CN103570059B - Preparation method of barium titanate and barium titanate powder prepared by the barium titanate - Google Patents
Preparation method of barium titanate and barium titanate powder prepared by the barium titanate Download PDFInfo
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- CN103570059B CN103570059B CN201310289292.0A CN201310289292A CN103570059B CN 103570059 B CN103570059 B CN 103570059B CN 201310289292 A CN201310289292 A CN 201310289292A CN 103570059 B CN103570059 B CN 103570059B
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention provides a preparation method of barium titanate, and barium titanate powder prepared by the barium titanate. The preparation method of high-crystallized barium titanate comprises the steps of: prepraing barium hydroxide raw material having ionized barium (Ba) by raising a relative temperature; preparing a titanium (Ti) raw material dispersed in acid or base; mixing and reacting the barium hydroxide raw material and the Ti raw material to obtain a barium titanate seed crystal; and mixing the barium titanate seed crystal with a sintering accelerant to complete grain growth. The barium titanate powder can have wonderful crystallite size distribution and a low sintering initial temperature, therefore, when being applied to multi-layer ceramic electronic elements, problems such as layered generation, and coverage rate degeneration are improved.
Description
Cross-Reference to Related Applications
This application claims the korean patent application No.10-2012- that on July 27th, 2012 is submitted to Korean Intellectual Property Office
0082777 priority, the disclosure of the korean patent application are incorporated by reference in the application.
Technical field
The present invention relates to a kind of preparation method of the Barium metatitanate. with lower sintering temperature, and prepared by the Barium metatitanate.
Barium titanate powder.
Background technology
According to recently thinning and lighten, and the trend of high capacitance, high reliability etc. is realized, in electronic component, needed
Barium metatitanate. crystal grain for the ferroelectric material of multilayer ceramic capacitor (MLCC) has fabulous dielectric constant and high reliability
And size is little.
Even if however, in the development of the microgranule dielectric powder with height dielectric constant, can cause due to height
Burning between the electrode layer with lower sintering temperature of the dielectric layer of sintering temperature and hundreds of degrees Celsius (DEG C) lower than dielectric layer
Interlaminar delamination and the problem as degeneration is covered caused by electrode caking caused by knot shrinkage factor difference.
In order to develop the multilayer ceramic capacitor with high capacitance, the sintering for controlling dielectric layer and electrode layer is needed to receive
The technology of shrinkage, is this purpose, reduces the different effort of sintering shrinkage of each layer by the paste for internal electrode
It is middle to increase base material and add glass agglutinant to carry out to dielectric powder before sintering.
According to prior art such as BaO, CaO, SiO2Blending ingredients Deng composition are often used as preparing multi-layer ceramics
The glass agglutinant of capacitor.However, for the agglutinant is prepared, having a disadvantage that, that is, need at 1400-1500 DEG C
Melt under high temperature, and also need to the separation process for mixing with dielectric powder.
Prior art document
Korean Patent Publication publication number No.10-2000-0031135
The content of the invention
An aspect of of the present present invention provides a kind of preparation method of the Barium metatitanate. with lower sintering temperature, and by the titanium
Barium titanate powder prepared by sour barium.
According to an aspect of the present invention, there is provided a kind of preparation method of barium titanate powder, the preparation method include：Pass through
Relative temperature is raised, the barium hydroxide raw material with ionization barium (Ba) is prepared；Titanium (Ti) during preparation is dispersed in acid or alkali is former
Material；The barium hydroxide raw material and the titanium material are mixed and reacted and obtains barium titanate seed crystal；And the Barium metatitanate. is brilliant
Plant and mix to complete grain growth with sintering aidses.
The sintering aidses can be at least one in slaine, metal alkoxide, boric acid and boron oxide.
The slaine can be metal nitrate, metal acetate salt, metal hydroxidess, metal silicate and metal carbon
At least one in hydrochlorate.
The slaine and the metal alkoxide can include at least one in alkali metal and transition metal.
