CN103030403A - Perovskite powder, fabricating method thereof and multi-layer ceramic electronic parts fabricated by using the same - Google Patents
Perovskite powder, fabricating method thereof and multi-layer ceramic electronic parts fabricated by using the same Download PDFInfo
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- CN103030403A CN103030403A CN2012100017516A CN201210001751A CN103030403A CN 103030403 A CN103030403 A CN 103030403A CN 2012100017516 A CN2012100017516 A CN 2012100017516A CN 201210001751 A CN201210001751 A CN 201210001751A CN 103030403 A CN103030403 A CN 103030403A
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- powder
- uhligite
- salt
- uhligite powder
- coating
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- 239000000843 powder Substances 0.000 title claims abstract description 130
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000919 ceramic Substances 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 56
- 150000003839 salts Chemical class 0.000 claims abstract description 31
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 30
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000005864 Sulphur Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims description 40
- 238000000576 coating method Methods 0.000 claims description 40
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 19
- 229910044991 metal oxide Inorganic materials 0.000 claims description 14
- 150000004706 metal oxides Chemical class 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 11
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- -1 rare-earth salts Chemical class 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- 238000010335 hydrothermal treatment Methods 0.000 claims description 4
- 150000003016 phosphoric acids Chemical class 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 7
- 239000011247 coating layer Substances 0.000 abstract 3
- 239000010410 layer Substances 0.000 abstract 1
- 150000003568 thioethers Chemical class 0.000 abstract 1
- 229910002113 barium titanate Inorganic materials 0.000 description 47
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 47
- 238000002360 preparation method Methods 0.000 description 15
- 239000003985 ceramic capacitor Substances 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000010936 titanium Substances 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 3
- 229910001863 barium hydroxide Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001935 peptisation Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000003991 Rietveld refinement Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000015654 memory Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 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
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- YBCVMFKXIKNREZ-UHFFFAOYSA-N acoh acetic acid Chemical compound CC(O)=O.CC(O)=O YBCVMFKXIKNREZ-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-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
- 239000011230 binding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 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
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- QVLTXCYWHPZMCA-UHFFFAOYSA-N po4-po4 Chemical compound OP(O)(O)=O.OP(O)(O)=O QVLTXCYWHPZMCA-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 230000003019 stabilising effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 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
- H01G4/30—Stacked capacitors
-
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
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- 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
- C04B2235/76—Crystal structural characteristics, e.g. symmetry
- C04B2235/768—Perovskite structure ABO3
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- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
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- Microelectronics & Electronic Packaging (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Ceramic Capacitors (AREA)
Abstract
The invention provides perovskite powder, a fabricating method thereof and multi-layer ceramic electronic parts fabricated by using the same. The perovskite powder comprises a coating layer formed on the surface of the perovskite powder particles. The coating layer is formed by one or a plurality of groups among groups formed by sulfides and salts having sulphur. When the perovskite powder is synthesized by means of a hydrothermal synthesis method, the perovskite powder can have particles with high degree of crystallinity to inhibit the growth of particles through forming one or multiple coating layers selected from sulfide and salt having sulphur.
Description
The cross reference of related application
The application requires to be committed on October 10th, 2011 right of priority of the patent application No.10-2011-0103194 of Korea S Department of Intellectual Property, and the content of this application is introduced among the application with for referencial use.
Technical field
The present invention relates to uhligite powder of a kind of particulate with high-crystallinity and preparation method thereof, and the laminated ceramic electronic component that uses this uhligite powder preparation.
Background technology
The uhligite powder is ferroelectric ceramic material, is used as for example starting material of laminated ceramic capacitor (MLCC), porcelain filter, piezoelectric element (piezoelectric elements), ferroelectric memory (ferroelectric memories), thermistor and voltage dependent resistor of electronic component.
Barium titanate (BaTiO
3) be the high dielectric material with perovskite structure, as the dielectric substance of laminated ceramic capacitor.
According to the electronic component light weight that in electronic industry, has heavy body and high reliability, slim and undersized recent trend, the size that needs ferroelectric particles to have to reduce and excellent insulation characterisitic and reliability.
When the median size as the barium titanate powder of the main component of dielectric layer increased, the surfaceness of described dielectric layer also increased, thereby increases the possibility of short circuit and cause insulation resistance not enough.
