WO2021066070A1 - Particules de titanate de baryum ainsi que procédé de fabrication de celles-ci, et dispersion liquide de particules de titanate de baryum - Google Patents

Particules de titanate de baryum ainsi que procédé de fabrication de celles-ci, et dispersion liquide de particules de titanate de baryum Download PDF

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WO2021066070A1
WO2021066070A1 PCT/JP2020/037304 JP2020037304W WO2021066070A1 WO 2021066070 A1 WO2021066070 A1 WO 2021066070A1 JP 2020037304 W JP2020037304 W JP 2020037304W WO 2021066070 A1 WO2021066070 A1 WO 2021066070A1
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barium titanate
titanate particles
barium
organic solvent
mixed solution
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PCT/JP2020/037304
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English (en)
Japanese (ja)
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和馬 渡邉
光章 熊澤
良 村口
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日揮触媒化成株式会社
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Priority to JP2021551421A priority Critical patent/JPWO2021066070A1/ja
Priority to KR1020217037796A priority patent/KR20220074821A/ko
Priority to CN202080042148.5A priority patent/CN113939476B/zh
Publication of WO2021066070A1 publication Critical patent/WO2021066070A1/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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H01G4/008—Selection of materials
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/30—Three-dimensional structures
    • C01P2002/34—Three-dimensional structures perovskite-type (ABO3)

Definitions

  • the present invention relates to barium titanate particles having a perovskite structure.
  • Barium titanate particles are used as dielectric materials for electronic parts and optical materials with high refractive index and excellent transparency. Barium titanate particles have a high dielectric constant and are therefore used in multilayer ceramic capacitors (MLCCs).
  • the MLCC has a structure in which electrode layers and dielectric layers are alternately overlapped.
  • the electrode layer contains Ni particles having a diameter of 80 to 300 nm and barium titanate particles as a co-material.
  • barium titanate particles are packed around the Ni particles. Therefore, the temperature at which Ni particles are sintered is high. That is, the effect of delaying the sintering of Ni particles can be obtained. Therefore, the temperature at which the Ni particles are sintered and the temperature at which the dielectric layer is sintered are close to each other. As a result, the difference in shrinkage between the electrode layer and the dielectric layer becomes small during firing, and an MLCC with few cracks can be obtained (see, for example, Patent Document 1).
  • the barium titanate particles have a perovskite structure, and the c-axis axis length of the crystal lattice is made longer than the a-axis axis length, that is, barium titanate. It is known that barium particles are tetragonal. (See, for example, Patent Document 2).
  • the barium titanate particles of Patent Document 2 have a high dielectric constant because the c-axis length of the perovskite structure is longer than the a-axis length.
  • barium titanate particles are pulverized and then fired, the particle size and crystallite diameter tend to increase. Therefore, the density of the barium titanate particles packed around the Ni particles tends to be low, and it is difficult to obtain the sintering delay effect.
  • An object of the present invention is to provide barium titanate particles having a high sintering delay effect and a method for producing the same.
  • the atomic ratio Ba / Ti of barium and titanium was set to 0.9 to 1.1, and the crystallite diameter was set to 5 to 25 nm.
  • the atomic ratio Ba / Ti of barium and titanium may be 0.95 to 1.05.
  • the ratio c / a of the lengths of the c-axis and the a-axis of the crystal lattice in the perovskite structure is preferably 1.005 or less.
  • the water content is preferably less than 3% by weight.
  • the method for producing barium titanate particles is a step of mixing barium hydroxide and alkyl cellosolve, and titanium alkoxide so that the atomic ratio Ba / Ti of barium and titanium is in the range of 0.9 to 1.1. It includes a step of adding, a step of adding water, and a step of heating.
  • the barium titanate particles having a perovskite structure according to the present invention have a barium-titanium atomic ratio Ba / Ti in the range of 0.9 to 1.1. As a result, impurities such as crystals other than the perovskite structure are less likely to be generated.