The slaine and the metal alkoxide can be including at least in lithium (Li), sodium (Na), potassium (K) and vanadium (V)
Kind.
More specifically, the slaine can be Lithium hydrate.
Concentration for mixing the sintering aidses to complete the grain growth can be as 1-10mol%.
The barium hydroxide raw material is barium hydroxide (Ba (OH)28H2O)。
In the preparation of the barium hydroxide raw material, barium hydroxide can be stirred and in a nitrogen atmosphere by being warmed up to 70
DEG C or the dissolving of higher temperature.
Titanium (Ti) raw material can be hydrated titanium or titanium dioxide.
The mixing of the barium hydroxide raw material and the titanium material and course of reaction can be in 80 DEG C or higher temperature
Under carry out.
In mixing and course of reaction of the barium hydroxide raw material with the titanium material, the mole mixture ratio of barium and titanium can
Think 1≤barium/titanium≤3.
During grain growth is completed, the barium titanate seed crystal is mixed with the sintering aidses, and should
Mixture seals in hydrothermal synthesis reaction kettle and 1-60 hours is stirred at 200-360 DEG C and reacted.
According to an aspect of the present invention, there is provided a kind of barium titanate powder, the barium titanate powder contains concentration for 500-
At least one in the lithium (Li) of 3000ppm, sodium (Na), potassium (K), vanadium (V), boron (B) and silicon (Si).
The ratio (D99/D50) of the D99 and D50 of the barium titanate powder can be 1.5-3.0, and specifically, the titanium
The ratio (D99/D50) of the D99 and D50 of sour barium dust can be 1.60-1.75.
The largest grain size of the barium titanate powder can be 100-1000nm, and specifically, the barium titanate powder
The largest grain size at end can be 100-135nm.
Description of the drawings
By detailed description below in conjunction with the accompanying drawings, it will be more clearly understood that above and other aspect, the spy of the present invention
Levy and further advantage, wherein：
Fig. 1 is a kind of flow chart of the preparation method of the barium titanate powder of embodiment of the invention；
Fig. 2 is X-ray diffraction (XRD) the analysis result curve chart of the barium titanate powder for showing according to embodiments of the present invention 1；
Fig. 3 is scanning electron microscope (SEM) photo of according to embodiments of the present invention 1 barium titanate powder；
Fig. 4 is scanning electron microscope (SEM) photo of according to embodiments of the present invention 1 barium titanate powder；
Fig. 5 is scanning electron microscope (SEM) photo of the barium titanate powder according to comparative example of the present invention 1；
Fig. 6 is scanning electron microscope (SEM) photo of the barium titanate powder according to comparative example of the present invention 1；
Fig. 7 is the sintering shrinkage behavior curve chart of the barium titanate powder for showing according to embodiments of the present invention 1 and comparative example 1.
Specific embodiment
Hereinafter, embodiments of the present invention will be described in detail with reference to the attached drawings.However, the present invention can be with various different
Mode embodies, and should not be construed as the embodiment for being limited to setting herein.More properly, there is provided these embodiments
Purpose be in order that the displosure will be complete and comprehensive, and fully be conveyed the scope of the invention to this area
Technical staff.
Fig. 1 is a kind of flow chart of the preparation method of the barium titanate powder of embodiment of the invention.With reference to Fig. 1,
Included according to the method for preparing Barium metatitanate. of embodiment of the present invention：By raising relative temperature, prepare with ionization barium (Ba)
Barium hydroxide raw material (S1)；Prepare titanium (Ti) raw material (S2) in being dispersed in acid or alkali；By the barium hydroxide raw material and
The titanium material mixes and reacts and obtains barium titanate seed crystal (S3)；The barium titanate seed crystal is mixed into (S4) with sintering aidses；
And complete grain growth (S5).
