KR20050063273A - 옥살레이트법에 의한 복합티탄산바륨계 파우더의 제조방법 - Google Patents
옥살레이트법에 의한 복합티탄산바륨계 파우더의 제조방법 Download PDFInfo
- Publication number
- KR20050063273A KR20050063273A KR1020030094658A KR20030094658A KR20050063273A KR 20050063273 A KR20050063273 A KR 20050063273A KR 1020030094658 A KR1020030094658 A KR 1020030094658A KR 20030094658 A KR20030094658 A KR 20030094658A KR 20050063273 A KR20050063273 A KR 20050063273A
- Authority
- KR
- South Korea
- Prior art keywords
- powder
- barium titanate
- barium
- composite
- oxalate
- Prior art date
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- 239000000843 powder Substances 0.000 title claims abstract description 71
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 42
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 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 35
- 239000000203 mixture Substances 0.000 title abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000002131 composite material Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 26
- 229910052788 barium Inorganic materials 0.000 claims abstract description 22
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- QKKWJYSVXDGOOJ-UHFFFAOYSA-N oxalic acid;oxotitanium Chemical compound [Ti]=O.OC(=O)C(O)=O QKKWJYSVXDGOOJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000654 additive Substances 0.000 claims abstract description 20
- 230000000996 additive effect Effects 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 11
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 10
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 8
- 239000011572 manganese Substances 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 12
- 239000011575 calcium Substances 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 239000010955 niobium Substances 0.000 claims description 6
- 238000001238 wet grinding Methods 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052689 Holmium Inorganic materials 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 150000001805 chlorine compounds Chemical class 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 150000004767 nitrides Chemical class 0.000 claims description 4
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 21
- 238000009826 distribution Methods 0.000 abstract description 13
- 239000000243 solution Substances 0.000 abstract description 9
- 239000003985 ceramic capacitor Substances 0.000 abstract description 5
- 230000003068 static effect Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract description 2
- WCMHZFHLWGFVCQ-UHFFFAOYSA-N [Ba].[Mn] Chemical compound [Ba].[Mn] WCMHZFHLWGFVCQ-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002994 raw material Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000010532 solid phase synthesis reaction Methods 0.000 description 5
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000003836 solid-state method Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- JBDFJDOQDLLTEY-UHFFFAOYSA-N [Ti][Mn][Ba] Chemical compound [Ti][Mn][Ba] JBDFJDOQDLLTEY-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-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
- XBYNNYGGLWJASC-UHFFFAOYSA-N barium titanium Chemical compound [Ti].[Ba] XBYNNYGGLWJASC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- PHGMGTWRSNXLDV-UHFFFAOYSA-N diethyl furan-2,5-dicarboxylate Chemical compound CCOC(=O)C1=CC=C(C(=O)OCC)O1 PHGMGTWRSNXLDV-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007935 neutral effect Effects 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
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
-
- 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
-
- 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
- H01G4/10—Metal-oxide dielectrics
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Ceramic Capacitors (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
구분 | 실시예 1 | 실시예 2 | 실시예 3 | 비교예 1 | 비교예 2 | |
금속함유 첨가제 | Mn | Y | Mn | Mn | Mn | |
BET | 4.356 | 4.015 | 4.772 | 5.612 | 5.783 | |
PSA(㎛) | D10 | 0.513 | 0.603 | 0.371 | 0.587 | 0.460 |
D50 | 1.010 | 1.224 | 0.715 | 1.484 | 1.024 | |
D100 | 3.01 | 3.20 | 3.25 | 23.44 | 25.13 | |
XRD | 이성질상발견안됨 | 이성질상발견안됨 | 이성질상발견안됨 | 이성질상발견안됨 | 이성질상발견안됨 |
Claims (6)
- 염화바륨(BaCl2)과 사염화티탄(TiCl4)의 혼합수용액을 옥살산(H2C2 O4) 수용액에 적가하여 바륨티타닐옥살레이트(BaTiO(C2O4)2ㆍ4H2O) 슬러리를 제조하는 단계;상기 제조된 바륨티타닐옥살레이트 슬러리에 산화물, 염화물 및 질화물 중에서 선택된 형태의 금속함유 첨가제와 혼합 습식분쇄한 후 건조하여 복합티타닐옥살레이트 파우더를 제조하는 단계;상기 제조된 복합티타닐옥살레이트 파우더를 열분해하여 복합티탄산바륨계(BaMTiO3) 파우더를 제조하는 단계; 및상기 복합티탄산바륨계 파우더를 재분쇄시키는 단계를 포함하는 것을 특징으로 하는 다음 화학식으로 표시되는 복합티탄산바륨계 파우더의 제조방법.[화학식](Ba1-xMx)m(Ti1-yMy)nO3상기 화학식에 있어서, 0.005 < x + y < 0.05이고 m/n 〉0.98 이다.