  • the crystallite diameter of the barium titanate particles is 5 to 25 nm. Therefore, the crystallinity of the barium titanate particles becomes high, and the particle size becomes small. Since such barium titanate particles enter the gaps between the Ni particles in the electrode layer, the barium titanate particles are present at a high density around the Ni particles. Therefore, the sintering delay effect of Ni becomes high.
  • the crystallite diameter When the crystallite diameter is larger than 25 nm, the viscosity of the dispersion liquid of barium titanate particles described later becomes high.
  • the particle size measured by a transmission electron microscope is also 5 to 25 nm.
  • the atomic ratio Ba / Ti of barium and titanium may be 0.95 to 1.05.
  • the ratio (axial ratio) c / a of the lengths of the c-axis and the a-axis of the crystal lattice in the perovskite structure is preferably 1.005 or less. This makes the barium titanate particles closer to cubic crystals. Therefore, the sintering delay effect of Ni becomes high.
  • the crystal structure and crystallite diameter can be measured using RINT-Ultima manufactured by Rigaku, which is an X-ray diffraction measuring device.
  • the crystal structure can be identified using PDXL, which is analysis software.
  • D is the crystallite diameter ( ⁇ )
  • K is the Scherrer constant
  • ⁇ is the X-ray wavelength (1.7889 ⁇ )
  • ⁇ is the reflection angle.
  • the axial ratio c / a is preferably 1.003 or less. More preferably 1.001 or less. The smaller the axial ratio c / a, the higher the sintering delay effect of Ni.
  • Barium titanate particles include Group 2, Group 3, Lantanoid, Actinoid, Group 4, Group 5, Group 6, Group 7, Group 8, Group 9, Group 10, Group 11, Group 12, Group 13, and. It is preferable that at least one element selected from Group 14 (hereinafter referred to as an additive element) is contained. As a result, the sintering delay effect is enhanced. It is more preferable that the additive element is contained in an amount of 0.1 to 10 mol% when the composition formula BaTIO 3 of barium titanate is 100 mol%. As a result, the sintering delay effect of Ni can be easily obtained. Moreover, even if the additive element is contained in this range, no peak other than the perovskite structure is observed.
  • a paste for printing the electrode layer can be prepared using a dispersion of barium titanate particles.
  • the dispersion of barium titanate particles contains barium titanate particles and an organic solvent.
  • the water content of the dispersion is preferably less than 3% by weight. When the water content is small, the viscosity of the paste is unlikely to increase even if a binder such as ethyl cellulose is added to the dispersion liquid. If the viscosity of the paste is high, it is difficult to apply the paste uniformly, so that cracks are likely to occur in the electrode layer during firing. Further, when the water content of the dispersion liquid is 3% by weight or less, the dispersion liquid is less likely to aggregate.
  • the amount of water adsorbed on the solid content of the dispersion liquid is preferably 5 parts by mass or more with respect to 100 parts by mass of the solid content.
  • the barium titanate particles in the dispersion have many hydroxyl groups on the surface.
  • the solid content is obtained by drying the dispersion at 200 ° C. for 3 hours.
  • the adsorbed water content is the amount of water adsorbed on the solid content when the solid content is exposed to the condition of 90 RH% at 25 ° C. for 1 hour.
  • the barium titanate particles are not surface-treated.
  • the viscosity of the paste tends to decrease.
  • the viscosity of the paste tends to be further lowered.
  • an organic acid-based surface treatment agent such as linoleic acid or oleic acid
  • the viscosity of the paste may increase.
  • the barium titanate particles may be surface-treated with a surface treatment agent as long as the viscosity of the paste does not increase.
  • the organic solvent preferably has an OH group. That is, it is preferable that the organic solvent has high hydrophilicity. As a result, the viscosity of the dispersion liquid or the paste tends to decrease.
  • the organic solvent has an OH group and the adsorbed water content is 5 parts by mass or more with respect to 100 parts by mass of the solid content, the viscosity of the dispersion liquid tends to be low.
  • the organic solvent preferably has at least one of an ester bond, an ether bond, and a ketone group together with an OH group. This makes the organic solvent more hydrophilic. In particular, by having an ether bond, high hydrophilicity can be obtained.
