JP5897043B2 - 石英ガラス適用のための高純度シリカ顆粒並びにその製造法 - Google Patents
石英ガラス適用のための高純度シリカ顆粒並びにその製造法 Download PDFInfo
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- JP5897043B2 JP5897043B2 JP2013554843A JP2013554843A JP5897043B2 JP 5897043 B2 JP5897043 B2 JP 5897043B2 JP 2013554843 A JP2013554843 A JP 2013554843A JP 2013554843 A JP2013554843 A JP 2013554843A JP 5897043 B2 JP5897043 B2 JP 5897043B2
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- purity silica
- silica
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- value
- silicate solution
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 185
- 239000000377 silicon dioxide Substances 0.000 title claims description 74
- 239000008187 granular material Substances 0.000 title claims description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 238000000034 method Methods 0.000 claims description 65
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000011521 glass Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000011148 porous material Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000002585 base Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000002535 acidifier Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 150000003141 primary amines Chemical class 0.000 claims description 2
- 150000003335 secondary amines Chemical class 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims 2
- 150000001412 amines Chemical class 0.000 claims 1
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 16
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 16
- 239000002253 acid Substances 0.000 description 15
- 238000001035 drying Methods 0.000 description 14
- 235000019353 potassium silicate Nutrition 0.000 description 14
- 238000001556 precipitation Methods 0.000 description 12
- 238000000197 pyrolysis Methods 0.000 description 12
- 125000005372 silanol group Chemical group 0.000 description 12
- 239000007787 solid Substances 0.000 description 10
- 239000012535 impurity Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- 150000007513 acids Chemical class 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 229910052814 silicon oxide Inorganic materials 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000008139 complexing agent Substances 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000005550 wet granulation Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910052729 chemical element Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012320 chlorinating reagent Substances 0.000 description 2
- 230000001143 conditioned effect Effects 0.000 description 2
- 150000002118 epoxides Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000012778 molding material Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- -1 silicon alkoxide Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 229910052915 alkaline earth metal silicate Inorganic materials 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003258 bubble free glass Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 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
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/124—Preparation of adsorbing porous silica not in gel form and not finely divided, i.e. silicon skeletons, by acidic treatment of siliceous materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/126—Preparation of silica of undetermined type
