JP4060791B2 - チタン酸バリウム系粉末の製造方法 - Google Patents
チタン酸バリウム系粉末の製造方法 Download PDFInfo
- Publication number
- JP4060791B2 JP4060791B2 JP2003521152A JP2003521152A JP4060791B2 JP 4060791 B2 JP4060791 B2 JP 4060791B2 JP 2003521152 A JP2003521152 A JP 2003521152A JP 2003521152 A JP2003521152 A JP 2003521152A JP 4060791 B2 JP4060791 B2 JP 4060791B2
- Authority
- JP
- Japan
- Prior art keywords
- barium
- barium titanate
- group
- producing
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000843 powder Substances 0.000 title claims abstract description 69
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052788 barium Inorganic materials 0.000 claims abstract description 56
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 53
- QKKWJYSVXDGOOJ-UHFFFAOYSA-N oxalic acid;oxotitanium Chemical compound [Ti]=O.OC(=O)C(O)=O QKKWJYSVXDGOOJ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 28
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 239000000654 additive Substances 0.000 claims abstract description 19
- 230000000996 additive effect Effects 0.000 claims abstract description 15
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 13
- 239000011324 bead Substances 0.000 claims abstract description 12
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 12
- 150000001412 amines Chemical class 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 238000001238 wet grinding Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- 150000003868 ammonium compounds Chemical class 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 150000001413 amino acids Chemical class 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005695 Ammonium acetate Substances 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- 239000004475 Arginine Substances 0.000 claims description 2
- 239000004472 Lysine Substances 0.000 claims description 2
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 235000019257 ammonium acetate Nutrition 0.000 claims description 2
- 229940043376 ammonium acetate Drugs 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 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
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 125000005587 carbonate group Chemical group 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical group OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 150000001805 chlorine compounds Chemical class 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
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- BJAARRARQJZURR-UHFFFAOYSA-N trimethylazanium;hydroxide Chemical compound O.CN(C)C BJAARRARQJZURR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 abstract description 24
- 239000000203 mixture Substances 0.000 abstract description 11
- 238000005507 spraying Methods 0.000 abstract description 7
