WO2003004415A1 - Poudre de titanate de baryum et procede de production associe - Google Patents

Poudre de titanate de baryum et procede de production associe Download PDF

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Publication number
WO2003004415A1
WO2003004415A1 PCT/JP2002/006719 JP0206719W WO03004415A1 WO 2003004415 A1 WO2003004415 A1 WO 2003004415A1 JP 0206719 W JP0206719 W JP 0206719W WO 03004415 A1 WO03004415 A1 WO 03004415A1
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WIPO (PCT)
Prior art keywords
barium titanate
titanate powder
powder
calcined
average particle
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PCT/JP2002/006719
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English (en)
Japanese (ja)
Inventor
Koji Tokita
Matsuhide Horikawa
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Toho Titanium Co., Ltd.
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Publication date
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Priority to JP2003510393A priority Critical patent/JPWO2003004415A1/ja
Publication of WO2003004415A1 publication Critical patent/WO2003004415A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/76—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by a space-group or by other symmetry indications
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • 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

Definitions

  • the present invention relates to an improved barium titanate powder having excellent dielectric properties and used as a dielectric material for electronic components such as multilayer ceramic capacitors and PTC thermistors, and a method for producing the same.
  • Barium titanate is widely used in electronic materials such as dielectric materials for multilayer ceramic capacitors.
  • the barium titanate particles which are the material for forming the dielectric layer, are as small as possible, specifically 0.5 m or less, in order to increase the number of layers, miniaturization, and capacity of capacitors.
  • a barium titanate material having a crystallinity of preferably 0.4 or less, high crystallinity, and a low content of alkaline metal components such as Na ions and K ions.
  • Barium titanate obtained by the solid phase method has disadvantages such as a large particle size of several meters and a wide particle size distribution even when crushed. For this reason, various liquid phase methods such as a hydrothermal synthesis method, a low-temperature direct synthesis method, a gel sol method, and an oxalic acid method have been proposed in many documents. Although the liquid phase method is costly, it has the advantage that spherical fine particles with a particle size of 1 m or less can be easily obtained, but the crystallinity is not easily increased. There is a problem that it is difficult to remove metal.
  • JP-A-5-330824 discloses that a titanium compound and a barium compound are mixed at a BaZTi ratio of 0.95 to 1.05, hydrogen peroxide is added thereto, and a wet reaction is carried out. It is disclosed that after obtaining a cubic barium titanate powder having a particle diameter of 0.2 to 5 and calcining at 900 to 1300 ° C., a truly spherical barium titanate can be obtained. Based on the advantages of the liquid phase method, which allows barium titanate with a small particle diameter to be obtained, there have been introduced many examples of methods for producing spherical fired barium titanate powder with a particle size of 0.1 to 0.2 m by low-temperature firing. I have.
  • JP-A-60-81023 and JP-A-60-90825 disclose that a reaction is carried out by reacting hydrous titanium oxide and barium hydroxide in a dilute aqueous solution at 60 to 110 ° C. : Calcined barium titanate powder of! ⁇ 0.2 at 800 ° C, then into tablets and fired at 1200 ° C to obtain calcined titanate with relative density of 93% and particle size of about 0.5m Examples of producing barium materials have been reported.
  • Japanese Patent Application Laid-Open No. 5-178619 discloses that the reaction product is not less than 300 ° C., preferably 400 ° C. It introduces a method of heating at ⁇ 700 ° C, washing with water of pH 7 ⁇ 10, and separating by filtration. Also, JP-A-61-146713 discloses that barium titanate obtained by a hydrothermal reaction is washed with hot water, the powder is calcined at 800 ° C, then washed with acetic acid water, and further washed with pure water. How to do is introduced. However, even with water washing or hot water washing, the Na content cannot be easily removed.
  • green calcined barium titanate refers to a so-called green material (green) to the extent that barium titanate obtained by synthesis is dried.