Using barium hydroxide as the barium raw material.Barium hydroxide (Ba (OH) is stirred in a nitrogen atmosphere28H2O) may be used
To prevent from brium carbonate being formed due to the carbon dioxide in air, and eight water are made by the temperature for being warmed up to 70 DEG C or higher
Barium hydroxide is completely dissolved (S1).
Because needing nucleus promptly to shape when the mixing being described below and reaction titanium (Ti) raw material, rising
It is critically important that at high temperature, barium (Ba) raw material is ionized completely.
Using hydrated titanium (TiOx/2(OH)4-X) or titanium dioxide (TiO2) colloidal sol is used as titanium material.Using the hydration
The situation of titanium, titanium (Ti) raw material can pass through addition base material in titanium material, such as add a small amount of ammonia to prepare and then pass through
Polishing is disperseed.For the titanium dioxide (TiO2) colloidal sol, it is possible to use colloidal sol by acid or alkali dispersion rather than
Using the dispersant with Long carbon chain.Can be using with the titanium material (S2) compared with little crystallite size.
Barium hydroxide (the Ba (OH) of the dissolving28H2O Barium metatitanate .) is mixed to get rapidly with scattered titanium colloidal sol brilliant
Plant (S3).Here, mixing when barium ionss and titanium (Ti) raw material each other rapidly reaction be critically important.
In the reaction, the mol ratio (Ba/Ti ratio) of reactant barium and titanium can be 1≤barium/titanium≤3, or
1.2≤barium/titanium≤2.
Until the generation of the barium titanate seed crystal terminates, less than 50-200 DEG C of temperature can be maintained, it is also possible to maintain
100-150 DEG C of temperature.Crystal seed is generated after terminating, and temperature is set as less than 100 DEG C, is carried out nitrogen purification, and is removed formation
Gas, so can effectively eliminate the such as impurity such as deflocculant.
Carry out to be swift in response, in mixing, temperature is set as 80 DEG C or higher.In addition, maintaining the reaction until institute
State crystal seed and generate and terminate.
In order to mix the titanium material and the barium raw material and react to produce rapidly the barium titanate seed crystal, the hydrogen-oxygen
The mixing and reaction for changing barium and titanium material can be carried out by the one kind in quick stirring, microwave and ultrasound.
The crystal seed is generated after terminating, and collects the crystal seed for producing.Here, aerial situation is exposed in the crystal seed
Under, brium carbonate (BaCO can be formed3), as long as accordingly, it would be desirable to it is to be noted that not allowing the crystal seed to expose in atmosphere.
The barium titanate seed crystal of collection is transferred to hydrothermal synthesis reaction kettle, and sintering aidses are dissolved in pure water, then will
The sintering aidses of dissolving are placed on (S4) in hydrothermal synthesis reaction kettle.
The sintering aidses can be at least one in slaine, metal alkoxide, boric acid and boron oxide.
The slaine can be metal nitrate, metal acetate salt, metal hydroxidess, metal silicate and metal carbon
At least one in hydrochlorate.
The slaine and the metal alkoxide can include at least one in alkali metal and transition metal.
The slaine and the metal alkoxide can be including at least in lithium (Li), sodium (Na), potassium (K) and vanadium (V)
Kind.
More specifically, the slaine can be Lithium hydrate.
The concentration that the sintering aidses can be added is 1-10mol%.It is less than in the concentration of the sintering aidses
In the case of 1mol%, the sintering temperature fully can not be reduced, and sintering aidses concentration higher than 10mol% feelings
Under condition, the physical property that the barium titanate powder of secondary phase or synthesis may be produced by metallic element may change.More
It is preferred that, the concentration of the sintering aidses can be 1-4mol%.
After the barium titanate seed crystal, the sintering aidses and pure water are mixed, its grain growth is closed in hydro-thermal
Carry out in reactor (S5).The grain growth can be slowly completed in higher temperature.The grain growth passes through high-energy
Situation about slowly completing, atom are arranged in relatively steady state, can just eliminate defect.Therefore, the grain growth is in water
Carry out stirring 1-60 hours at 200-360 DEG C in thermal synthesis reactor.