- 238000000197 pyrolysis Methods 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000000227 grinding Methods 0.000 description 7
- 239000012530 fluid Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 150000001768 cations Chemical class 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- -1 barium titanyl oxalate compound Chemical class 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000004063 acid-resistant material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 1
- PWHCIQQGOQTFAE-UHFFFAOYSA-L barium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ba+2] PWHCIQQGOQTFAE-UHFFFAOYSA-L 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- 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
- C01P2006/40—Electric properties
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
- C04B2235/3234—Titanates, not containing zirconia
- C04B2235/3236—Alkaline earth titanates
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/449—Organic acids, e.g. EDTA, citrate, acetate, oxalate
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5409—Particle size related information expressed by specific surface values
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/608—Green bodies or pre-forms with well-defined density
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/79—Non-stoichiometric products, e.g. perovskites (ABO3) with an A/B-ratio other than 1
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
塩化バリウム(BaCl2・2H2O)と四塩化チタン(TiCl4)との混合水溶液をシュウ酸(H2C2O4) 水溶液にノズルによって高速噴射することで、バリウムチタニルシュウ酸塩[BaTiO(C2O4)2・4H2O]の結晶を沈殿させる工程;
前記生成したバリウムチタニルシュウ酸塩の結晶に、アンモニア、アミン、アンモニウム化合物及びアミノ酸の中から選択された窒素含有添加剤を加えた後、ビーズミル(beads mill)を用いて湿式粉砕する工程;
熱分解して、チタン酸バリウム(BaTiO3)粉末を製造する工程;及び
前記得られたチタン酸バリウム粉末を再粉砕する工程
からなることを特徴とする。
(式中、R1、R2及びR3は、各々水素原子または炭素数1〜5のアルキル基であり;nは、1、2または3の整数であって、n=1の場合、Aはヒドロキシル基、硝酸基、重炭酸基、C1〜C10のカルボキシル基であり、n=2の場合、Aは硫酸基、炭酸基、C2〜C10のジカルボキシル基であり、n=3の場合、Aは燐酸基である。)
1モル/lの濃度のTiCl4水溶液1200lと1モル/lの濃度のBaCl2水溶液1320lを4M3のグラスライニングした(glass-lined)反応器に加え、よく混合し、混合溶液を作製した後、これを6M3の反応器に予め作製しておいた1モル/lの濃度のシュウ酸水溶液2520lに、例えばフルコーン(full-con)タイプなどの一流体ノズルによって21l/分の速度で噴射した。この際、シュウ酸溶液を、機械攪拌機を用いて150rpmの攪拌速度で攪拌しながら噴射し、シュウ酸溶液の温度は90℃に維持した。ノズルで噴射する時、混合溶液の供給ポンプとしてダイヤフラムポンプを使用した。シュウ酸溶液に混合物を2時間噴射した後、混合溶液を反応温度で1時間攪拌した後、室温で1時間攪拌して、バリウムチタニルシュウ酸塩のスラリーを製造した。
湿式粉砕時に使用したアンモニア水の使用量を各々異にした以外は前記実施例1と同様の方法でチタン酸バリウム粉末を製造し、得られたスラリーの特性の分析結果を次の表1に示した。
前記実施例1と同様の方法でバリウムチタニルシュウ酸塩を製造し、Ti対するBaのモル比が0.999であるバリウムチタニルシュウ酸塩(含水率24%)を得た。
湿式粉砕時に使用した添加剤の種類及び使用量を各々異にした以外は前記実施例1と同様の方法でチタン酸バリウム粉末を製造し、得られた粉砕前後のスラリーの特性の分析結果を次の表2に示した。
バリウムチタニルシュウ酸塩の結晶を粉砕する工程中に、アンモニア水と共にCaCO3及びZrO2をさらに添加したこと以外は前記実施例1と同様の方法でバリウムチタニルシュウ酸塩の結晶を製造した。その後、乾燥し、1190℃で熱分解(焼成)し、粉砕して、(Ba0.952Ca0.05)(Ti0.84Zr0.16)O3の粉末を製造した。
バリウムチタニルシュウ酸塩の結晶を粉砕する工程の際にアンモニア水を添加しなかったこと以外は前記実施例13と同様の方法で(Ba0.952Ca0.05)(Ti0.84Zr0.16)O3の粉末を製造した。
前記実施例13及び比較例2で製造したチタン酸バリウムの粉末にそれぞれPVA結合剤とY5V用のいくつかの添加剤を加えた。各混合物を、アルミナ乳鉢でよく混合し、乾燥した後、各混合物を前記乳鉢で粉砕し、顆粒を得るために篩にかけた。各顆粒のうち約0.4gを2トンで5秒プレスし、Ф10mmのディスクを鋳型で製作した。これに対して、いくつかの誘電特性を測定し、結果を表3に示した。