  • calcined barium titanate refers to It refers to raw material that has been subjected to heat treatment (also called calcination) at a higher temperature, that is, at least 500 ° C or more and 980 ° C or less. This includes those that have been crushed or have been crushed and washed.
  • the fired barium titanate powder of the present invention is appropriately mixed with other components and sintered at a normal firing temperature (about 110 to 1300 ° C.) to form a desired dielectric material. To be served.
  • the BaZT i atomic ratio (hereinafter referred to as the Ba / T i ratio unless otherwise specified) is in a very narrow range, specifically 1.003 to 1.009, especially 1. Obtaining a barium titanate powder controlled to 003 to 1.005 and firing it to obtain a fired barium titanate with high crystallinity;
  • the firing can be performed at a temperature much lower than conventionally known, so that the growth of particles can be suppressed, and the average particle size is not more than 0.5 m.
  • a first invention according to the present invention is an unfired barium titanate powder obtained by subjecting a titanium compound and a vacuum compound to a liquid phase reaction, and having an average particle size (here, 350 ° C The crystal is characterized by having a particle size of 0.05 to 0.5 / m and a BaZT i ratio of 1.003 to 1.009, measured by degassing for 30 minutes at a temperature. It is an unfired barium titanate powder having a cubic structure. The unburned The barium titanate powder is suitable as a raw material powder for producing the barium titanate powder of the second invention described below.
  • the second invention has an average particle size of 0.05 to 0.5 m, a BaZT i ratio of 1.003 to 1.006, a loss on ignition of 0.5% by weight or less, and a square crystal structure. It is a barium titanate powder that has been calcined.
  • the third invention of the present invention relates to a method for producing a highly crystalline and fine barium titanate powder, wherein (i) a titanium compound and a barium compound are subjected to a liquid phase reaction in an aqueous alkali solution to obtain an average particle diameter.
  • the loss on ignition (also referred to as L) in the present invention refers to the weight (W1) after the barium titanate powder is kept at 110 ⁇ 5 ° C for 60 minutes in the air. Then, the temperature is raised to 110 ° C in air at 10 ° C per minute, and the weight (W2) after holding at 1100 ⁇ 30 ° C for 60 minutes is calculated by the following formula. Value.
  • the cube as a shape display of the barium titanate powder of the present invention is observed with an electron microscope, and the appearance of the particles is a cube, a rectangular parallelepiped, or a pseudo cube in which the corners of individual particles are slightly missing, Alternatively, it means a pseudo-cuboid.
  • FIG. 1 is an electron micrograph showing an unfired barium titanate powder according to the present invention.
  • FIG. 2 is an electron micrograph showing the fired barium titanate powder according to the present invention. BEST MODE FOR CARRYING OUT THE INVENTION
  • the “green calcined barium titanate powder” of the first invention is a barium titanate powder obtained by a liquid phase reaction between a titanium compound and a vacuum compound.
  • the diameter is 0.05 to 0.5, preferably a fine powder of 0.07 to 0.4 m, and (b) the ratio of 8 & / 1.009, from the viewpoint of crystallinity, that is, dielectricity, preferably 1.003 to 1.007, particularly preferably 1.004 to 1.006, extremely close to 1.000, but the number of valence atoms is titanium atom It has a composition that is very slightly greater than the number.
  • the fired barium titanate powder produced therefrom has poor crystallinity.
  • the BaZT i ratio is from 1.003 to 1.007, more preferably from 1.003 to 1.006, as described above.
  • the unsintered barium titanate powder includes those subjected to a heat treatment of 250 or less mainly for drying. From the unfired barium titanate powder having such a Ba / T i ratio (that is, the raw material powder to be fired), a “fired barium titanate powder” of the second invention described below is obtained.
  • the specific unfired barium titanate powder is subjected to a heat treatment at 930 to 980 ° C, particularly 930 to 970 ° C, thereby obtaining a fired barium titanate powder having extremely high crystallinity as described later.
