WO2015190556A1 - Poudre de particules fines de titanate de baryum, dispersion et film de revêtement - Google Patents

Poudre de particules fines de titanate de baryum, dispersion et film de revêtement Download PDF

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WO2015190556A1
WO2015190556A1 PCT/JP2015/066867 JP2015066867W WO2015190556A1 WO 2015190556 A1 WO2015190556 A1 WO 2015190556A1 JP 2015066867 W JP2015066867 W JP 2015066867W WO 2015190556 A1 WO2015190556 A1 WO 2015190556A1
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barium titanate
particle powder
fine particle
titanate fine
dielectric constant
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PCT/JP2015/066867
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English (en)
Japanese (ja)
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敬介 國森
山本　一美
晴己 黒川
誉元 河口
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戸田工業株式会社
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Priority to JP2016527858A priority Critical patent/JP6635031B2/ja
Priority to CN201580030091.6A priority patent/CN106458630A/zh
Priority to KR1020167034040A priority patent/KR102539617B1/ko
Publication of WO2015190556A1 publication Critical patent/WO2015190556A1/fr

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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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • 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

  • An object of the present invention is to provide a barium titanate fine particle powder which is fine but has a high dielectric constant (relative dielectric constant).
  • Barium titanate having a high dielectric constant is widely used as a dielectric material for multilayer ceramic capacitors.
  • an inorganic film filler such as zirconia is added to a transparent resin to control dielectric constant and refractive index for optical films used for various displays.
  • Liquid crystal display control TFTs are also required to have fine particles and a high dielectric constant as a material for an insulating film or the like in order to reduce power consumption.
  • Patent Documents 1 and 2 barium titanate particle powder whose dielectric constant is increased by performing a heat treatment at 500 ° C. or higher, fine barium titanate particle powder (Patent Document 3) obtained by hydrothermal reaction, etc. are known.
  • the barium titanate fine particle powder satisfying the above properties is currently most demanded, but has not yet been obtained.
  • Patent Documents 1 and 2 described above it is described that the barium titanate particle powder is heat-treated in a temperature range of 500 ° C. or higher. However, since the heat treatment temperature is high, the particle size may be coarsened. .
  • the present invention is a barium titanate fine particle powder having an average primary particle size of 20 to 60 nm and a relative dielectric constant of 300 to 800 (Invention 1).
  • the present invention is the barium titanate fine particle powder according to the present invention 1, wherein the value obtained by dividing the particle size distribution of the primary particles by the average particle size of the primary particles is 0.20 to 0.25 (Invention 2).
  • the present invention is the barium titanate fine particle powder according to claim 1 or 2, wherein the lattice constant ratio c / a is less than 1.003 (Invention 3).
  • the present invention is a dispersion containing the barium titanate fine particle powder according to any one of the present inventions 1 to 3 (Invention 4).
  • the present invention is a coating film containing the barium titanate fine particle powder according to any one of the present inventions 1 to 3 (Invention 5).
  • the barium titanate fine particle powder according to the present invention is suitable for an optical material because it has a high dielectric constant while being very fine particles.
  • Example 1 It is the barium titanate fine particle powder (before heat treatment) used in Example 1. It is a barium titanate fine particle powder (after heat treatment) obtained in Example 1.
  • the average particle diameter (x) of the primary particles of the barium titanate fine particle powder according to the present invention is 20 to 60 nm.
  • the average particle size is preferably 22 to 58 nm, more preferably 25 to 55 nm.
  • the barium titanate fine particle powder according to the present invention has a relative dielectric constant of 300 to 800 measured by an evaluation method described later. By controlling the relative dielectric constant of the barium titanate fine particle powder within the above range, fine particles with suppressed particle growth can be obtained. A more preferable relative dielectric constant is 410 to 750.