Claims (11)
- チタン酸バリウム系粉末の製造方法であり、該方法は、
塩化バリウム(BaCl2)と四塩化チタン(TiCl4)の混合水溶液を、シュウ酸(H2C2O4) 水溶液にノズルによって高速噴射することによって沈殿させ、熟成させ、濾過し、洗浄して、バリウムチタニルシュウ酸塩[BaTiO(C2O4)2・4H2O]の結晶を得る工程;
前記得られたバリウムチタニルシュウ酸塩の結晶にアンモニア、アミン、アンモニウム化合物及びアミノ酸の中から選択された窒素含有添加剤を加えた後、ビーズミル(beads mill)を用いて湿式粉砕し、乾燥し、熱分解して、チタン酸バリウム(BaTiO3)粉末を製造する工程;及び
前記得られたチタン酸バリウム粉末を再粉砕する工程
からなることを特徴とする、チタン酸バリウム系粉末の製造方法。 - 前記窒素含有添加剤は、バリウムチタニルシュウ酸塩のモル数に対して0.5〜20モル%の範囲内で使用することを特徴とする、請求項1に記載のチタン酸バリウム系粉末の製造方法。
- 前記アミンは、メチルアミン、ジメチルアミン、トリメチルアミン、ジエチルアミン及びトリエチルアミンからなる群より選択されることを特徴とする、請求項3に記載のチタン酸バリウム系粉末の製造方法。
- 前記アンモニウム化合物は、水酸化アンモニウム、炭酸アンモニウム、酢酸アンモニウム、燐酸アンモニウム、シュウ酸アンモニウム、重炭酸アンモニウム及びトリメチルアンモニウムヒドロキシドからなる群より選択されることを特徴とする、請求項5に記載のチタン酸バリウム系粉末の製造方法。
- 前記アミノ酸は、アルギニン及びリジンからなる群より選択されることを特徴とする、請求項1に記載のチタン酸バリウム系粉末の製造方法。
- 前記窒素含有添加剤と共に、二価又は四価の金属を使用することを特徴とする、請求項1に記載のチタン酸バリウム系粉末の製造方法。
- 前記二価の金属は、Mg、Ca、Sr及びPbからなる群より少なくとも1種以上選択されることを特徴とする、請求項8に記載のチタン酸バリウム系粉末の製造方法。
- 前記四価の金属は、Zr、Hf及びSnからなる群より少なくとも1種以上選択されることを特徴とする、請求項8に記載のチタン酸バリウム系粉末の製造方法。
- 前記金属の形態は、前記金属の酸化物、炭酸塩、塩化物及び硝酸塩の中から選択されることを特徴とする、請求項8乃至請求項10のいずれか一つの請求項に記載のチタン酸バリウム系粉末の製造方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR10-2001-0049048A KR100434883B1 (ko) | 2001-08-14 | 2001-08-14 | 티탄산바륨계 파우더의 제조방법 |
PCT/KR2002/000836 WO2003016219A1 (en) | 2001-08-14 | 2002-05-06 | Method for preparing barium-titanate based powder |
Publications (3)
Publication Number | Publication Date |
---|---|
JP2005500239A JP2005500239A (ja) | 2005-01-06 |
JP2005500239A5 JP2005500239A5 (ja) | 2005-11-17 |
JP4060791B2 true JP4060791B2 (ja) | 2008-03-12 |
Family
ID=19713199
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2003521152A Expired - Fee Related JP4060791B2 (ja) | 2001-08-14 | 2002-05-06 | チタン酸バリウム系粉末の製造方法 |
Country Status (9)
Country | Link |
---|---|
US (1) | US7179441B2 (ja) |
EP (1) | EP1441985B1 (ja) |
JP (1) | JP4060791B2 (ja) |
KR (1) | KR100434883B1 (ja) |
CN (1) | CN1272251C (ja) |
AT (1) | ATE372301T1 (ja) |
DE (1) | DE60222289T2 (ja) |
TW (1) | TWI243150B (ja) |
WO (1) | WO2003016219A1 (ja) |
Families Citing this family (32)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070122698A1 (en) | 2004-04-02 | 2007-05-31 | Maxwell Technologies, Inc. | Dry-particle based adhesive and dry film and methods of making same |
US20050266298A1 (en) * | 2003-07-09 | 2005-12-01 | Maxwell Technologies, Inc. | Dry particle based electro-chemical device and methods of making same |
US7318897B2 (en) | 2003-08-14 | 2008-01-15 | Ferro Corporation | Method of removing spectator ions from aqueous suspension of solid particles |
JP4684657B2 (ja) | 2005-01-07 | 2011-05-18 | 日本化学工業株式会社 | 蓚酸バリウムチタニル粉末の製造方法及びチタン系ペロブスカイト型セラミック原料粉末の製造方法 |
KR100708488B1 (ko) * | 2006-06-16 | 2007-04-18 | 한국화학연구원 | 유기용매에 대한 분산성이 우수한 결정성 바륨티타네이트의제조 방법 |