The Barium metatitanate. serosity obtained after completing the grain growth is cleaned with pure water, the serosity for cleaning exists in an oven
100-200 DEG C of drying is collecting the barium titanate powder.
In the case of by said method synthetic powder, will not be produced by transition metal or alkali-metal secondary phase
It is raw, but pass through synthetically produced single-phase Barium metatitanate..In addition, showing the particle size distribution of formed powder and without the burning
The situation level of knot accelerator is close.
However, according to the embodiment of the present invention, in the case of by said method synthetic powder, the sintering starting
About at 870 DEG C, more than about 50 DEG C are reduced relative to the barium titanate powder for not adding the sintering aidses.In addition, root
According to embodiments of the present invention, in the case of by said method synthetic powder, because completing the crystalline substance by hydro-thermal method
Add the sintering aidses during grain growth, avoid the need for individually adding agglutinant.
Meanwhile, can include that concentration is 500- by the barium titanate powder prepared by the preparation method of the Barium metatitanate.
At least one in the lithium (Li) of 3000ppm, sodium (Na), potassium (K), vanadium (V), boron (B) and silicon (Si).
In addition, the ratio (D99/D50) of the D99 and D50 of the barium titanate powder can be 1.5-3.0, more specifically, described
The ratio (D99/D50) of the D99 and D50 of barium titanate powder can be the ratio of 1.60-1.75.
The largest grain size of the barium titanate powder can be 100-1000nm, and the more specifically, Barium metatitanate.
The largest grain size of powder can be 100-135nm.
The synthesis of the barium titanate powder of Lithium hydrate of the embodiment 1) containing addition
Barium hydroxide (Ba (OH)28H2O it is after being purified in) being injected into reactor and by nitrogen, at 95 DEG C or higher
Temperature stirs cleaned material so that its dissolving.Again by being warmed up to 60 DEG C or higher of temperature preparing titanium dioxide
(TiO2) colloidal sol.Injection barium (Ba) solution and the titanium dioxide (TiO2) colloidal sol in reactor after, at 95 DEG C or it is higher enter
Row high-speed stirred is collecting barium titanate seed crystal.After the barium titanate seed crystal of shaping is transferred to hydrothermal synthesis reaction kettle, add hydroxide
It is 2.0mol% that lithium and pure water make the concentration of the Lithium hydrate.Clean at 260 DEG C the hydrothermal synthesis reaction kettle and
It is dried at 150 DEG C in baking oven.As shown in Fig. 2 the X-ray diffraction (XRD) of the barium titanate powder is obtained by said process
Analysis result, it is recognised that not producing the barium titanate powder of secondary phase by lithium (Li) and synthesis in single-phase.
What was certain was that existing lithium concentration is about 1251ppm in the barium titanate powder.
Table 1 below be displayed in the barium titanate powder of embodiment 1 and with the powder identical of embodiment 1 under the conditions of synthesis but
Be the Lithium hydrate for wherein not containing addition barium titanate powder (comparative example 1) between particle size distribution contrast.
Table 1
| Embodiment 1 (nm) | Comparative example 1 (nm) | |
| D 1 | 36.2 | 27.3 |
| D 50 | 56.6 | 53.5 |
| D 90 | 74.7 | 73.1 |
| D 99 | 96.6 | 93.0 |
| D 99.9 | 121.0 | 120.8 |
| D max | 128.2 | 140.9 |
| D 99/D 50 | 1.71 | 1.74 |
With reference to upper table 1, it is recognised that the ratio (D99/D50) of the D99 and D50 of embodiment 1 is 1.71, but comparative example 1
D99 and the ratio (D99/D50) of D50 be 1.74, the particle size distribution that such comparative example 1 shows is not relative to embodiment 1
Uniformly.In addition, when the value of Dmax-D1 is compared, embodiment 1 meets equation：128.2-36.2=92.0, however, right
Ratio 1 meets equation：140.9-27.3=113.6, be implemented example 1 display particle size distribution relative to comparative example 1 more
Uniformly.
