cerium core behind the centrifugal drying is the polishing material of the nucleocapsid structure of cerium oxide.
Embodiment 5
The solution of the Cerium II Chloride 2mol/L of being made into soluble in water is put into reactor, is the precipitation agent ammonia soln of 2.0mol/L with the concentration for preparing, and joins in the end liquid with the speed of 2L/min; After treating reinforced finishing, continued stirring reaction 5 hours, react fully and carry out, and obtain precipitation, the adding weight percent is 5% hydrofluoric acid, and the particle surface that precipitation obtains is fluoridized, and continues to stir for some time; Be deposited in 50 ℃ of following ageings 48 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the polishing material presoma, precursor powder obtains CeF 800 ℃ of calcinings
2Be shell CeO
2Be the powder of core, cross 500 mesh sieves behind the wet ball grinding, centrifugal drying obtains having the polishing material of nucleocapsid structure, and median size is 1.0um, and dispersity is 1.14, and specific surface area is 7.43m
2/ g.
Embodiment 6
The solution of the lanthanum-cerium chloride 2mol/L of being made into soluble in water is put into reactor, is an amount of precipitation agent ammonia soln of 2.0mol/L with the concentration for preparing, and joins in the end liquid with the speed of 2L/min; Treat reinforced finish afterreaction to finish to add weight percent be 5% nonionogenic tenside Macrogol 4000, the solution that adds the 1.0mol/L of cerous nitrate then adds precipitation agent 2.0mol/L ammonium fluoride solution again, continues stirring reaction 5 hours, react fully and carry out, and obtain precipitation; With the precipitation ageing at room temperature that obtains 48 hours; With precipitate and separate, collection, washing, drying, promptly obtain the polishing material presoma, precursor powder is 700 ℃ of calcinings, and obtaining oxidation lanthanum cerium is the powder of shell for the core cerium fluoride, cross 500 mesh sieves behind the wet ball grinding, centrifugal drying obtains having the polishing material of nucleocapsid structure.
Embodiment 7
With weight percent is that 7% Neutral ammonium fluoride solid joins in the cerium oxide, puts into High Temperature Furnaces Heating Apparatus simultaneously, and the calcining 6 hours down of temperature programming to 900 degree obtains the rare-earth polishing material of nucleocapsid structure through aftertreatment.Polishing powder is made 20% slurries, soft glass is polished, polishing powder product cutting force is 0.037mm/h, and the range estimation cut is 3/m
2Polishing powder is made 20% slurries, high-accuracy opticglass is polished, polishing powder product cutting force is 0.035mm/h, and the range estimation cut is 4/m
2
Embodiment 8
With the carbonate of cerium and oxalate and weight percent is that 10% ammonium bifluoride solid is put into High Temperature Furnaces Heating Apparatus, and the calcining 7 hours down of temperature programming to 850 degree obtains the rare-earth polishing material of nucleocapsid structure through aftertreatment.
Embodiment 9
With Citrate trianion, the stearate adding weight percent of cerium is that 5% hydrofluoric acid solution mixes, and puts into High Temperature Furnaces Heating Apparatus, and temperature programming to 750 degree was calcined 18 hours down, obtained the rare-earth polishing material of nucleocapsid structure through aftertreatment.
Embodiment 10
The hydrofluoric acid solution that ceria oxide powder is added weight percent 12% mixes, and puts into High Temperature Furnaces Heating Apparatus, and temperature programming to 750 degree was calcined 18 hours down, obtained the rare-earth polishing material of nucleocapsid structure through aftertreatment.Polishing powder is made 15% slurries, high-accuracy opticglass is polished, polishing powder product cutting force is 0.028mm/h, and the range estimation cut is 3/m
2Polishing powder is made 15% slurries, high-accuracy opticglass is polished, polishing powder product cutting force is 0.020mm/h, and the range estimation cut is 3/m
2
Claims (14)
1, a kind of rare-earth polishing material of nucleocapsid structure is characterized in that, this rare-earth polishing material is a powder, particulate state, and its kernel is the mineral compound based on rare earth oxide, shell is to contain rare earth oxide or/and the mineral compound of fluorochemical.
2, rare-earth polishing material according to claim 1 is characterized in that, shell is fluorine-containing mineral compound, and fluorine content is more than 2 times of fluorine content in the kernel, and the thickness of shell is 2nm-1 μ m.
3, rare-earth polishing material according to claim 1 is characterized in that, described shell contains rare earth oxide and/or fluorochemical, comprises the oxide compound of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium and in the fluorochemical one or more.
According to claim 1 or 3 described rare-earth polishing materials, it is characterized in that 4, shell is that cerium or lanthanum cerium oxide are or/and the mineral compound of fluorochemical.