Therefore, need reduction as the median size of the barium titanate powder of dielectric layer main component.
Yet, when the median size of barium titanate powder reduces, may be disadvantageous because the tetragonal system ratio may reduce, so, need exploitation to have high-crystallinity and contain fine-grained barium titanate powder, so as to prevent degree of crystallinity unfavorable.
The example of preparation uhligite powder method comprises solid state process and wet method, and the example of wet method comprises oxalate precipitation method and hydrothermal synthesis method.
Be difficult to adopt solid state process to prepare and contain fine-grained uhligite powder, because the smallest particles size of uhligite powder is sizable usually, be approximately 1 micron, solid state process may be difficult to control particle size, and particle may lump and may occur polluting in sintering process.
In various techniques, along with the median size of uhligite powder reduces, tetragonality can reduce usually, and is reduced to 100nm when following when the median size of electrolyte granular, may be difficult to guarantee crystallographic axis (c/a) ratio of being scheduled to.
Further, when reducing, the particle size of powder is difficult to guarantee to disperse.Therefore, in fine-particle powder, need high dispersibility.
In known solid state method or coprecipitation method, at high temperature use calcining to form crystalline phase, therefore, need high-temperature calcination and attrition process.
Therefore, shortcoming is that the shape of the uhligite powder particle that synthesizes is unsatisfactory, and the distribution of median size is wide, and because caking may appear in thermal treatment, disperses thereby hinder.
Summary of the invention
One aspect of the present invention provides uhligite powder with high-crystallinity particulate and preparation method thereof, and the laminated ceramic electronic component that uses this uhligite powder preparation.
According to an aspect of the present invention, the uhligite powder is provided, described uhligite powder contains the coating on the surface that is formed on described uhligite powder particle (grain), and described coating is selected from the group that is comprised of sulfide and the salt (salt including sulfur) that contains sulphur one or more.
Described sulfide can comprise ammonium sulfate, and the described salt that contains sulphur can comprise and is selected from the group that is comprised of phosphoric acid salt (phosphate) and acetate (acetate) one or more.
Described coating can have the thickness of 0.1-10nm.
Described uhligite powder can comprise and being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that (0＜x＜1) forms one or more.
Described uhligite powder can have the median size of 10-150nm and the crystallographic axis of 1.001-1.010 (c/a) ratio.
According to a further aspect in the invention, provide a kind of method for preparing the uhligite powder, the method comprises that mixed metal salt and metal oxide are to form the uhligite granular core; Mix described uhligite granular core and be dissolved in being selected from by sulfide and containing in the group that the salt of sulphur forms one or more in pure water, with the formation mixture; And utilize hydrothermal treatment consists to grow particle with the described uhligite powder of the coating that obtains comprising the surface that is formed on described uhligite powder particle from described mixture, and described coating is selected from by sulfide and contains in the group that the salt of sulphur forms one or more.
Described sulfide can comprise ammonium sulfate, and the described salt that contains sulphur can comprise and is selected from the group that is comprised of phosphoric acid salt and acetate one or more.
Described metal-salt comprises the mixture of hydrated barta or hydrated barta and rare-earth salts, and described metal oxide can comprise titanium oxide or zirconium white.
Described coating can have the thickness of 0.1-10nm.
Described uhligite powder can have the median size of 10-150nm, comprises being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that (0＜x＜1) forms one or more, and crystallographic axis (c/a) ratio with 1.001-1.010.
According to a further aspect in the invention, provide a kind of laminated ceramic electronic component, described laminated ceramic electronic component comprises ceramic main body, and described ceramic main body has dielectric layer and inner electrode layer; Described dielectric layer comprises the uhligite powder, and described uhligite powder has the coating on the surface that is formed on described uhligite powder particle, and described coating is selected from the group that is comprised of sulfide and the salt that contains sulphur one or more; When having described dielectric layer in described ceramic main body inside when being inserted between the inner electrode layer, described inner electrode layer toward each other.
Described coating can have the thickness of 0.1-10nm.
Described uhligite powder can comprise and being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that (0＜x＜1) forms one or more, and have crystallographic axis (c/a) ratio of 1.001-1.010.