US8137647B2 (en) * | 2006-12-28 | 2012-03-20 | E. I. Du Pont De Nemours And Company | Processes for producing titanium dioxide |
KR101426345B1 (ko) * | 2007-01-29 | 2014-08-07 | 삼성전기주식회사 | 옥살레이트 공정에 의한 티탄산바륨 분말의 제조방법 및 그방법에 의하여 제조된 티탄산바륨 분말 |
KR101551853B1 (ko) * | 2008-04-03 | 2015-09-08 | 사켐,인코포레이티드 | 오늄 디카르복실레이트를 사용하여 세라믹 분말을 제조하는 방법 |
KR101451987B1 (ko) * | 2008-05-14 | 2014-10-21 | 삼성전기주식회사 | 옥살레이트 공정에 의한 고결정성의 티탄산바륨 미분말의 제조방법 및 그 방법에 의하여 제조된 고결정성의 티탄산바륨 미분말 |
PL2411141T3 (pl) | 2009-03-23 | 2014-06-30 | Vaelinge Photocatalytic Ab | Wytwarzanie zawiesiny nanocząsteczek koloidalnych ditlenku tytanu z zachowaniem krystaliczności za pomocą młyna kulkowego z kulkami o rozmiarach mikrometrowych |
CN101708861B (zh) * | 2009-11-09 | 2011-12-21 | 贵州红星发展股份有限公司 | 一种制备钛酸钡的方法 |
CN101891466B (zh) * | 2010-07-21 | 2012-12-19 | 陕西科技大学 | 一种板状钛酸钡纳米粉体的制备方法 |
RU2607558C2 (ru) | 2011-07-05 | 2017-01-10 | Велинге Фотокаталитик Аб | Изделия из древесины с покрытием и способ получения изделий из древесины с покрытием |
JP5879078B2 (ja) | 2011-09-15 | 2016-03-08 | 日本化学工業株式会社 | シュウ酸バリウムチタニルの製造方法及びチタン酸バリウムの製造方法 |
CN104203406B (zh) | 2012-03-20 | 2019-03-12 | 瓦林格光催化股份有限公司 | 包含二氧化钛和抗光致变灰添加剂的光催化组合物 |
US9375750B2 (en) | 2012-12-21 | 2016-06-28 | Valinge Photocatalytic Ab | Method for coating a building panel and a building panel |
KR101770701B1 (ko) | 2012-12-21 | 2017-09-06 | 삼성전자주식회사 | 티탄산 바륨을 포함한 이산화탄소 흡착제, 이를 포함한 이산화탄소 포집 모듈, 및 이를 이용한 이산화탄소 분리 방법 |
CN103964839B (zh) * | 2013-01-30 | 2015-12-02 | 比亚迪股份有限公司 | 一种正温度系数热敏电阻材料及其制备方法 |
MY180856A (en) | 2013-09-25 | 2020-12-10 | Valinge Photocatalytic Ab | A method of applying a photo catalytic dispersion and a method of manufacturing a panel |
WO2015099203A1 (ko) * | 2013-11-26 | 2015-07-02 | 삼성전기 주식회사 | 바륨티타닐옥살레이트의 제조방법, 티탄산바륨의 제조방법, 및 티탄산바륨 |
KR20150060303A (ko) * | 2013-11-26 | 2015-06-03 | 삼성전기주식회사 | 바륨티타닐옥살레이트의 제조방법 및 티탄산바륨의 제조방법 |
KR20150060190A (ko) * | 2013-11-26 | 2015-06-03 | 삼성전기주식회사 | 티탄산바륨의 제조방법 및 이로부터 제조되는 티탄산바륨 |
JP6217599B2 (ja) * | 2014-11-17 | 2017-10-25 | 株式会社村田製作所 | チタン酸バリウム系粉末の製造方法 |
JP6871235B2 (ja) | 2016-04-01 | 2021-05-12 | デンカ株式会社 | チタン酸バリウム質粉末及びその製造方法、用途 |
CN108117097B (zh) * | 2017-12-11 | 2020-06-19 | 浙江蓝天知识产权运营管理有限公司 | 一种粒径均匀纳米钛酸钡的制备方法 |
WO2021010368A1 (ja) * | 2019-07-16 | 2021-01-21 | 日本化学工業株式会社 | Me元素置換有機酸バリウムチタニル、その製造方法及びチタン系ペロブスカイト型セラミック原料粉末の製造方法 |
JP7438867B2 (ja) | 2019-07-16 | 2024-02-27 | 日本化学工業株式会社 | Me元素置換有機酸バリウムチタニル、その製造方法及びチタン系ペロブスカイト型セラミック原料粉末の製造方法 |
JP7102462B2 (ja) | 2020-06-12 | 2022-07-19 | 日本化学工業株式会社 | シュウ酸バリウムチタニル、その製造方法及びチタン酸バリウムの製造方法 |
WO2022107695A1 (ja) | 2020-11-19 | 2022-05-27 | 日本化学工業株式会社 | シュウ酸バリウムチタニルの製造方法及びチタン酸バリウムの製造方法 |
CN113174233B (zh) * | 2021-04-27 | 2022-11-11 | 南京林业大学 | 一种防静电无醛胶黏剂及其制备方法及应用 |
JP7524129B2 (ja) | 2021-05-13 | 2024-07-29 | 日本化学工業株式会社 | 誘電体セラミック形成用組成物及び誘電体セラミック材料 |
CN114213120B (zh) * | 2021-11-29 | 2023-03-07 | 深圳市信维通信股份有限公司 | 用于小尺寸mlcc的介质材料及其制备方法与电容器 |