  • the value obtained by dividing the particle size distribution ( ⁇ ) of the primary particles of the barium titanate fine particles according to the present invention by the average particle size (x) of the primary particles is preferably 0.20 to 0.25. By controlling the numerical value within the above range, it becomes a barium titanate fine particle powder having an excellent particle size distribution. A more preferred range is 0.205 to 0.248.
  • the crystallinity of the barium titanate fine particle powder according to the present invention is less than 1.003 when expressed by the lattice constant ratio c / a using the a-axis length (a) and the c-axis length (c) of the lattice constant. preferable. Barium titanate fine particle powder having a lattice constant ratio c / a of 1.003 or more is difficult to produce industrially with the particle size of the present invention.
  • the specific surface area of the barium titanate fine particle powder according to the present invention is preferably 10 to 80 m 2 / g. In the case of less than 10 m 2 / g, the particle powder becomes coarse and particles are sintered between the particles, and the dispersibility is easily impaired when the binder is mixed. It is difficult to industrially produce fine barium titanate powder having a specific surface area value exceeding 80 m 2 / g.
  • the half width (FWHM) of the (111) plane calculated from the X-ray diffraction peak of the barium titanate fine particle powder according to the present invention is preferably 0.2 to 0.4.
  • the particle shape of the barium titanate fine particle powder according to the present invention is preferably spherical or granular.
  • the barium titanate fine particle powder according to the present invention can be obtained by heat-treating a barium titanate fine particle powder having an average particle diameter of 10 to 50 nm prepared in advance by a hydrothermal reaction in a temperature range of 100 to 400 ° C.
  • the hydrothermal reaction is not particularly limited.
  • a barium hydroxide aqueous solution is dropped and neutralized in a titanium chloride aqueous solution to obtain a titanium hydroxide colloid, and then the titanium hydroxide colloid is converted into water. It put into the barium oxide aqueous solution, and the obtained mixed solution was heated, and barium titanate was produced
  • hydrothermal treatment is performed in a temperature range of 100 to 250 ° C., washing with water, drying and pulverization.
  • barium titanate having different sizes can be produced by changing the reaction temperature, concentration, pH, and the like.
  • the average particle size of barium titanate obtained by hydrothermal reaction is preferably 10 to 50 nm.
  • the barium titanate fine particle powder intended for the present invention can be obtained.
  • the heat treatment temperature within the above range, growth of the particle diameter of the barium titanate fine particles can be suppressed and the dielectric constant can be increased. If the heat treatment temperature is too high, the particles may be fused together.
  • the heat treatment time is preferably 1 to 3 hours.
  • the dispersion medium in the present invention either an aqueous system or a solvent system can be used.
  • a dispersion medium of the aqueous dispersion water or alcohol solvents such as methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, and butyl alcohol; glycol ether solvents such as methyl cellosolve, ethyl cellosolve, propyl cellosolve, and butyl cellosolve; Oxyethylene or oxypropylene addition polymers such as diethylene glycol, triethylene glycol, polyethylene glycol, dipropylene glycol, tripropylene glycol, and polypropylene glycol; alkylene glycols such as ethylene glycol, propylene glycol, and 1,2,6-hexanetriol; glycerin Water-soluble organic solvents such as 2-pyrrolidone can be used.
  • alcohol solvents such as methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, and butyl alcohol
  • glycol ether solvents such as methyl cellosolve, ethyl
  • Dispersion media for solvent-based dispersions include aromatic hydrocarbons such as toluene and xylene; ketones such as methyl ethyl ketone and cyclohexanone; amides such as N, N-dimethylformamide, N, N-dimethylacetamide and N-methylpyrrolidone
  • Ether glycols such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol monomethyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether; ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, propylene glycol monomethyl Ether acetates such as ether acetate and propylene glycol monoethyl ether acetate; Acetates such as butyl acetate and isobutyl acetate; lactate esters such as lactate methyl ester, lactate ethyl este
  • the disperser used for producing the dispersion according to the present invention is not particularly limited, and an apparatus that can apply shearing force, impact force, compressive force, and / or frictional force to the powder layer is preferable.