Description of drawings
To more clearly understand above-mentioned aspect of the present invention and other aspects, feature and other advantages from the detailed description below in conjunction with accompanying drawing, wherein:
Fig. 1 is the skeleton view that schematically shows laminated ceramic capacitor according to the embodiment of the present invention;
Fig. 2 is that Fig. 1 is along the sectional view of A-A ' line;
Fig. 3 is the schema that shows the method for preparing according to the embodiment of the present invention the uhligite powder;
Fig. 4 A to Fig. 4 C be according to the embodiment of the present invention the barium titanate powder particle and according to scanning electronic microscope (SEM) figure of the barium titanate powder particle of correlation technique; And
Fig. 5 A is scanning transmission electron microscope (STEM) figure that relies on according to the embodiment of the present invention the barium titanate powder of temperature variation to Fig. 5 C.
Embodiment
Describe embodiments of the present invention in detail below with reference to accompanying drawing.
Yet the present invention can be with multiple multi-form performance and should be interpreted as being limited to embodiment in this setting.Or rather, provide these embodiments in order to disclose the present invention thoroughly with complete, and pass on fully scope of the present invention to those skilled in the art.In the accompanying drawings, for clear, the shape and size of assembly may enlarge, and identical reference number runs through in full use to indicate identical or close assembly.
Uhligite powder according to the embodiment of the present invention has the coating on the surface that is formed on described uhligite powder particle, and described coating is selected from the group that is comprised of sulfide and the salt that contains sulphur one or more.
Described uhligite powder is not particularly limited, and still, for example, comprises being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that (0＜x＜1) forms one or more.
Described uhligite powder according to the embodiment of the present invention especially, adopts barium titanate (BaTiO
3) powder, but the present invention is not limited to this.
According to the embodiment of the present invention, use the described barium titanate (BaTiO of hydrothermal synthesis method preparation
3) powder contains the coating on the surface that is formed on described barium titanate powder particle, and described coating is selected from by sulfide and contains in the group that the salt of sulphur forms one or more, thereby high-crystallinity and particulate are provided.
Described sulfide and the described salt that contains sulphur are not particularly limited, still, for example, ammonium sulfate and be selected from the group that is formed by phosphoric acid salt and acetate one or more.
In known Hydrothermal Synthesis process, need to reduce temperature of reaction in order to reduce barium titanate (BaTiO
3) particle size of powder, but the degree of crystallinity of powder can reduce.Reaction needed at high temperature carries out guaranteeing high-crystallinity, but particle size can increase.
Yet, according to the embodiment of the present invention, owing to be formed with on the surface of described barium titanate powder particle and be selected from by sulfide and contain one or more coating in the group that the salt of sulphur forms, even thereby reaction is at high temperature carried out, also can suppress the particle growth of powder, therefore high-crystallinity and particulate are provided.
The thickness of described coating is not particularly limited, still, for example, 0.1-10nm.
Even the particle growth of barium titanate powder is at high temperature carried out, also can be at described barium titanate (BaTiO
3) form on the surface of powder particle have 0.1-10nm thickness coating to suppress the particle growth of powder, therefore reduced particle size.
When the thickness of described coating during less than 0.1nm, in the process that particle is at high temperature grown, be not enough to suppress barium titanate (BaTiO
3) particle growth of powder to be to prevent the formation of fine-particle powder.
Further, when the thickness of described coating during greater than 10nm, reduced barium titanate (BaTiO
3) specific inductivity of powder.
According to the embodiment of the present invention, prepared and have high-crystallinity and contain fine-grained described barium titanate (BaTiO
3) powder, and especially, described barium titanate (BaTiO
3) powder has the median size of 10-150nm and the crystallographic axis of 1.001-1.010 (c/a) ratio.
Fig. 1 is the skeleton view that schematically shows laminated ceramic capacitor according to the embodiment of the present invention.
Fig. 2 is that Fig. 1 is along the sectional view of A-A ' line.
Referring to Fig. 1 and Fig. 2, laminated ceramic electronic component according to the embodiment of the present invention comprises ceramic main body 10, and described ceramic main body 10 comprises dielectric layer 1 and inner electrode layer 21 and 22; Described dielectric layer 1 comprises the uhligite powder, and described uhligite powder has the coating that is formed on described uhligite powder particle surface, and described coating is selected from the group that is comprised of sulfide and the salt that contains sulphur one or more; When having described dielectric layer 1 in described ceramic main body 10 inside when being inserted between inner electrode layer 21 and 22, described inner electrode layer 21 and 22 toward each other.