- 제 1 항에 있어서, 상기 금속함유 첨가제는 망간(Mn), 마그네슘(Mg), 칼슘(Ca), 지르코늄(Zr), 이트륨(Y), 홀뮴(Ho), 디그프로슘(Dy), 에르븀(Er), 이테르븀(Yb), 하프늄(Hf), 납(Pb), 스트론튬(Sr), 니오브(Nb) 및 탄탈(Ta) 중에서 선택된 1종 또는 2종 이상의 금속을 함유하는 산화물, 염화물 및 질화물인 것을 특징으로 하는 복합티탄산바륨계 파우더의 제조방법.
- 제 1 항에 있어서, 상기 복합티탄산바륨계(BaMTiO3) 파우더의 바륨(Ba) : 금속(M) 1 : 0.005 ∼ 0.05 의 몰비를 이루고 있는 것을 특징으로 하는 복합티탄산바륨계 파우더의 제조방법.
- 제 1 항에 있어서, 상기 혼합습식분쇄는 10 ∼ 300분 동안 수행되는 것을 특징으로 하는 복합티탄산바륨계 파우더의 제조방법.
- 제 1 항에 있어서, 상기 열분해는 가열속도가 0.5 ∼ 10 ℃/min이고, 유지온도가 700 ∼ 1200 ℃인 조건으로 수행하는 것을 특징으로 하는 복합티탄산바륨계 파우더의 제조방법.
- 제 1 항에 있어서, 상기 복합티탄산바륨계(BaMTiO3) 파우더는 페롭스카이드 구조인 것을 특징으로 하는 복합티탄산바륨계 파우더의 제조방법.
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KR1020030094658A KR100555400B1 (ko) | 2003-12-22 | 2003-12-22 | 옥살레이트법에 의한 복합티탄산바륨계 파우더의 제조방법 |
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KR1020030094658A KR100555400B1 (ko) | 2003-12-22 | 2003-12-22 | 옥살레이트법에 의한 복합티탄산바륨계 파우더의 제조방법 |
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KR20050063273A true KR20050063273A (ko) | 2005-06-28 |
KR100555400B1 KR100555400B1 (ko) | 2006-03-03 |
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Cited By (1)
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KR100955802B1 (ko) * | 2009-07-21 | 2010-05-06 | 한화케미칼 주식회사 | 미립 티탄산바륨계 분말의 제조방법 |
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KR101356990B1 (ko) * | 2013-09-25 | 2014-02-03 | 한국에너지기술연구원 | 형상이 조절된 철 옥살레이트 수화물 입자 및 그 제조방법, 이 철 옥살레이트 수화물 입자를 이용하여 제조된 산화철/탄소 복합체 및 그 제조방법 |
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KR100955802B1 (ko) * | 2009-07-21 | 2010-05-06 | 한화케미칼 주식회사 | 미립 티탄산바륨계 분말의 제조방법 |
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