  • a roller mill, a high-speed rotary mill, a high-speed rotary mill with a built-in classifier, a ball mill, a medium agitation mill, an airflow-type pulverizer, a compaction shear mill, a colloid mill, a roll mill and the like can be used.
  • the dispersion according to the present invention contains barium titanate particle powder in an amount of 0.1 to 60 parts by weight, preferably 0.5 to 50 parts by weight, more preferably 1 to Contains 40 parts by weight.
  • the base material of the dispersion of the barium titanate particle powder includes a dispersion medium in addition to the barium titanate particle powder, and if necessary, a dispersant, an additive (resin, antifoaming agent, auxiliary agent, etc.) Etc. can also be added.
  • the dispersant in the present invention can be appropriately selected and used according to the type of barium titanate particle powder and dispersion medium used, and organosilicon compounds such as alkoxysilane, silane coupling agent and organopolysiloxane , Surfactants or polymer dispersants can be used, and these can be used alone or in combination of two or more.
  • organosilicon compound examples include methyltrimethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, phenyltriethoxysilane, ethyltriethoxysilane, propyltriethoxysilane, butyltriethoxysilane, hexyltriethoxysilane, and octyltriethoxy.
  • Silanes alkoxysilanes such as tetraethoxysilane and tetramethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, ⁇ -aminopropyltriethoxysilane, ⁇ -glycidoxypropyltrimethoxysilane, ⁇ -mercaptopropyltrimethoxysilane, ⁇ -Methacryloyloxypropyltrimethoxysilane, N- ( ⁇ -aminoethyl) - ⁇ -aminopropyltrimethoxysilane, ⁇ -glycidoxypropylmethyldimethoxy Orchids, .gamma.-chloropropyl trimethoxy silane silane coupling agent such as a polysiloxane, methyl hydrogen polysiloxane, organopolysiloxane and the like of the modified polysiloxane.
  • alkoxysilanes such as
  • surfactant examples include anionic surfactants such as fatty acid salts, sulfate ester salts, sulfonate salts and phosphate ester salts; polyethylene glycol type nonionic surfactants such as polyoxyethylene alkyl ethers and polyoxyethylene aryl ethers Agents, nonionic surfactants such as polyhydric alcohol type nonionic surfactants such as sorbitan fatty acid esters; chaotic surfactants such as amine salt type cationic surfactants and quaternary ammonium salt type cationic surfactants Agents: amphoteric surfactants such as alkylbetaines such as alkyldimethylaminoacetic acid betaine and alkylimidazolines.
  • anionic surfactants such as fatty acid salts, sulfate ester salts, sulfonate salts and phosphate ester salts
  • polyethylene glycol type nonionic surfactants such as polyoxyethylene alkyl ethers and polyoxy
  • styrene-acrylic acid copolymer a styrene-maleic acid copolymer, a polycarboxylic acid, a salt thereof, and the like can be used.
  • the amount of the dispersant added depends on the total surface area of the barium titanate particle powder in the dispersion and may be appropriately adjusted according to the use of the barium titanate particle powder dispersion and the type of the dispersant. Specifically, by adding 0.01 to 100% by weight of a dispersant with respect to the barium titanate particle powder in the dispersion medium, the barium titanate particle powder can be uniformly and finely dispersed in the dispersion medium. At the same time, the dispersion stability can be improved. In addition to adding the dispersing agent directly to the dispersion medium, the dispersing agent may be pretreated in the barium titanate particle powder.
  • the coating film according to the present invention is prepared by adding a resin to the above-mentioned dispersion, mixing, and then forming on a film such as a PET film using a coater such as a bar coater or a spin coater.
  • a resin to be used acrylic resin, silicone resin, epoxy resin, polyester resin, polyimide resin, polymethyl methacrylate (PMMA), polystyrene (PS), polycarbonate (PC) and the like are generally used.