  • the organic solvent preferably has a hydrophobic structure together with the OH group.
  • the hydrophobic structure represents a cyclic structure or a chain structure in which two or more carbon atoms are continuously carbon-carbon bonded from the end.
  • the cyclic structure include a cyclic hydrocarbon group (R 6 ) which is a monovalent substituent obtained by removing a hydrogen atom from an arbitrary carbon atom such as cycloalkane, cycloalkene (cycloolefin), and aromatic ring.
  • R 6 may be any of a three-membered ring, a four-membered ring, a five-membered ring, a six-membered ring, a seven-membered ring, and the like. Illustrating the structure of R 6 six-membered ring in FIG. 1, (a) is a six-membered ring aromatic ring, (b) is a six-membered ring cycloalkene, and (c) is a six-membered ring cycloalkane. In the structure of R 6 , a part of the carbon atom may be replaced with a hetero atom such as oxygen, nitrogen or sulfur atom.
  • R 1 to R 5 can be selected from a hydrophilic group such as a hydrogen group, an OH group and a carboxy group, and a hydrophobic group such as a methyl group, an ethyl group, an isopropyl group and a t-butyl group.
  • R 1 to R 5 may be the same or different.
  • R 1 to R 5 are preferably four hydrogen groups and one methyl group. As a result, the compatibility between the organic solvent and the binder is increased.
  • the organic solvent having a cyclic structure can be represented by R 6 to R 7 (however, R 7 has a structure containing elements such as carbon, hydrogen, nitrogen and oxygen).
  • the OH group is preferably contained in R 7.
  • the organic solvent enhances the compatibility between the binder and the barium titanate particles.
  • Examples of the chain structure include a linear structure such as an alkyl group and a branched structure such as an isopropyl group and a tert-butyl group.
  • the organic solvent having a chain structure can be expressed as R 3- CR 4 R 5- CH 3 by the demonstrative formula.
  • the methyl group (-CH 3 ) is the terminal.
  • the carbon atom bonded to the terminal methyl group is the second carbon atom from the terminal. That is, the carbon atom of the methyl group and the carbon atom bonded to the methyl group are continuously carbon-carbon bonded from the end.
  • R 3 , R 4 and R 5 have a structure containing elements such as carbon, hydrogen, nitrogen and oxygen.
  • R 3 , R 4 and R 5 may be combined to form a cyclic structure.
  • the organic solvent has a hydrophobic structure, it is considered that the compatibility between the organic solvent and the binder is high.
  • the organic solvent has a hydrophobic structure and an OH group, the organic solvent enhances the compatibility between the binder and the barium titanate particles. Therefore, the paste is less likely to aggregate.
  • the number of carbon atoms that form a continuous carbon-carbon bond from the end of the chain structure is preferably 5 or less. This increases the hydrophilicity of the organic solvent. More preferably, the number of carbon atoms in a carbon-carbon bond is 4 or less.
  • the organic solvent has an ether bond, it is preferable that the alkyl group is bonded to the oxygen atom of the ether bond.
  • the alkyl group preferably has 3 to 5 carbon atoms.
  • the solubility parameter (SP value) of the organic solvent is preferably 8.5 or more. When it is 8.5 or more, the hydrophilicity of the organic solvent becomes high.
  • the boiling point of the organic solvent under atmospheric pressure is preferably 300 ° C. or lower.
  • the carbon chain of the organic solvent is shorter than that of the organic solvent having a boiling point higher than 300 ° C. Therefore, the viscosity of the dispersion liquid decreases. Further, since the viscosity of the printing paste is also lowered, the printing paste is easily applied uniformly at the time of printing.
  • the boiling point of the organic solvent under atmospheric pressure is preferably 200 to 300 ° C. As a result, when the paste is applied and dried, the paste is easily dried uniformly with the Ni particles and the barium titanate particles dispersed. Therefore, the effect of delaying the sintering of Ni particles becomes high. In addition, cracks are less likely to occur in the MLCC.