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/126—Preparation of silica of undetermined type
- C01B33/128—Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
- C03B19/106—Forming solid beads by chemical vapour deposition; by liquid phase reaction
- C03B19/1065—Forming solid beads by chemical vapour deposition; by liquid phase reaction by liquid phase reactions, e.g. by means of a gel phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1095—Thermal after-treatment of beads, e.g. tempering, crystallisation, annealing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/022—Purification of silica sand or other minerals
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/008—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in molecular form
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- 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
- C01P2006/14—Pore volume
-
- 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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Description
b.シリケート溶液を用意する工程であって、その際、殊に粘度を、沈殿によって精製された酸化ケイ素を製造するために、好ましくは特定の粘度範囲に設定することが可能である;有利なのは、殊に0.1〜10000ポアズの粘度であり、その際、この粘度範囲は、プロセス操作に応じて−後で説明するように−更なるプロセスパラメーターが条件となってさらに拡大され得る、
c.工程b)からのシリケート溶液を、工程a)からの装入物に、得られた沈殿懸濁液(Faellsuspension)のpH値が常に2.0より低く、有利には1.5より低く、特に有利には1.0より低く、極めて有利には0.5より低くなるように添加する工程、
d.得られたシリカを分離及び洗浄する工程であって、その際、洗浄媒体は、2.0より小さい、有利には1.5より小さい、特に有利には1.0より小さい、極めて有利には0.5より小さいpH値を有する、
e.シリカをVE水で、その電気伝導度が、100μSより低い値、有利には10μSより低い値を有するまで中性に洗浄する工程、
f.得られたシリカを乾燥する工程、
g.シリカを塩基で処理する工程、
h.シリカをVE水で洗浄し、乾燥し、そして乾燥された残留物を微粉砕する工程、
i.得られたシリカ顆粒を、200〜1000μm、有利には200〜600μm、特に有利には200〜400μm及び殊に250〜350μmの範囲の粒径画分に篩分する工程、
J.シリカ画分を、少なくとも600℃、有利には少なくとも1000℃、特に有利には少なくとも1200℃で焼結する工程。
1.)工程段階a.〜f.に従ったシリカの製造
14.1%の硫酸1800リットルを初めに装入し、そして、この初期装入物に水ガラス37/40の水溶液(密度=1350kg/m3、Na2O含有率=8%、SiO2含有率=26.8%、%SiO2/%Na2Oのモジュラス=3.35)350リットルをポンプ循環させながら1時間以内に加えた。添加するとミリメートルサイズの小球体が自然発生的に形成し、これらは流過可能な層を作り出し、かつ水ガラスを継続的に添加している間、初期装入物の内容分を篩板に通して800リットル/時間でポンプ循環させること若しくは液相を持続的に均質化することを可能にした。
例1
上記方法により製造された湿ったシリカ(固形分23.6%)500gに、5リットルのキャニスター内でVE水500g及び25%のアンモニア溶液50gを混ぜた。勢いよく振り動かした後、ネジで蓋を閉めた状態のこの混合物を一晩かけて乾燥キャビネット内でエージングした;温度は、アルカリエージングプロセスの間、80℃であった。翌日に、生成物を3000mlのビーカー(石英ガラス)に移し、かつ傾瀉洗浄した。計5回、そのつどVE水500mlで洗浄した;引き続き、ビーカー(石英ガラス)内の生成物を、160℃に調温された乾燥キャビネット内で一晩かけて乾燥した。乾燥した生成物を微粉砕し、かつ250〜350μmの画分に篩分した。この画分の20gを、1000mlのビーカー(石英ガラス)内で1050℃へとマッフル炉内で4時間以内に加熱し、かつ、この温度で1時間保った;冷却はゆっくりと、炉内に放置することによって行った。
上記方法により製造された湿ったシリカ(固形分35%)2000gに、5リットルのキャニスター内でVE水2000g及び25%のアンモニア溶液20gを混ぜた。勢いよく振り動かした後、ネジで蓋を閉めた状態のこの混合物を一晩かけて乾燥キャビネット内でエージングした;温度は、アルカリエージングプロセスの間、80℃であった。次の日に、生成物を5000mlのビーカー(石英ガラス)に移し、かつ傾瀉洗浄した。計3回、そのつどVE水1000mlで洗浄した;引き続き、磁気皿における生成物を、160℃に調温された乾燥キャビネット内で一晩かけて乾燥した。2000gを上回る収量を得るために、この処置を何回も繰り返した。乾燥した生成物を、3000mlの石英ガラスビーカー内で石英ガラスフラスコにより圧潰し、かつ125〜500μmの画分に篩分した。
例2で用いた湿ったシリカ(固形分35%)の一部を用いて、50℃でゆるやかに乾燥した後、振動による篩い分けによって、本発明による処理抜きに溶融してガラス棒とした材料の125〜500μm画分を製造した。シラノール基含有量の測定の試験は、この場合、ガラス棒の高い気泡含有量若しくはそれが原因である不透過性ゆえに失敗した。
溶融されるべきシリカ顆粒を、片側だけが溶封されたガラス管内に充填し、かつ高真空下で排気する。安定した真空が生じた後、ガラス棒を顆粒面より少なくとも20cm上回る高さで溶封する。引き続き、管内の粉末を酸水素ガスバーナーで溶融してガラス棒を形成する。該ガラス棒を約5mm厚の切片に切断し、そして面平行な端面を研磨して光沢を出す。ガラス切片の正確な厚みをノギスで測定し、かつ評価に含める。該切片を、IR測定装置の赤外光路に留める。シラノール基含有量のIR分光測定は、該切片のエッジ領域では行わず、それというのも、これは溶融物を包むガラス管の材料から成るからである。