  • the total light transmittance is 85% or more, the haze is 0.65 or more, and the transparency is excellent. Is.
  • the present invention fine particles of barium titanate having a high dielectric constant while being fine are obtained.
  • the fine barium titanate particle powder after the hydrothermal reaction is subjected to heat treatment in a temperature range in which sintering between particles is less likely to occur, so that the particles of the barium titanate particle powder before the heat treatment are granulated.
  • the diameter, the lattice constant ratio c / a, and the half width of the (111) reflection were hardly changed, and only the dielectric constant could be improved.
  • the particle size effect is considered.
  • the relative dielectric constant of the barium titanate particle powder having a particle size of 175 nm obtained by the hydrothermal reaction was about 130. Since the particle growth by the heat treatment in the present invention is sufficiently small, it is considered that the result of the present invention cannot be explained only by the influence of the increase in the particle size on the dielectric constant. Another possible cause of the increase in the dielectric constant due to heat treatment is the modification of the particle surface layer by removing hydroxyl groups. In general, the heat treatment at low temperature cannot be expected to change the characteristics. However, in the present invention, since the barium titanate particles to be heat-treated are nano-sized, it is considered that the surface area is large and the dielectric constant is greatly increased.
  • the heat treatment can be performed at a higher temperature to improve the inside of the particle, further improvement in the dielectric constant can be expected.
  • the heat treatment at a high temperature causes the particle diameter to grow rapidly due to fusion between particles. This is not suitable for the production of barium titanate particle powder for optical film use.
  • a typical embodiment of the present invention is as follows.
  • the average particle diameter (x) of the primary particles of the barium titanate fine particle powder is about 500 particles in a photograph (magnification 50,000 times) observed with a scanning electron microscope (Hitachi, Ltd. S-4300). The diameter was measured and the particle size distribution ( ⁇ ) was determined.
  • the average particle size of primary particles is a particle size obtained by setting the diameter of a circle having an area equivalent to the area obtained from a photograph for each particle as the particle size and averaging it for all measured particles. In order to make it difficult for the difference in the measured values depending on the field of view, each field of view was observed widely at a low magnification, and the field of view was considered average.
  • the fine barium titanate powder was evaluated by powder X-ray diffraction, and the c / a ratio of the lattice constant and the full width at half maximum (FWHM) of the (111) plane were measured.
  • the specific surface area value is a value measured by the BET method.
  • the relative dielectric constant of the barium titanate fine particle powder was measured by the following evaluation method. That is, a mixture of 2.5 g of barium titanate fine particle powder and 0.5 g of a polyvinyl alcohol aqueous solution having a concentration of 3 wt% is compacted at a pressure of 100 kg / cm 2 , and has a disk shape with a diameter of 25 mm and a thickness of 1 to 2 mm. A green compact was produced. Since the green compact contains water, it was left in a dry air at 50 ° C. for 12 hours or more. From the weight and volume of the green compact after drying, the volume ratio of barium titanate particle powder, PVA and voids was determined.
  • the green compact was adjusted so that the barium titanate fine particle powder was 41 to 55 vol%, the PVA was 0.1 to 3 vol%, and the balance was a void.
  • the relative dielectric constant at 10 MHz was measured in an environment of room temperature of about 25 ° C. and humidity of about 40% RH using an impedance analyzer E4991A manufactured by Agilent and a dielectric constant measurement fixture 16453A. Since the measurement result of the obtained relative dielectric constant includes contributions from the respective components of barium titanate particle powder, PVA and voids, the present invention uses only the logarithmic mixing rule to determine only the barium titanate from the measured values. The contribution was estimated.