  • the viscosity of the organic solvent is preferably 100 mPa ⁇ s or less at 25 ° C. under atmospheric pressure. As a result, the viscosity of the dispersion liquid is lowered, and the viscosity of the printing paste is also lowered.
  • a hydroxide of barium and an alkyl cellosolve as a solvent are mixed to prepare a mixed solution A (first step).
  • a hydroxide of barium and an alkyl cellosolve as a solvent are mixed to prepare a mixed solution A (first step).
  • the solvent is alkyl cellosolve
  • the viscosity of the dispersion is reduced.
  • the viscosity of the paste is less likely to increase.
  • the water content of the mixed solution A is preferably 5% by mass or less. This makes it difficult for the titanium alkoxide to be hydrolyzed when the titanium alkoxide described later is added. Therefore, the particle size tends to be small.
  • the mixed liquid A may be depressurized or heated before the second step described later to reduce the water content of the mixed liquid A to 5% by mass or less.
  • the mixed solution B preferably has an atomic ratio Ba / Ti of barium and titanium of 0.95 to 1.05. Within this range, crystals other than the perovskite structure are less likely to be formed.
  • the atomic ratio of barium to titanium may be 0.9 to 1.1.
  • Titanium alkoxide is preferably added in a nitrogen atmosphere. This slows down the reaction rate of the titanium alkoxide. Therefore, barium titanate particles having a small particle size and crystallite size can be easily obtained.
  • the structure of the titanium alkoxide is preferably "Ti (OR) 4".
  • R is a hydrocarbon group having 1 to 4 carbon atoms, or a substituted hydrocarbon group in which one or more of these hydrogen atoms are substituted with halogen atoms. Further, R may be the same as or different from each other. With such a structure, the crystallinity of barium titanate particles tends to be high. Specific examples thereof include titanium tetramethoxyde, titanium tetraethoxydo, titanium tetra n propoxide, titanium tetraisopropoxide, titanium tetra n butoxide, titanium tetraisobutoxide and the like.
  • the amount of water added is preferably the number of moles equal to or more than the equivalent amount of titanium alkoxide. As a result, the amount of titanium alkoxide remaining in the mixed solution C without being hydrolyzed is reduced. Therefore, the crystallinity of the barium titanate particles is increased.
  • the mixed liquid C is heated (fourth step). It is preferable to heat at 40 ° C. or higher for 2 to 200 hours. Aging proceeds by this step, and barium titanate particles are generated in the aged product.
  • the heating temperature is 40 ° C. or higher, the particle size distribution tends to be uniform, although it depends on the gel concentration. Furthermore, the crystallinity is improved. Further, a heating temperature of 120 ° C. or lower is industrially easy to handle. When heated for 2 hours or more, the particle size distribution tends to be uniform. Furthermore, the crystallinity tends to improve. If the heating time is 200 hours or less, the particle size and crystallite size tend to be small. More preferably, it is 5 hours or more and 100 hours or less.
  • the water content of the dispersion is adjusted to less than 3% by weight.
  • Organic solvents may be added prior to ultrafiltration or distillation. Ultrafiltration is preferred when the boiling point of the organic solvent is lower than the alkyl cellosolve. If it is higher than alkyl cellosolve, distillation is preferred.
  • the organic solvent preferably has the characteristics of the organic solvent described in the description of the dispersion liquid described above.
  • the dispersion prepared by such a manufacturing method has a small amount of water. Therefore, the viscosity of the paste is less likely to increase.
  • the barium titanate particles in the dispersion have a small particle size and crystallite diameter, and have high crystallinity. Furthermore, since the crystal system of barium titanate particles is close to that of cubic crystals, the effect of delaying the sintering of Ni becomes high when used in the electrode layer.
  • the 2nd, 3rd, lanthanoid, actinoid, 4th, 5th, 6th, 7th, 8th, 9th, 10th, 11th, 12th, and 13th groups are preferable to add.