  • Can be Cubic crystals cannot be obtained below 930 ° C, and grain growth occurs above 980 ° C.
  • the contained aluminum metal such as Na can be removed very effectively.
  • the calcined barium titanate powder of the second invention has extremely high crystallinity while being extremely fine particles having an average particle diameter of 0.05 to 0.5 m.
  • the ratio of barium atoms is extremely slightly higher than titanium atoms, with a ratio of 1.003 to 1.006, preferably 1.003 to 1.005, and in a limited range.
  • the structure is tetragonal, and the shape observed with an electron microscope is square, ie, rectangular or cubic crystalline. This is a finely baked powder having a high particle size.
  • the calcined barium titanate powder has a loss on ignition (L) of 0.5% by weight or less, preferably 0.4% by weight or less, particularly preferably 0.4% by weight or less. 3% by weight or less.
  • L loss on ignition
  • the calcined barium titanate powder of the present invention is a fine particle having a particle size of 0.5 / m or less, but has a CZa ratio (C-axis length of tetragonal crystal axis length) Is an extremely high crystallinity of 1.009 or more.
  • the BET specific surface area, particle size 0.1 approximately at the 4 Paiiota ones 1. 5 ⁇ 2. 5m 2 / g, 0. intended for 2 m 3. 5 ⁇ 5.
  • the loss on ignition (L) when heated to 1100 ° C has an extremely thermally stable crystal structure of 0.5% by weight.
  • the particle shape is a cube or a rectangular parallelepiped, and has a shape different from a generally known spherical or potato-like shape. These clearly show excellent crystallinity. An even more excellent point is that, despite being obtained by the liquid phase method, the high purity of the metal component content of the aluminum alloy is not more than 50 ppm and not more than 40 ppm. Despite such a fine fired powder, a cubic or rectangular parallelepiped fired barium titanate powder having high crystallinity has not been known.
  • the third invention of the present invention is to produce the unfired barium titanate powder of the first invention by a liquid phase method, and to obtain the obtained raw material in 930 to 98 O: This is to produce the fired barium titanate powder of the second invention by firing. Dielectrics manufactured using the fired barium titanate powder of the present invention have extremely excellent dielectric properties and are effective in reducing the size of parts.
  • Titanium compounds as liquid phase reaction raw materials include titanium tetrachloride, oxytitanium chloride, titanium tetrachloride hydrolyzate (titanium hydroxide hydrate, orthotitanic acid, metatitanic acid), peroxotitanic acid, titanyl sulfate, etc. It is. Titanium tetrachloride hydrolyzate is hydrolyzed with alkaline water such as ammonia, or produced by adding water. The resulting hydrochloric acid is obtained by evaporation and separation as a solid or gel.
  • the solid is used as a slurry or a very dilute aqueous solution.
  • the barium compound include barium chloride, barium hydroxide, barium nitrate, barium sulfate, and barium acetate. Of these, barium chloride or barium hydroxide is preferably used.
  • an aqueous solution of titanium tetrachloride (concentration is about 0.2 to 2.0 mol and this is called liquid I) and an aqueous solution of barium chloride or barium hydroxide (concentration is 0.1 to 1.0 mol Zl, hereafter referred to as solution II), and bringing them into contact with each other in a reaction vessel at a temperature of 90 to 10 O: under strong alkaline conditions.
  • the pH is maintained at 13 or higher, preferably 13.5 or higher, more preferably 13.8 or higher. More preferably, it is preferable that the solution II is previously prepared as an aqueous alkali solution.
  • a necessary amount of an alkaline aqueous solution is supplied from another system as needed to maintain the predetermined PH. More preferably, before starting the supply of both liquids, an aqueous solution of an aqueous solution adjusted to a predetermined concentration is charged into the reaction vessel in advance, and then the both liquids are supplied to prevent local pH decrease. It is valid.
  • the supply amounts of both liquids to produce barium titanate with a BaZT i ratio of 1.03 to 1.009, which is the target product, the supply amounts of the titanium compound and the barium compound to the reaction system must be adjusted. Strict control is important.