  • Example 1 Barium hydroxide octahydrate (manufactured by Kanto Chemical Co., Ltd., 97% Ba (OH) 2 / 8H 2 O reagent special grade) 1.12 kg dissolved in water and purified, dropped into 688 g of titanium chloride aqueous solution and neutralized Thus, a titanium hydroxide colloid was obtained. Next, 1.28 kg of barium hydroxide octahydrate dissolved and purified in water was kept in a reaction vessel in a nitrogen atmosphere at a temperature of 70 ° C. and a pH of 12.5. Next, the titanium hydroxide colloid was charged into the barium hydroxide aqueous solution over 2 minutes. The mixed solution produced barium titanate at 100 ° C. for 0.5 hour.
  • barium titanate fine particle powder After cooling to room temperature, it was washed with Nutsche until no Ba ions were observed in the filtrate, filtered and dried to obtain barium titanate fine particle powder.
  • the average particle diameter of the obtained barium titanate fine particle powder was 32 nm.
  • An electron micrograph of the obtained barium titanate fine particle powder is shown in FIG.
  • the obtained barium titanate particle powder having an average particle diameter of 32 nm was heated in the air at 400 ° C. for 2 hours using an electric furnace.
  • the obtained heat-treated powder was observed by SEM, some particles fused to a size of about several tens of nanometers were seen in firing at 400 ° C., but the particle size was 60 nm or less, and the overall particle growth was It was slight.
  • An electron micrograph of the obtained barium titanate fine particle powder is shown in FIG.
  • Example 2 The barium titanate particle powder having an average particle size of 46 nm was obtained by changing the conditions of the hydrothermal reaction, and then heat-treated at a temperature of 400 ° C. by the same method as described in Example 1 to obtain the barium titanate fine particle powder. Obtained. Various characteristics of the obtained barium titanate fine particle powder are shown in 1.
  • Example 3 The barium titanate particle powder having an average particle diameter of 51 nm was obtained by changing the conditions of the hydrothermal reaction, and then heat-treated at a temperature of 400 ° C. by the same method as described in Example 1 to obtain the barium titanate fine particle powder. Obtained. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Example 4 Barium titanate fine particle powder was obtained in the same manner as in Example 1 except that the heat treatment temperature was changed to 300 ° C. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Example 5 Barium titanate fine particle powder was obtained in the same manner as in Example 2 except that the heat treatment temperature was changed to 300 ° C. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Example 6 The barium titanate particle powder having an average particle diameter of 20 nm was obtained by changing the hydrothermal reaction conditions, and then heat-treated at a temperature of 300 ° C. in the same manner as described in Example 1 to obtain the barium titanate fine particle powder. Obtained. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Example 7 Barium titanate particles having an average particle diameter of 32 nm were heat-treated at a temperature of 100 ° C. in the same manner as described in Example 1, and the relative permittivity, c / a ratio, half width and specific surface area were determined as in Example 1. Evaluation was performed in the same manner as described in 1. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Comparative Example 1 The relative dielectric constant, c / a ratio, half width and specific surface area of the barium titanate particles having an average particle diameter of 32 nm before heat treatment obtained in Example 1 were evaluated in the same manner as described in Example 1. went. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Comparative Example 2 The relative dielectric constant, c / a ratio, half width and specific surface area of the barium titanate particles having an average particle diameter of 46 nm before heat treatment obtained in Example 2 were evaluated in the same manner as described in Example 1. went. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Comparative Example 3 The relative dielectric constant, c / a ratio, half width and specific surface area of the barium titanate particles having an average particle diameter of 51 nm before heat treatment obtained in Example 3 were evaluated in the same manner as described in Example 1. went. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Comparative Example 4 Barium titanate particles having an average particle diameter of 32 nm were heat-treated at a temperature of 700 ° C. in the same manner as described in Example 1, and the relative permittivity, c / a ratio, half width and specific surface area were determined as in Example 1. Evaluation was performed in the same manner as described in 1. Although the relative dielectric constant is greatly increased by the heat treatment at high temperature, the average particle size is also greatly increased. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Comparative Example 5 The relative dielectric constant, c / a ratio, half width and specific surface area of unheat-treated barium titanate particles having an average particle diameter of 62 nm were evaluated in the same manner as described in Example 1. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Comparative Example 6 The relative dielectric constant, c / a ratio, half width and specific surface area of unheat-treated barium titanate particles having an average particle size of 64 nm were evaluated in the same manner as described in Example 1. Various properties of the obtained barium titanate fine particle powder are shown in Table 1.