窒素比表面積(BET表面積)を、ISO 9277に従って多点−表面積として測定する。
Claims (27)
- 0.01〜10.0ppmのアルカリ金属含有量、0.01〜10.0ppmのアルカリ土類金属含有量、0.001〜1.0ppmのホウ素含有量、0.001〜1.0ppmのリン含有量、0.01〜1.5ml/gの窒素細孔容積及び5〜200nmの最大細孔寸法を有し、かつ、0.01〜40.0ppmの炭素含有量を有することを特徴とする、高純度シリカ顆粒。
- 0.01〜1.0ml/gの窒素細孔容積を有することを特徴とする、請求項1に記載の高純度シリカ顆粒。
- 0.01〜0.6ml/gの窒素細孔容積を有することを特徴とする、請求項1又は2記載の高純度シリカ顆粒。
- 0.01〜100.0ppmの塩素含有量を有することを特徴とする、請求項1から3までのいずれか1項記載の高純度シリカ顆粒。
- 0.1〜2000μmの粒径分布を有することを特徴とする、請求項1から4までのいずれか1項記載の高純度シリカ顆粒。
- 10〜1000μmの粒径分布を有することを特徴とする、請求項1から5までのいずれか1項記載の高純度シリカ顆粒。
- 100〜800μmの粒径分布を有することを特徴とする、請求項1から5までのいずれか1項記載の高純度シリカ顆粒。
- ガラス製品を製造するための、請求項1から7までのいずれか1項記載の高純度シリカ顆粒の使用。
- 高純度シリカ顆粒の製造法であって、酸性化剤を含み2.0より小さいpH値を有する初期装入物への、粘度0.1〜10000ポアズのシリケート溶液の添加を、該添加中のpH値が常に2.0を下回っているという条件下で行い、引き続き、得られたシリカを、pH値が2.0より小さい酸性洗浄媒体で少なくとも一度処理し、その後、中性に洗浄された状態で塩基性処理に供し、最後に200〜1000μmの範囲の粒径画分の分離及び該粒径画分の少なくとも600℃での焼結を行い、前記シリカの塩基性処理を窒素含有塩基で行う、前記方法。
- 前記酸性化剤を含む初期装入物のpH値が1.5より小さい、請求項9に記載の方法。
- 前記酸性化剤を含む初期装入物のpH値が1.0より小さい、請求項9に記載の方法。
- 前記酸性化剤を含む初期装入物のpH値が0.5より小さい、請求項9に記載の方法。
- 添加した前記シリケート溶液の粘度が0.4〜1000ポアズである、請求項9から12までのいずれか1項記載の方法。
- 添加した前記シリケート溶液の粘度が5ポアズより大きい、請求項9から12までのいずれか1項記載の方法。
- 添加した前記シリケート溶液の粘度が2ポアズ未満である、請求項9から12までのいずれか1項記載の方法。
- 前記シリケート溶液の添加中のpH値が常に1.5を下回り、かつ前記洗浄媒体のpH値も同様に1.5を下回る、請求項9から15までのいずれか1項記載の方法。
- 前記シリケート溶液の添加中のpH値が常に1.0を下回り、かつ前記洗浄媒体のpH値も同様に1.0を下回る、請求項9から15までのいずれか1項記載の方法。
- 前記シリケート溶液の添加中のpH値が常に0.5を下回り、かつ前記洗浄媒体のpH値も同様に0.5を下回る、請求項9から15までのいずれか1項記載の方法。
- 前記塩基性処理前のシリカを、中性化のために使用した完全脱塩水が100μSを下回る電気伝導度を有するまで中性に洗浄する、請求項9から18までのいずれか1項記載の方法。
- 前記窒素含有塩基がアンモニアである、請求項9から19までのいずれか1項記載の方法。
- 前記窒素含有塩基が第一級アミン及び/若しくは第二級アミン及び/若しくは第三級アミンであるか又は前記アミンを包含する、請求項9から19までのいずれか1項記載の方法。
- 完全脱塩水による前記塩基性処理後のシリカを洗浄、乾燥及び微粉砕する、請求項9から21までのいずれか1項記載の方法。
- 200〜600μmの範囲の粒径画分を分離する、請求項9から22までのいずれか1項記載の方法。
- 200〜400μmの範囲の粒径画分を分離する、請求項9から22までのいずれか1項記載の方法。
- 250〜350μmの範囲の粒径画分を分離する、請求項9から22までのいずれか1項記載の方法。
- 分離された前記粒径画分の焼結を少なくとも1000℃で行う、請求項9から25までのいずれか1項記載の方法。
- 分離された前記粒径画分の焼結を少なくとも1200℃で行う、請求項9から25までのいずれか1項記載の方法。
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PCT/EP2012/052251 WO2012113655A1 (de) | 2011-02-22 | 2012-02-10 | Hochreines siliciumdioxidgranulat für quarzglasanwendungen sowie dessen herstellungsverfahren |
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- 2012-02-10 CN CN2012800100352A patent/CN103402933A/zh active Pending
- 2012-02-10 CN CN201810913825.0A patent/CN108658451A/zh active Pending
- 2012-02-10 RU RU2013142832/03A patent/RU2602859C2/ru active
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ES2628382T3 (es) | 2017-08-02 |
RU2013142832A (ru) | 2015-03-27 |
CA2827899C (en) | 2018-06-12 |
EP2678280B1 (de) | 2017-05-03 |
TW201247540A (en) | 2012-12-01 |
KR101911566B1 (ko) | 2018-10-24 |
KR20140022380A (ko) | 2014-02-24 |
TWI557073B (zh) | 2016-11-11 |
CN108658451A (zh) | 2018-10-16 |
RU2602859C2 (ru) | 2016-11-20 |
US20170066654A1 (en) | 2017-03-09 |
WO2012113655A1 (de) | 2012-08-30 |
DE102011004532A1 (de) | 2012-08-23 |
CN103402933A (zh) | 2013-11-20 |
JP2014514229A (ja) | 2014-06-19 |
PL2678280T3 (pl) | 2017-10-31 |
US20140072803A1 (en) | 2014-03-13 |
CA2827899A1 (en) | 2012-08-30 |
EP2678280A1 (de) | 2014-01-01 |
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