  • the molar ratio of both compounds supplied to the reaction vessel is set in the range of 1.05 to 1.10, and both liquids are quantitatively supplied to the reaction vessel at this set value.
  • the total supply ratio of both liquids according to this that is, (barium concentration of liquid II x supply rate) Z (Titanium concentration X supply rate of liquid I) and instantaneous supply ratio are strictly controlled.
  • a premixing region having functions such as high-speed stirring and high-pressure spray contact may be provided in order to promote uniform contact.
  • the contacting and the reaction are preferably carried out at a temperature as close as possible to 100 ° C. under normal pressure, ie 80 to 98 t: 110 to 150 ° C. under pressure.
  • the solution I and the solution II are brought into contact in the reaction vessel with stirring.
  • the resulting slurry liquid containing solid titanium titanate may be continuously withdrawn from the reaction system and moved to another aging vessel (continuous reaction), or may be withdrawn after the reaction is completed in the reaction vessel. Good (batch reaction).
  • the barium titanate thus produced is desirably aged by heating it for a certain period of time while stirring it in a slurry state.
  • the aging treatment is performed at a temperature of 85 to 150 ° C.
  • the resulting barium titanate particles and water as a solvent are separated by decantation, centrifugation, filtration, or the like.
  • the barium titanate powder separated from the reaction system is washed with water to remove unreacted raw material compounds, alkali components, and the like attached thereto.
  • the production of the unfired barium titanate powder in the present invention is not limited to the above production method.
  • the reaction product obtained above is dried at 80 to 250 ° C, preferably 100 to 200 ° C, to obtain the unfired barium titanate powder of the present invention.
  • the above reaction products are spherical cubic particles having an average particle diameter of 0.05 to 0.5 ⁇ ⁇ ⁇ . Through the above operations, the unfired barium titanate powder of the present invention is obtained.
  • the fired barium titanate powder of the present invention is obtained by subjecting the unfired barium titanate powder to a heat treatment at 930 to 980 ° C., more preferably 940 to 975 (this heat treatment is referred to as firing in the present invention). It is obtained by doing.
  • the firing atmosphere may be any of air, vacuum, and inert gas. However, it is more suitable to remove chlorine, which is an impurity, in a vacuum or when water vapor is present at a partial pressure of 0.1 to 0.4.
  • the unfired barium titanate powder has a property of being fired at 930 to 980 ° C.
  • a tetragonal rectangular parallelepiped fired barium titanate powder having a loss on ignition of 0.5% by weight or less is obtained. Further, the firing temperature Another feature of the present invention is that alkali metals such as sodium ions contained in the crystals are very effectively removed. As a result, a fine baked barium titanate powder having a low purity and a low alkali metal content such as Na can be obtained.
  • the calcined barium titanate is pulverized by various means as necessary.
  • Preferred pulverizing means include pulverizing means by contact between powders, particularly wet pulverizing means, specifically wet pulverizing means in the presence of a medium such as water, rather than pulverizing using media such as balls and beads. It is preferable for maintaining crystallinity.
  • Sintering density The sintering density was determined based on Archimedes' principle.
  • Ba / Ti ratio The atomic ratio of Ba / Ti (BaZTi ratio) was determined by X-ray fluorescence analysis.
  • Example No. BT-12 an unfired barium titanate powder having a Ba / Ti ratio of 1.004 (sample No. BT-12) was obtained.
  • the Na metal content in the powder was 190 ppm.
  • An electron micrograph of the powder BT-12 is shown in FIG.
  • T i C 1 4 aqueous solution (T i C 1 4 concentration: 0.600 mol 1) and, B a C 1 2 / N a OH solution (B aC 1 2 concentration: 0.335 mol Z 1, Na_ ⁇ _H concentration : 3. 0 molar Z 1) and, T i C 1 4 aqueous 100 c cZ min, at B aC 1 2 / NaOH aqueous 2 1 7 cc / min flow rate, the reaction vessel in the same manner as in example 1 , And maintained at 90 ° C with stirring.