  • a metal salt containing at least one selected from Group 14 and Group 14. By adding such a metal salt, the sintering delay effect is enhanced. Further, since it is a metal salt, it becomes difficult to form crystals other than the perovskite structure. Furthermore, by adding the metal salt prior to the fourth step, the metal salt is dispersed in the barium titanate gel. Therefore, the sintering delay effect tends to be high.
  • Example 1 ⁇ Preparation of dispersion> 50 g of barium hydroxide / octahydrate (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.) and 315 g of 2-methoxyethanol (methylcellosolve) were placed in a beaker and dissolved at 30 ° C. for 20 minutes. The Ba concentration of this solution was 6.0% by weight and the water content was 6.2% by weight. This solution was placed in a 1 dm 3 eggplant-shaped flask and distilled with a rotary evaporator to obtain a mixed solution A. The distillation conditions were 1 hour at a temperature of 70 ° C. and a reduced pressure of 0.015 MPa. The Ba concentration of the mixed solution A was 16.0% by weight, and the water content was 0.5% by weight.
  • the dispersion was measured as follows. The measurement results of each Example and Comparative Example are shown in Table 2.
  • ⁇ Measurement of adsorbed water content 30 g of the dispersion was dried at 200 ° C. for 3 hours and cooled in a desiccator to obtain a dry powder. The dry powder was allowed to stand for 1 hour in a constant temperature and humidity chamber (PL-3J manufactured by ESPEC CORPORATION) adjusted to 25 ° C. and 90 RH%. The amount of adsorbed water was calculated from the weight change before and after that.
  • a binder solution was prepared by dispersing 3 g of ethyl cellulose powder in 74 g of tarpineol (manufactured by Yasuhara Chemical Co., Ltd.). 4.5 g of this binder liquid and 3 g of the dispersion liquid were mixed to obtain a paste for measuring viscosity.
  • ⁇ Preparation of paste for dielectric layer> 90 g of barium titanate (manufactured by Sakai Chemical Co., Ltd .: BT-01, average particle size 300 nm) and 10 g of ethyl cellulose powder were added to 56.5 g of a tarpineol solvent and first dispersed using Awatori Rentaro. Further, a paste for a dielectric layer was prepared by secondary dispersion using three rolls.
  • Example 1 In the following Examples and Comparative Examples, each sample was prepared, measured and evaluated in the same manner as in Example 1.
  • Example 2 A dispersion was obtained in the same manner as in Example 1 except that the mixed solution of Example 1 was changed to a mixed solution of 71.3 g of water and 214.0 g of methanol.
  • Example 3 Same as Example 1 except that the mixed solution of Example 1 was changed to a mixed solution of nickel acetate tetrahydrate (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.) 2.46 g, water 57.1 g and methanol 171.3 g. A dispersion was obtained.
  • nickel acetate tetrahydrate manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.
  • Example 4 Same as Example 1 except that the mixed solution of Example 1 was changed to a mixed solution of magnesium acetate tetrahydrate (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.) 0.85 g, water 57.1 g and methanol 171.3 g. A dispersion was obtained.
  • Example 5 When the barium hydroxide / octahydrate of Example 1 was dissolved in 2-methoxyethanol, 1.79 g of tin methoxydo (manufactured by Alfa Aesar) was added. Other than that, a dispersion was prepared in the same manner as in Example 1.
  • Example 6 When the barium hydroxide / octahydrate of Example 1 was dissolved in 2-methoxyethanol, 2.02 g of calcium methoxydo (manufactured by Strem Chemicals) was added. A dispersion was obtained in the same manner as in Example 1 except that 178 g of this solution was used.
  • Example 7 When the barium hydroxide / octahydrate of Example 1 was dissolved in 2-methoxyethanol, 0.67 g of tantalum methoxydo (manufactured by Strem Chemicals) was added. Other than that, a dispersion liquid was obtained in the same manner as in Example 1.
  • Example 8 Same as Example 1 except that the mixed solution of Example 1 was changed to a mixed solution of nickel hydroxide / hydrate (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.) 0.92 g, water 57.1 g and methanol 171.2 g. A dispersion was obtained.