Fig. 3 and Fig. 4 are scanning electron microscope (SEM) photos of according to embodiments of the present invention 1 barium titanate powder,
And Fig. 5 and Fig. 6 are scanning electron microscope (SEM) photos of the barium titanate powder according to comparative example of the present invention 1.From
SEM photograph it is recognised that the particle size distribution of the barium titanate powder of embodiment 1 it is similar to the barium titanate powder of comparative example 1 or
Person is uniform relative to the particle size distribution of the barium titanate powder of comparative example 1.
Fig. 7 is the sintering shrinkage behavior curve chart of the barium titanate powder for showing according to embodiments of the present invention 1 and comparative example 1.
From Fig. 7 it is recognised that starting sintering shrinkage in the barium titanate powder of embodiment 1 reduces about 50 relative to 1 temperature of comparative example
℃。
Therefore, when completing the grain growth of the barium titanate seed crystal according to hydro-thermal method, it is allowed to add transition metal or alkali
Metal, sintering initial temperature reduce about 50 DEG C and independent mixed process are not carried out between dielectric powder and agglutinant even,
Sintering behavior so between dielectric layer and electrode layer is similar, and when laminated ceramic electronic component is applied to, improves
Such as it is layered generation, covers the problems such as degenerating, it thus provides a kind of multilayer ceramic capacitor with high reliability.
In sum, the barium titanate powder tool prepared by Barium metatitanate. preparation method according to the embodiment of the present invention
There is appropriate particle size distribution and compared with low frit initial temperature feature, so between the dielectric layer and the electrode layer
Sintering behavior is similar, therefore, layering such as is improved when being applied to laminated ceramic electronic component and produced, covered the problems such as degenerating.
Although the present invention has been shown and described already in connection with embodiment, do not having to those skilled in the art
In the case of deviateing the spirit and scope of the present invention of appended claims definition, the modification made by the present invention and modification
It is obvious.
Claims (10)
1. a kind of preparation method of barium titanate powder, the preparation method include：
By raising relative temperature, the barium hydroxide raw material with ionization barium is prepared；
Prepare the titanium material in being dispersed in acid or alkali；
The barium hydroxide raw material and the titanium material are mixed and reacted, barium titanate seed crystal is obtained；And
The barium titanate seed crystal is mixed to complete grain growth with sintering aidses LiOH；
Wherein, the ratio of the D99 and D50 of the barium titanate powder is 1.5-3.0.
2. preparation method according to claim 1, wherein, promoted with the sintering for completing the grain growth for mixing
The concentration for entering agent is 1-10mol%.
3. preparation method according to claim 1, wherein, the barium hydroxide raw material is barium hydroxide.
4. preparation method according to claim 1, wherein, in the preparation of the barium hydroxide raw material, barium hydroxide exists
Stir under nitrogen atmosphere and dissolved by the temperature for being warmed up to 70 DEG C or higher.
5. preparation method according to claim 1, wherein, the titanium material is hydrated titanium or titanium dioxide.
6. preparation method according to claim 1, wherein, the barium hydroxide raw material and the mixing of the titanium material and anti-
Process is answered to carry out at 80 DEG C or higher of temperature.
7. preparation method according to claim 1, wherein, the barium hydroxide raw material and the titanium material mixing and
In course of reaction, the mole mixture ratio of barium and titanium is 1≤barium/titanium≤3.
8. preparation method according to claim 1, wherein, it is during grain growth is completed, the Barium metatitanate. is brilliant
Plant and mix with the sintering aidses, and the mixture in hydrothermal synthesis reaction kettle is sealed and stirred at 200-360 DEG C
Mix 1-60 hours to be reacted.