  • Molar ratio of B a C 1 2 / ⁇ i C 1 4 of the supplied raw material compound 1. was 2 1 2.
  • Subsequent washing and drying were performed under the same conditions as in Example 1.
  • an unfired barium titanate powder (sample No. BT-3) having 1.06 in & 8 was obtained.
  • Table 1 shows the properties of the unfired barium titanate powders obtained in Examples 1 to 4 and Comparative Examples 5 to 7.
  • Unfired barium titanate powder in Table 1 No. BT-1, BT-2, BT-5, and BT-7 were fired in an air atmosphere at 930 to 1100 for 1.5 hours. Next, 1.5 cc of aqueous ammonia was added per 100 g of the obtained calcined powder, and the mixture was wet-pulverized. After that, water was separated by filtration, and further heated to 120 ° C and dried. The fired barium titanate powders of Examples 5 to 8 and Comparative Examples 4 to 7 shown in Table 1 were obtained. Tables 2 and 3 show the sample numbers and properties of these calcined barium titanate powders.
  • FIG. 2 shows an electron micrograph of the calcined powder: CBT-2B obtained in Example 7. According to FIG. 2, it is clear that the particle shape is a cube or a rectangular parallelepiped. Table 2
  • Table 3 shows the crystallinity and dielectric properties of each fired powder in Table 2.
  • X (te t) as a crystallinity (tetragonality) scale shown in Table 3 is a value obtained by the following method. The closer this value is to 1.0, the higher the crystallinity.
  • the X-ray diffraction peak intensities of the (200) and (002) planes of the crystal are I (200) and I (002), respectively, and the Rabin intensity between the valleys of both peaks is I (ravine), and X (tet ) Is calculated by the following equation.
  • the lengths of the tetragonal C-axis and a-axis are determined by (002) and (200) times of the X-ray diffraction pattern. It is calculated from the folding peak position, and the ratio c / a ratio is calculated by the following formula.
  • MnCo3, MgO, MgCo3, CaCo3, SiO2 and a rare earth oxide were added to the calcined powder (No. CBT-2B) having a BaZTi ratio of 1.004 in Example 7.
  • the mixture was heated at 1300 ° C for 2 hours in a reducing atmosphere, and then sintered at 1,000 ° C for 10 hours under a nitrogen gas flow to obtain a sintered body of Example 9. I got
  • Example 9 instead of No. CBT-2B, calcined barium titanate powder (No. CBT-5) having a Ba / Ti ratio of 1.001 in Comparative Example 6 was used, and the comparison was performed in the same manner. A sintered body of Example 8 was obtained.
  • the dielectric properties (relative permittivity) of the sintered bodies of Example 9 and Comparative Example 8 were measured using an LCR meter (model: 4284A type) manufactured by Hewlett-Packard Company, frequency: 1 mm, and applied voltage: The measurement was performed under the conditions of IV. Table 4 shows the measurement results.
  • the sintered body (Example 9) manufactured using the fired barium titanate powder of the present invention has a high relative dielectric constant over a wide temperature range, and has a high dielectric constant. Proved to be very suitable as a forming material - ⁇ -

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Abstract

L'invention concerne un procédé de production d'une poudre de titanate de baryum cuite quadratique ayant un diamètre moyen des particules compris entre 0,05 et 0,5 νm, un rapport atomique Ba/Ti compris entre 1,003 et 1,006, plus avantageusement entre 1,003 et 1,005 et une perte au feu inférieure ou égale à 0,5 %. Ce procédé consiste à préparer une poudre fine de titanate de baryum quadratique ayant un diamètre moyen des particules compris entre 0,05 et 0,5 νm, un rapport atomique Ba/Ti compris entre 1,003 et 1,009, dans un processus en phase liquide, et à cuire la poudre à une température comprise entre 930 et 980 °C. La poudre de titanate de baryum cuite, obtenue selon ce procédé, possède un indice de cristallinité élevé, une haute propriété diélectrique et une teneur réduite en métaux alcalins, tels que du Na. Cette poudre peut par conséquent être utilisé dans la fabrication d'une couche diélectrique d'un condensateur céramique monolithique ou analogue.