  • nickel hydroxide / hydrate manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.
  • Example 9 When the barium hydroxide / octahydrate of Example 1 was dissolved in 2-methoxyethanol, 0.67 g of dysprosium isopropoxide (manufactured by Fuji Film Wako Chemical Co., Ltd.) was added. Other than that, a dispersion liquid was obtained in the same manner as in Example 1.
  • Example 10 A solution for hydrolysis, which was a mixture of 57.1 g of water and 171.3 g of methanol, was added to the mixed solution B obtained in Example 1 over 1 minute while keeping the temperature at 25 ° C. under stirring. As a result, a hydrate gel was obtained. The hydrate gel was heated to 80 ° C. and aged for 96 hours. Ethanol was mixed with this aged product and ultrafiltration was performed to obtain a dispersion liquid containing 40% by mass of barium titanate.
  • Example 11 A mixed solution B was prepared in the same manner as in Example 1 except that the weight of the mixed solution A was changed to 178 g.
  • a dispersion was obtained in the same manner as in Example 1 except that 70 g of butyl carbitol (manufactured by Kanto Chemical Co., Inc.) was mixed with the aged product and solvent substitution was performed using a rotary evaporator instead of limit filtration.
  • the solvent replacement conditions were a temperature of 70 ° C. and a reduced pressure of 0.015 MPa for 1 hour.
  • Example 12 A dispersion was obtained in the same manner as in Example 11 except that the weight of the mixed solution A was changed to 170 g.
  • Example 13 The same as in Example 12 except that the hydrolysis solution was changed to a solution of nickel acetate tetrahydrate (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.) 2.46 g, water 57.1 g and methanol 171.3 g. A dispersion was obtained.
  • Example 14 The weight of the mixed solution A was changed to 168 g, and the mixture was dispersed in the same manner as in Example 12 except that 70 g of tarpineol and 3.5 g of linoleic acid (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.) were mixed with the aged product instead of butyl carbitol. I got the liquid.
  • Example 15 To the aged product obtained in Example 11, 3.5 g of linoleic acid was added, and the mixture was stirred at 50 ° C. for 15 hours. 70 g of butyl carbitol was added thereto and distilled with a rotary evaporator to obtain a dispersion liquid. The distillation conditions were a temperature of 70 ° C. and a reduced pressure of 0.015 MPa for 1 hour.
  • Example 16 70 g of tarpineol was added to the aged product obtained in Example 10. Distillation was carried out using a rotary evaporator under the conditions of a temperature of 70 ° C. and a reduced pressure of 0.015 MPa for 1 hour.
  • Example 17 70 g of triethanolamine was added to the aged product obtained in Example 10. Distillation was carried out using a rotary evaporator under the conditions of a temperature of 70 ° C. and a reduced pressure of 0.015 MPa for 1 hour.

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Abstract

L'invention fournit des particules de titanate de baryum présentant un effet de retard de frittage élevé, et un procédé de fabrication de celles-ci.　Plus précisément, l'invention concerne des particules de titanate de baryum de structure pérovskite, qui présentent un rapport (Ｂａ／Ｔｉ) de Ba et Ti compris entre ０,９５ et １,０５, et un diamètre de particules cristallines compris entre ５ et ２５ｎｍ.
PCT/JP2020/037304 2019-09-30 2020-09-30 Particules de titanate de baryum ainsi que procédé de fabrication de celles-ci, et dispersion liquide de particules de titanate de baryum WO2021066070A1 (fr)

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JP2021551421A JPWO2021066070A1 (fr) 2019-09-30 2020-09-30
KR1020217037796A KR20220074821A (ko) 2019-09-30 2020-09-30 티타늄산바륨 입자와 그의 제조 방법, 티타늄산바륨 입자의 분산액
CN202080042148.5A CN113939476B (zh) 2019-09-30 2020-09-30 钛酸钡粒子、其制造方法及钛酸钡粒子的分散液

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Citations (3)

* Cited by examiner, † Cited by third party
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