Family Cites Families (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61146710A (ja) * | 1984-12-19 | 1986-07-04 | Central Glass Co Ltd | 高純度チタン酸バリウム微粒子の製造方法 |
US5219811A (en) * | 1989-08-31 | 1993-06-15 | Central Glass Company, Limited | Powder composition for sintering into modified barium titanate semiconductive ceramic |
US5468427A (en) * | 1993-09-27 | 1995-11-21 | Alfred University | Process for making ultra-fine ceramic particles |
US5523065A (en) * | 1993-09-27 | 1996-06-04 | Alfred University | Process for making ultra-fine barium titanate particles |
SG48535A1 (en) * | 1996-08-05 | 1998-04-17 | Murata Manufacturing Co | Dielectric ceramic composition and monolithic ceramic capacitor using the same |
JP2000189830A (ja) * | 1998-12-28 | 2000-07-11 | Chufun Hightech Kk | 微粒子分散体の製法および微粒子分散体 |
KR100360118B1 (ko) * | 1999-07-05 | 2002-11-04 | 삼성전기주식회사 | 옥살레이트법에 의한 티탄산바륨계 산화물 분말 제조방법 |
JP3361091B2 (ja) * | 2000-06-20 | 2003-01-07 | ティーディーケイ株式会社 | 誘電体磁器および電子部品 |
US6409983B1 (en) * | 2000-07-11 | 2002-06-25 | Korea Institute Of Science And Technology | Process for preparing crystalline barium titanate powder |
TW527321B (en) * | 2000-08-09 | 2003-04-11 | Samsung Electro Mech | A method for producing barium titanate based powders by oxalate process |
KR100414832B1 (ko) * | 2001-02-22 | 2004-01-13 | 삼성전기주식회사 | 고품질 티탄산바륨계 파우더의 제조방법 |
US6692721B2 (en) * | 2002-01-15 | 2004-02-17 | Samsung Electro-Mechanics Co., Ltd. | Method for preparing barium titanate powder by oxalate synthesis |
-
2001
- 2001-08-14 KR KR10-2001-0049048A patent/KR100434883B1/ko not_active IP Right Cessation
-
2002
- 2002-05-02 TW TW091109178A patent/TWI243150B/zh not_active IP Right Cessation
- 2002-05-06 CN CNB028159187A patent/CN1272251C/zh not_active Expired - Fee Related
- 2002-05-06 JP JP2003521152A patent/JP4060791B2/ja not_active Expired - Fee Related
- 2002-05-06 EP EP02730930A patent/EP1441985B1/en not_active Expired - Lifetime
- 2002-05-06 WO PCT/KR2002/000836 patent/WO2003016219A1/en active IP Right Grant
- 2002-05-06 AT AT02730930T patent/ATE372301T1/de not_active IP Right Cessation
- 2002-05-06 DE DE60222289T patent/DE60222289T2/de not_active Expired - Lifetime
- 2002-05-06 US US10/486,695 patent/US7179441B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
ATE372301T1 (de) | 2007-09-15 |
EP1441985B1 (en) | 2007-09-05 |
WO2003016219A1 (en) | 2003-02-27 |
US7179441B2 (en) | 2007-02-20 |
CN1272251C (zh) | 2006-08-30 |
DE60222289D1 (de) | 2007-10-18 |
EP1441985A1 (en) | 2004-08-04 |
US20040253172A1 (en) | 2004-12-16 |
DE60222289T2 (de) | 2008-05-29 |
TWI243150B (en) | 2005-11-11 |
JP2005500239A (ja) | 2005-01-06 |
KR20030015011A (ko) | 2003-02-20 |
CN1541188A (zh) | 2004-10-27 |
KR100434883B1 (ko) | 2004-06-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP4060791B2 (ja) | チタン酸バリウム系粉末の製造方法 | |