9. the barium titanate powder that the preparation method according to any one in claim 1-8 is prepared, the barium titanate powder
The last at least one containing in lithium, sodium, potassium, vanadium, boron and the silicon that concentration is 500-3000ppm, wherein, the barium titanate powder
The ratio of D99 and D50 is 1.5-3.0.
10. barium titanate powder according to claim 9, wherein, the largest grain size of the barium titanate powder is 100-
1000nm。
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| KR1020120082777A KR101730195B1 (en) | 2012-07-27 | 2012-07-27 | A manufacturing method of Barium-Titanate and Barium-Titanate powder manufactured by the same |
| KR10-2012-0082777 | 2012-07-27 |
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| CN110129772B (en) * | 2019-04-10 | 2021-06-22 | 广东省医疗器械研究所 | Preparation method of barium titanate in-situ coating |
| CN110092657B (en) * | 2019-04-25 | 2021-01-26 | 苏州宝顺美科技有限公司 | Nano barium titanate microcrystal and preparation method thereof, and barium titanate powder and preparation method thereof |
| CN110028317B (en) * | 2019-04-25 | 2021-01-26 | 苏州宝顺美科技有限公司 | Nano barium titanate powder and preparation method thereof, ceramic dielectric layer and manufacturing method thereof |
| KR102555686B1 (en) | 2021-06-23 | 2023-07-14 | 한국세라믹기술원 | Manufacturing method of barium titanate powder |
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| JPH0676258B2 (en) * | 1985-07-27 | 1994-09-28 | 堺化学工業 株式会社 | Method for manufacturing ceramic dielectric |
| GB2193713B (en) * | 1986-07-14 | 1990-12-05 | Cabot Corp | Method of producing perovskite-type compounds. |
| FR2636060A1 (en) * | 1988-09-02 | 1990-03-09 | Thomson Csf | PROCESS FOR PRODUCING HYBRID CHEMICAL CERAMIC MATERIAL AND MATERIAL OBTAINED |
| JPH0597510A (en) * | 1991-10-02 | 1993-04-20 | Murata Mfg Co Ltd | Production of dielectric porcelain composition and its raw material powder |
| JP2002519298A (en) * | 1998-07-01 | 2002-07-02 | キャボット コーポレイション | Hot water production method of barium titanate powder |
| JP4184313B2 (en) * | 2004-04-19 | 2008-11-19 | Ｔｄｋ株式会社 | Method for producing barium titanate powder |
| TWI290539B (en) * | 2004-08-31 | 2007-12-01 | Showa Denko Kk | Barium titanate and capacitor |
| KR100633723B1 (en) * | 2005-08-04 | 2006-10-13 | 한화석유화학 주식회사 | Process for preparing barium titanate |
| JP5057300B2 (en) * | 2006-01-20 | 2012-10-24 | 独立行政法人産業技術総合研究所 | Manufacturing method of ceramic powder |
| JP4967599B2 (en) * | 2006-10-23 | 2012-07-04 | Ｔｄｋ株式会社 | Barium titanate powder, dielectric ceramic composition and electronic component |
| JP5112979B2 (en) * | 2008-07-30 | 2013-01-09 | 関東電化工業株式会社 | Barium titanate fine particles and production method thereof |
| CN101372359A (en) * | 2008-09-18 | 2009-02-25 | 华东师范大学 | Preparation of superfine cubic phase barium titanate powder |
| JP5111426B2 (en) * | 2009-04-01 | 2013-01-09 | 株式会社村田製作所 | Barium titanate-based powder and manufacturing method thereof, dielectric ceramic and multilayer ceramic capacitor |
| CN101602522B (en) * | 2009-07-15 | 2011-07-27 | 中山大学 | Synthetic method of monodisperse barium titanate polyhedral nano particles |
| KR20120060542A (en) * | 2010-12-02 | 2012-06-12 | 삼성전기주식회사 | A fabricating method for titanic acid barium powder and titanic acid barium powder using thereof |
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