Description according to the described laminated ceramic electronic component of embodiment of the present invention is carried out with reference to laminated ceramic capacitor, but the present invention is not limited to this.
In the laminated ceramic capacitor according to embodiment of the present invention, the L direction of Fig. 1 is called length direction, and the W direction is called width, and the T direction is called thickness direction.Described thickness direction has identical meaning with the direction of lamination dielectric layer, that is, and and laminating direction.
According to the embodiment of the present invention, the material that is used for dielectric layer 1 is not particularly limited, as long as it can guarantee enough electric capacity.For example, can use barium titanate (BaTiO
3) powder.
Described barium titanate (BaTiO
3) powder can have and be formed on described barium titanate (BaTiO
3) coating on surface of powder particle, and described coating is selected from by sulfide and contains in the group that the salt of sulphur forms one or more.
Described coating can have the thickness of 0.1-10nm.
Described barium titanate (BaTiO
3) powder can have the median size of 10-150nm and the crystallographic axis of 1.001-1.010 (c/a) ratio.
According to the embodiment of the present invention, described dielectric substrate 1 is by barium titanate (BaTiO
3) powder formation, described barium titanate (BaTiO
3) powder comprises and be formed on described barium titanate (BaTiO
3) coating on surface of powder particle, and described coating is selected from by sulfide and contains in the group that the salt of sulphur forms one or more, thus high-crystallinity and particulate are provided.
Therefore, described barium titanate (BaTiO
3) the described laminated ceramic capacitor that forms of powder can have seldom crackle to improve reliability.
Can add various ceramic additives, organic solvent, softening agent, tackiness agent and dispersion agent to the powder that forms described dielectric layer 1 (for example according to the barium titanate (BaTiO of purpose of the present invention
3) powder) in.
Because described barium titanate (BaTiO
3) powder has and the characteristic the same according to those uhligite powder of above-mentioned embodiment of the present invention, therefore will omit its description.
The material that is used for the first and second interior electrodes 21 and 22 is not particularly limited.For example, described interior electrode can be by comprising that at least a conductive resin forms in silver (Ag), plumbous (Pb), platinum (Pt), nickel (Ni) and the copper (Cu).
Described laminated ceramic capacitor according to the embodiment of the present invention may further include and is electrically connected to the first external electrode 31 on the first interior electrode 21 and is electrically connected to the second external electrode 32 on the described the second inner electrode 22.
Described the first and second outer electrodes 31 and 32 are electrically connected to respectively on the described first and second interior electrodes 21 and 22, to allow to form betwixt electric capacity.Described the first and second outer electrodes 31 and 32 have dissimilar polarity.
The material that is used for described the first and second outer electrodes 31 and 32 is not particularly limited, as long as it can allow described the first and second outer electrodes 31 and 32 to be electrically connected to the described first and second interior electrodes 21 and 22 to form electric capacity.For example, described the first and second outer electrodes 31 and 32 can comprise and are selected from the group that is comprised of copper (Cu), nickel (Ni), silver (Ag) and silver-palladium (Ag-Pd) one or more.
Fig. 3 is the schema that shows the method for preparing according to the embodiment of the present invention the uhligite powder.
Referring to Fig. 3, the method for preparing according to the embodiment of the present invention the uhligite powder can comprise that mixed metal salt and metal oxide are to form the uhligite granular core; Mix described uhligite granular core and be dissolved in being selected from by sulfide and containing in the group that the salt of sulphur forms one or more in pure water, with the formation mixture; And utilize hydrothermal treatment consists to grow particle with the described uhligite powder of the coating that obtains comprising the surface that is formed on described uhligite powder particle from described mixture, and described coating is selected from by sulfide and contains in the group that the salt of sulphur forms one or more.
Below will describe according to the embodiment of the present invention each step of the described uhligite powder of preparation in detail.
In embodiments of the present invention, described uhligite powder has ABO
3Structure, and described metal oxide is the source corresponding to the element of B position, and described metal-salt is the source corresponding to the element of A position.
At first, described metal-salt and described metal oxide can mix mutually to form the uhligite granular core.
Metal in the described metal oxide can comprise one or more in the group that is selected from titanium (Ti) and zirconium (Zr) composition.