PCT/JP2002/006719 2001-07-04 2002-07-03 Poudre de titanate de baryum et procede de production associe WO2003004415A1 (fr)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006156450A (ja) * 2004-11-25 2006-06-15 Kyocera Corp 積層セラミックコンデンサおよびその製法
WO2006101059A1 (fr) * 2005-03-22 2006-09-28 Nippon Chemical Industrial Co., Ltd Composition de formation de ceramique dielectrique et materiau ceramique dielectrique
JP2007063056A (ja) * 2005-08-30 2007-03-15 Tdk Corp 誘電体磁器組成物の製造方法
JP2007238407A (ja) * 2006-03-10 2007-09-20 Tdk Corp セラミック粉末及びこれを用いた誘電体ペースト、積層セラミック電子部品、その製造方法
JP4965435B2 (ja) * 2005-03-25 2012-07-04 京セラ株式会社 積層セラミックコンデンサおよびその製法

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JPS6016372B2 (ja) * 1980-11-07 1985-04-25 義治 尾崎 チタン酸バリウム（ＢａＴｉｏ↓３）の製造方法
JPH0873219A (ja) * 1994-09-08 1996-03-19 Murata Mfg Co Ltd セラミック粉体の製造方法
JP2000344519A (ja) * 1999-06-02 2000-12-12 Toho Titanium Co Ltd チタン酸バリウム粉末の製造方法
JP2002060219A (ja) * 2000-08-11 2002-02-26 Murata Mfg Co Ltd 微粒チタン酸バリウム粉末、カルシウム変性微粒チタン酸バリウム粉末、ならびにその製造方法

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Publication number Priority date Publication date Assignee Title
JPS6016372B2 (ja) * 1980-11-07 1985-04-25 義治 尾崎 チタン酸バリウム（ＢａＴｉｏ↓３）の製造方法
JPH0873219A (ja) * 1994-09-08 1996-03-19 Murata Mfg Co Ltd セラミック粉体の製造方法
JP2000344519A (ja) * 1999-06-02 2000-12-12 Toho Titanium Co Ltd チタン酸バリウム粉末の製造方法
JP2002060219A (ja) * 2000-08-11 2002-02-26 Murata Mfg Co Ltd 微粒チタン酸バリウム粉末、カルシウム変性微粒チタン酸バリウム粉末、ならびにその製造方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006156450A (ja) * 2004-11-25 2006-06-15 Kyocera Corp 積層セラミックコンデンサおよびその製法
JP4511323B2 (ja) * 2004-11-25 2010-07-28 京セラ株式会社 積層セラミックコンデンサおよびその製法
WO2006101059A1 (fr) * 2005-03-22 2006-09-28 Nippon Chemical Industrial Co., Ltd Composition de formation de ceramique dielectrique et materiau ceramique dielectrique
US7767608B2 (en) 2005-03-22 2010-08-03 Nippon Chemical Industrial Co., Ltd. Dielectric ceramic-forming composition
JP4965435B2 (ja) * 2005-03-25 2012-07-04 京セラ株式会社 積層セラミックコンデンサおよびその製法
JP2007063056A (ja) * 2005-08-30 2007-03-15 Tdk Corp 誘電体磁器組成物の製造方法
JP4706398B2 (ja) * 2005-08-30 2011-06-22 Ｔｄｋ株式会社 誘電体磁器組成物の製造方法
JP2007238407A (ja) * 2006-03-10 2007-09-20 Tdk Corp セラミック粉末及びこれを用いた誘電体ペースト、積層セラミック電子部品、その製造方法

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