JP4401237B2 (ja) | チタン酸バリウムの製造方法 | |
JP3798652B2 (ja) | シュウ酸塩工程によるチタン酸バリウム系粉末の製造方法 | |
JP2002211926A (ja) | 球状チタン酸バリウム粒子粉末及びその製造法 | |
JP4064241B2 (ja) | 高品質チタン酸バリウム系パウダーの製造方法 | |
JP4702515B2 (ja) | 正方晶系チタン酸バリウム微粒子粉末及びその製造法 | |
KR100955802B1 (ko) | 미립 티탄산바륨계 분말의 제조방법 | |
KR20090118748A (ko) | 옥살레이트 공정에 의한 고결정성의 티탄산바륨 미분말의제조방법 및 그 방법에 의하여 제조된 고결정성의티탄산바륨 미분말 | |
JPH07277710A (ja) | ペロブスカイト型複合酸化物粉末の製造方法 | |
JP4671618B2 (ja) | チタン酸カルシウムおよびその製造方法 | |
TW202136153A (zh) | 鈣鈦礦型化合物之製造方法及鈣鈦礦型化合物 | |
JP6573653B2 (ja) | ペロブスカイト型チタン酸バリウム粉末の製造方法 | |
KR100921352B1 (ko) | 미립 티탄산바륨계 분말의 제조방법 | |
KR100395218B1 (ko) | BaTiO3계 분말 제조 방법 | |
KR20150060188A (ko) | 바륨티타닐옥살레이트의 제조방법 및 티탄산바륨의 제조방법 | |
TWI576314B (zh) | 鈦酸鋇之製備方法及由其所製備之鈦酸鋇 | |
KR20060102928A (ko) | 티탄산바륨 분말의 제조방법 | |
KR100435534B1 (ko) | 티탄산바륨의 제조방법 | |
JP3393157B2 (ja) | 多結晶半導体繊維およびその製造方法 | |
KR100558460B1 (ko) | 옥살레이트 공정에 의한 초미립 티탄산바륨계 분말의 제조방법 | |
JPS61127624A (ja) | ペロブスカイト型酸化物固溶体の製造方法 | |
KR20150060303A (ko) | 바륨티타닐옥살레이트의 제조방법 및 티탄산바륨의 제조방법 | |
JPH04132614A (ja) | ペロブスカイト型複合酸化物粉末の製造方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20070508 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20070808 |
|
RD03 | Notification of appointment of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7423 Effective date: 20070808 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20071005 |
|
TRDD | Decision of grant or rejection written | ||
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A821 Effective date: 20071005 |
|
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20071204 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20071220 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101228 Year of fee payment: 3 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 4060791 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101228 Year of fee payment: 3 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20111228 Year of fee payment: 4 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121228 Year of fee payment: 5 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121228 Year of fee payment: 5 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131228 Year of fee payment: 6 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313117 |
|
S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
R360 | Written notification for declining of transfer of rights |
Free format text: JAPANESE INTERMEDIATE CODE: R360 |
|
R360 | Written notification for declining of transfer of rights |
Free format text: JAPANESE INTERMEDIATE CODE: R360 |
|
R371 | Transfer withdrawn |
Free format text: JAPANESE INTERMEDIATE CODE: R371 |
|
S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313117 |
|
R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
LAPS | Cancellation because of no payment of annual fees |