Titanium and zirconium are very easy to hydrolysis, and can be in the situation that does not have independent additive mix to form aqueous titanium and moisture zirconium with the colloidal form precipitation with pure water.
Can wash moisture metal oxide to remove impurity.
More specifically, can under predetermined pressure, filter described moisture metal oxide removing remaining solution, and pure water can be poured into the impurity that its surface refilters to remove particle surface.
Then pure water and acid or alkali can be added in the moisture metal oxide.
Can add in the moisture metal oxide powder that pure water obtains after filter, and use the high viscosity agitator to stir 0.1-72 hour to prepare moisture metal oxide slurry down at 0-60 ℃.
Based on the content of described moisture metal oxide, described acid or the alkali of 0.0001-0.2 mole can be added in the slurry of preparation as peptizing agent.
Described acid is not particularly limited, as long as described acid is the normally used acid in this area, and the example of described acid comprises hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, polycarboxylic acid (polycarboxylic acid) etc., and described acid can be used separately or in them two or more use with mixture.
Described alkali is not particularly limited, as long as described alkali is the normally used alkali in this area, and the example of described alkali comprises Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide etc., and described alkali can use separately or use with mixture.
Described metal-salt can comprise the mixture of hydrated barta or hydrated barta and rare-earth salts (rare earth salt).
Described rare-earth salts is not particularly limited, and the example of the metal in the described rare-earth salts comprises yttrium (Y), dysprosium (Dy), holmium (Ho) etc.
Described uhligite granular core can be 60-150 ℃ of lower formation.
Then, described uhligite granular core can be placed hydrothermal reactor, and be dissolved in pure water in be selected from least a mixing in the group that is formed by described sulfide and the described salt that contains sulphur.
When the temperature of described uhligite granular core is increased to 400 ℃ from 150 ℃, can obtain the uhligite powder.
Use hydrothermal treatment consists can make particle growth in the mixture with the described uhligite powder of the coating that obtains comprising the surface that is formed on described uhligite powder particle, and described coating is selected from by sulfide and contain in the group that the salt of sulphur forms one or more.
According to the embodiment of the present invention, because will be selected from by sulfide and contain one or more coating formation in the group that the salt of sulphur forms on the surface of described uhligite powder particle, so, even the growth of particle is at high temperature carried out, also can prepare the powder that has excellent degree of crystallinity and comprise particulate.
Particularly, in hydrothermal reactor, heat down described uhligite granular core and then keep 0.1-240 hour to carry out the growth of particle at 150 ℃ to 400 ℃.
Obtain having the described uhligite powder particle of high-crystallinity by above-mentioned steps.
Described uhligite powder can comprise and being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that (0＜x＜1) forms any one.
Use the above-mentioned described uhligite powder with high-crystallinity for preparing for the preparation of the method for uhligite powder to have the median size of 10-150nm and the crystallographic axis of 1.001-1.010 (c/a) ratio.
In the situation of the tetragonal crystal particle with crystallographic axis a, b and c, described crystallographic axis (c/a) ratio refers to the ratio of the lattice length of crystallographic axis c and crystallographic axis a, and wherein, the length of crystallographic axis a and b is identical and represent the two by crystallographic axis a.
In order to the embodiment that illustrates the present invention is better understood according to following setting, but can not be interpreted as limitation of the present invention.
Then the hydrolysis titanium tetraisopropylate filters to form aqueous titanium.
Subsequently, add pure water in aqueous titanium, and add nitric acid to wherein take the ratio of H+/Ti as 0.05, and when using the high viscosity agitator to stir, be heated to about 60 ℃ carrying out peptization (peptization) 3 hours, thereby preparation titanium oxide (TiO
2) colloidal sol.
Colloidal sol by peptization preparation is translucent, has light bluely, and is very stable under monodisperse status.The transparency of using near infrared liquid stabilising analyser (turbiscan) to measure described colloidal sol is 75%.The transparency of pure water is 90%.TiO
2Particle has the size of about 3nm and as the monocrystalline of anatase octahedrite (anatase).
With barium hydroxide (Ba (OH)
28H
2O) place the ratio of reactor so that barium and titanium to be equal to or greater than 1, then use nitrogen to take a breath to prevent that barium hydroxide is converted into barium carbonate (BaCO
3).