  • Comparative Example 7 The relative dielectric constant of the barium titanate particle powder prepared by the solid phase method was measured by the same method as described in Example 1. As a result, the relative dielectric constant at 10 MHz was about 170.
  • Example 8 The barium titanate particles obtained in Example 1 were placed in a zirconia 0.5-liter stirring vessel of a vertical bead mill (“Ultra Apex Mill UAM-05” manufactured by Kotobuki Giken Kogyo Co., Ltd.) with zirconia beads (particle size 50 ⁇ m). Add a solution in which ED153 (manufactured by Enomoto Kasei) and PGMEA as a solvent are mixed as a dispersant, and disperse for 1 hour while circulating to disperse the barium titanate particle powder dispersion. Obtained.
  • ED153 manufactured by Enomoto Kasei
  • PGMEA PGMEA
  • Examples 10 and 11 The barium titanate particle powders of Examples 3 and 6 were formed into sheets according to the methods of Examples 8 and 9. Various properties of the obtained sheet are shown in Table 2.
  • Comparative Examples 8 and 9 The barium titanate particle powders of Comparative Examples 1 and 2 were formed into sheets according to the methods of Examples 8 and 9. Various properties of the obtained sheet are shown in Table 2.
  • the coating films (Examples 9 to 11) using the barium titanate particles (Examples) according to the present invention had a total light transmittance of 85% or more and a haze of 0.1. It was found to be 65 or more and excellent in transparency.
  • the barium titanate particles according to the present invention can be suitably used for various dielectric materials because aggregation is suppressed and the dispersibility is excellent. Since the barium titanate particle powder according to the present invention has a high dielectric constant, it is considered that when the barium titanate particle powder and the transparent resin are mixed, the amount of the barium titanate particle powder used can be suppressed than before, Moreover, since barium titanate is a fine particle, it becomes easy to ensure the transparency required for optical film applications.

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Abstract

La présente invention concerne : une poudre de particules de titanate de baryum ayant une constante diélectrique élevée tout en conservant une petite taille de particule et étant appropriée à une utilisation dans des films optiques et analogues ; et un procédé de production de titanate de baryum avec lequel il est possible de produire efficacement ladite poudre de particules de titanate de baryum. Cette poudre de particules fines de titanate de baryum présente un diamètre de grain moyen de particule primaire allant de 20 à 60 nm, et une permittivité relative allant de 300 à 800, la valeur obtenue en divisant la distribution de taille de grain de particule primaire par la taille de grain moyenne de particule primaire étant comprise entre 0,20 et 0,25.
PCT/JP2015/066867 2014-06-13 2015-06-11 Poudre de particules fines de titanate de baryum, dispersion et film de revêtement WO2015190556A1 (fr)

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JP2016527858A JP6635031B2 (ja) 2014-06-13 2015-06-11 チタン酸バリウム微粒子粉末、分散体及び塗膜
CN201580030091.6A CN106458630A (zh) 2014-06-13 2015-06-11 钛酸钡微粒粉末、分散体和涂膜
KR1020167034040A KR102539617B1 (ko) 2014-06-13 2015-06-11 티타늄산바륨 미립자 분말, 분산체 및 도막

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WO2016140305A1 (fr) * 2015-03-05 2016-09-09 戸田工業株式会社 Poudre de particules de titanate de baryum, dispersion et film de revêtement contenant cette poudre

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JP6972115B2 (ja) * 2017-04-04 2021-11-24 デンカ株式会社 粉末混合物

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JPH05330824A (ja) * 1991-04-19 1993-12-14 Teika Corp チタン酸バリウムおよびその製造方法
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