5, rare-earth polishing material according to claim 1 is characterized in that, the mineral compound main body of kernel is a rare earth oxide, comprises in the oxide compound of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium one or more.
6, rare-earth polishing material according to claim 5 is characterized in that, the mineral compound main body of kernel is cerium or lanthanum cerium mixed oxide.
7, rare-earth polishing material according to claim 1 is characterized in that, kernel is CeO
2, shell is CeF
3, CeOF.
8, rare-earth polishing material according to claim 1 is characterized in that, the content of rare-earth polishing material middle-weight rare earths is weight percentage 50～99%, and the content of other compositions is weight percentage 0.9～50%, and other are unavoidable impurities＜0.1%.
9, rare-earth polishing material according to claim 1 is characterized in that, median size is calcined the back specific surface area down less than 20m at 800 ℃ between 0.02～3.0um
2/ g, dispersity is less than 2.0.
According to claim 1 or 9 described rare-earth polishing materials, it is characterized in that 10, median size is calcined the back specific surface area down less than 15m at 900 ℃ between 0.1～2.0um
2/ g, dispersity is less than 1.5.
11, a kind of preparation method who prepares the rare-earth polishing material of the described a kind of nucleocapsid structure of claim 1 adopts coprecipitation method, it is characterized in that concrete steps are:
1) nitrate, muriate, vitriol or their composite solution with nuclear matter is made into the solution that concentration is 0.05～2mol/L;
2) get precipitation agent: the mixture of one or more in ammoniacal liquor, bicarbonate of ammonia, the volatile salt, precipitation agent total concn are 0.1～2.0mol/L;
3) stirring joins precipitation agent in the salts solution of nuclear matter down, and stirring is continued in the reinforced back that finishes;
4) will form nitrate, muriate, vitriol or their composite solution of shell material and Neutral ammonium fluoride that concentration is 0.01～1.0mol/L or hydrofluoric acid joins above-mentioned solution simultaneously and makes and mix;
5) mixed solution is incubated ageing 0.5～48 hour down at 30 ℃～100 ℃, filters or centrifugation, obtain the presoma of polishing material after the drying; The presoma powder 600 ℃～1100 ℃ following calcinations, through dispersion, sorting or sieve, is obtained polishing powder from rare earth again, obtain having the polishing material of nucleocapsid structure.
12, preparation technology according to claim 11, it is characterized in that, add ammonium salt in the preparation process, in the tensio-active agent one or more are as additive and stir, add-on is the 0.01-10% of polishing powder gross weight, ammonium salt comprises ammonium chloride, ammonium nitrate, Neutral ammonium fluoride, ammonium sulfate, ammonium persulphate, monoammonium phosphate, ammonium bifluoride, ammonium molybdate, Tetrabutyl amonium bromide, the ammonium acetate ammonium formiate, ammonium sulfide, the sulphur ammonium, primary ammonium phosphate, Tetramethylammonium hydroxide, monoammonium sulfate, ammonium oxalate, ammonium polyphosphate, ammonium phosphomolybdate, ammonium phosphate, ammonium bisulfite, ammonium polyphosphate, tensio-active agent comprises anion surfactant, cats product, nonionogenic tenside, preferred polyoxyethylene glycol, polyethylene, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, Witconol AL 69-66, polyethylene anhydrous sorbitol Stearinsaeure, cetyl trimethylammonium bromide, Triton X-100.
13, the preparation method of the rare-earth polishing material of the described a kind of nucleocapsid structure of preparation claim 1, it is characterized in that, with the cerium oxide is nucleus, the mode that coats nucleation prepares the polishing powder of nucleocapsid structure, its concrete steps are: ceria oxide powder is dispersed in the solution that contains rare earth or other components, add Neutral ammonium fluoride or hydrofluoric acid that weight percent is 1%-10% again, make it form the fluorochemical precipitation on the cerium oxide surface, fully react after-filtration or centrifugation, obtain the presoma of polishing material after the drying; Obtain having the powder of nucleocapsid structure after the calcination, through dispersion, sorting or sieve, obtain the polishing material of nucleocapsid structure again.
14, the preparation method of the rare-earth polishing material of the described a kind of nucleocapsid structure of preparation claim 1, it is characterized in that, carbonate, oxalate, Citrate trianion, the stearate of cerium are added a kind of or two or more High Temperature Furnaces Heating Apparatuss of putting in hydrofluoric acid and the fluorochemical, calcining temperature was calcined 1-20 hour down at 700-1200 ℃, obtained the rare-earth polishing material of nucleocapsid structure again through aftertreatment.
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