Then, pure water is added to wherein and be heated to 95 ℃ with barium hydroxide (Ba (OH)
28H
2O) fully dissolving, and with the TiO that heats
2Colloidal sol adds and high-speed stirring together with nitrogen.
Reaction carries out producing barium titanate (BaTiO at 95 ℃
3) granular core.
With described barium titanate (BaTiO
3) after granular core transfers in the 30L hydrothermal reactor, ammonium sulfate is dissolved in the pure water then drops in the described hydrothermal reactor.
Described 30L hydrothermal reactor is heated to 260 ℃, and under agitation reacted 3-10 hour.
Use the described barium titanate (BaTiO that obtains after the pure water washing reaction
3) slurry, and dry with preparation barium titanate (BaTiO in 150 ℃ baking oven
3) powder.
In the following Table 1, when using hydrothermal synthesis method to prepare described barium titanate (BaTiO
3) during powder, described barium titanate (BaTiO in variable grain growth temperature and the ammonium sulfate situation of adding relatively
3) physical properties of powder.
[table 1]
Fig. 4 A is according to the barium titanate powder particle of embodiment of the present invention (Fig. 4 A and 4B) with according to scanning electronic microscope (SEM) figure of the barium titanate powder particle of correlation technique (Fig. 4 C) to Fig. 4 C.
Referring to table 1 and Fig. 4, can find out when the particle growth temperature to be reduced to 200 ℃ when reducing particle size from 260 ℃ that specific surface area has increased (Fig. 4 A).Similarly, when the particle growth temperature maintains 260 ℃, comprise the barium titanate (BaTiO of the ammonium sulfate that adds to wherein
3) specific surface area of powder increased.
In addition, to the described barium titanate (BaTiO according to embodiment of the present invention
3) powder carries out XRD test, and to use rietveld method (Rietveld method) to calculate crystallographic axis (c/a) ratio be 1.00634, be higher than not add ammonium sulfate to wherein barium titanate (BaTiO
3) crystallographic axis (c/a) ratio 1.00593 of powder, therefore, can find out to increase specific inductivity (permitivity).
Therefore, the ammonium sulfate that comprises according to embodiment of the present invention adds described barium titanate (BaTiO wherein to
3) dielectric properties of powder increase.
Fig. 5 A is to scheme according to the scanning transmission electron microscope (STEM) of barium titanate powder under the differing temps of embodiment of the present invention to Fig. 5 C.
To 5C, can see portals is present in the described barium titanate (BaTiO for preparing under the low particle growth temperature according to Fig. 5 A
3) in the powder.
Since the hole in the particle, described barium titanate (BaTiO
3) degree of crystallinity of powder reduces, and when reaction is carried out at low temperatures, the formation hole.
Simultaneously, in hydrothermal synthesis method, at described barium titanate (BaTiO
3) the process of particle growth in because the electrostatic force in the reaction process, the sulfate ion that produces by the ammonium sulfate dissolving is adsorbed on described barium titanate (BaTiO
3) powder particle the surface or be present in their surface.
Further, after the end reaction sulphur is applied or is substituted in described barium titanate (BaTiO
3) surface of powder particle.
In sintering process, reducing the quantity of laminated ceramic capacitor crackle, so that described laminated ceramic capacitor has excellent reliability to sulphur as the catalyzer of unsticking mixture (de-binder).
As previously mentioned, according to the embodiment of the present invention, when using the synthetic described uhligite powder of hydrothermal synthesis method, can be selected from by sulfide and contain one or more coating in the group that the salt of sulphur forms by formation and have the uhligite powder of particulate of high-crystallinity with preparation with the growth of inhibition particle.
Further, thus can have seldom crackle by the laminated ceramic electronic component that uses described uhligite powder preparation improves reliability.
Although shown in conjunction with embodiment and described the present invention, in the situation of the spirit and scope of the present invention that do not depart from subsidiary claims definition, various modifications and variations all are apparent for a person skilled in the art.
Claims (20)
1. uhligite powder, described uhligite powder comprises the coating on the surface of the particle that is formed on described uhligite powder, and described coating is selected from by sulfide and contains in the group that the salt of sulphur forms one or more.
2. uhligite powder according to claim 1, wherein, described sulfide comprises ammonium sulfate.
3. uhligite powder according to claim 1, wherein, the described salt that contains sulphur comprises and is selected from the group that is comprised of phosphoric acid salt and acetate one or more.
4. uhligite powder according to claim 1, wherein, described coating has the thickness of 0.1-10nm.
5. uhligite powder according to claim 1, wherein, described uhligite powder comprises and being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that forms one or more, wherein 0＜x＜1.
6. uhligite powder according to claim 1, wherein, described uhligite powder has the median size of 10-150nm.
7. uhligite powder according to claim 1, wherein, described uhligite powder has the crystallographic axis c/a ratio of 1.001-1.010.
8. method for preparing the uhligite powder, the method comprises:
Mixed metal salt and metal oxide are to form the uhligite granular core;
Mix described uhligite granular core and be dissolved in being selected from by sulfide and containing in the group that the salt of sulphur forms one or more in pure water, with the formation mixture; And
Utilize hydrothermal treatment consists from described mixture, to grow particle with the described uhligite powder of the coating that obtains comprising the surface that is formed on described uhligite powder particle, and coating is selected from by sulfide and contain in the group that the salt of sulphur forms one or more.
9. method according to claim 8, wherein, described sulfide comprises ammonium sulfate.
10. method according to claim 8, wherein, the described salt that contains sulphur comprises and is selected from the group that is comprised of phosphoric acid salt and acetate one or more.
11. method according to claim 8, wherein, described metal-salt comprises the mixture of hydrated barta or hydrated barta and rare-earth salts.
12. method according to claim 8, wherein, described metal oxide comprises titanium oxide or zirconium white.
13. method according to claim 8, wherein, described coating has the thickness of 0.1-10nm.
14. method according to claim 8, wherein, described uhligite powder has the median size of 10-150nm.
15. method according to claim 8, wherein, described uhligite powder comprises and being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that forms one or more, wherein 0＜x＜1.
16. method according to claim 8, wherein, described uhligite powder has the crystallographic axis c/a ratio of 1.001-1.010.
17. a laminated ceramic electronic component, described laminated ceramic electronic component comprises:
Ceramic main body, described ceramic main body comprises dielectric layer and inner electrode layer; Described dielectric layer comprises the uhligite powder, and described uhligite powder has the coating that is formed on described uhligite powder particle surface, and described coating is selected from the group that is comprised of sulfide and the salt that contains sulphur one or more; When having described dielectric layer in described ceramic main body inside when being inserted between the inner electrode layer, described inner electrode layer toward each other.
18. laminated ceramic electronic component according to claim 17, wherein, described coating has the thickness of 0.1-10nm.
19. laminated ceramic electronic component according to claim 17, wherein, described uhligite powder comprises and being selected from by BaTiO
3, BaTi
xZr
1-xO
3, Ba
xY
1-xTiO
3, Ba
xDy
1-xTiO
3And Ba
xHo
1-xTiO
3In the group that forms one or more, wherein 0＜x＜1.
20. laminated ceramic electronic component according to claim 17, wherein, described uhligite powder has the crystallographic axis c/a ratio of 1.001-1.010.
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| KR10-2011-0103194 | 2011-10-10 |
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| CN110092657A (en) * | 2019-04-25 | 2019-08-06 | 苏州宝顺美科技有限公司 | Nano barium phthalate crystallite and preparation method thereof and barium carbonate powder and preparation method thereof |
| CN115522179A (en) * | 2022-09-30 | 2022-12-27 | 武汉苏泊尔炊具有限公司 | Method for manufacturing composite material for non-stick cookware |
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| KR101539851B1 (en) * | 2013-09-23 | 2015-07-27 | 삼성전기주식회사 | Perovskite powder, manufacturing method thereof and paste composition for internal electrode comprising the same |
| CN115667151B (en) * | 2020-05-27 | 2024-03-12 | 松下知识产权经营株式会社 | Barium compound structure and method for producing same |
| JP2023009752A (en) | 2021-07-08 | 2023-01-20 | ヒューレット－パッカード デベロップメント カンパニー エル．ピー． | Image forming apparatus that can adjust tension of endless belt |
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| JP2013082600A (en) | 2013-05-09 |
| CN103030403B (en) | 2017-04-12 |
| KR20130038695A (en) | 2013-04-18 |
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