WO2020110183A1 - Matériau particulaire de titanate de baryum à surface modifiée, composition de résine contenant du titanate de baryum et dispersion de titanate de baryum - Google Patents

Matériau particulaire de titanate de baryum à surface modifiée, composition de résine contenant du titanate de baryum et dispersion de titanate de baryum Download PDF

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WO2020110183A1
WO2020110183A1 PCT/JP2018/043461 JP2018043461W WO2020110183A1 WO 2020110183 A1 WO2020110183 A1 WO 2020110183A1 JP 2018043461 W JP2018043461 W JP 2018043461W WO 2020110183 A1 WO2020110183 A1 WO 2020110183A1
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barium titanate
particle material
test example
group
mass
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PCT/JP2018/043461
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English (en)
Japanese (ja)
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雄己 新井
冨田　亘孝
桂輔 栗田
優里 青木
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株式会社アドマテックス
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Priority to JP2019520170A priority Critical patent/JP6564551B1/ja
Priority to PCT/JP2018/043461 priority patent/WO2020110183A1/fr
Publication of WO2020110183A1 publication Critical patent/WO2020110183A1/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

Definitions

  • the present invention relates to a surface-modified barium titanate particle material, a barium titanate-containing resin composition, and a barium titanate dispersion liquid in which a particle material containing barium titanate is dispersed.
  • Barium titanate is used as a thin film dielectric material for thin film capacitors because it has a high dielectric constant.
  • a method of forming a dielectric layer when manufacturing a thin film capacitor there is a method of using a dispersion liquid in which a particle material made of barium titanate is dispersed in a dispersion medium, or a resin composition dispersed in a resin material.
  • the barium titanate used is also required to have a small particle size, and the barium titanate dispersion liquid in which the powder is dispersed and the resin composition are also required to have high homogeneity.
  • the present invention has been completed in view of the above circumstances, surface-modified barium titanate particle material having high dispersibility in a dispersion medium or resin, and barium titanate-containing dispersion of the surface-modified barium titanate particle material. It is an object to be solved to provide a resin composition and a barium titanate dispersion liquid.
  • the surface-modified barium titanate particle material of the present invention which solves the above-mentioned problems, is a particle material whose main component is barium titanate, and an amount of 0.05 or more and less than 6.0 ⁇ mol/m 2 based on the surface area.
  • a silane compound having a surface treatment layer reacted on the surface of the particle material, FT-IR IR spectrum measured by diffuse reflection method has a peak at 1500-1600 cm -1 ,
  • the average particle diameter (D50) by dynamic light scattering when dispersed in ethanol at a concentration of 0.1% by mass is 10 nm to 1000 nm.
  • the surface-modified barium titanate particle material of the present invention which solves the above-mentioned problems, comprises a particle material whose main component is barium titanate and a compound represented by the general formula (1): X—(CH 2 ) n —Si(OR 3 (in the general formula (1), X is a vinyl group, a phenyl group, a methacryloxy group, an N-phenylamino group, a glycidyloxy group or an amino group, and R is a hydrocarbon group having 1 to 3 carbon atoms, n Has a surface treatment layer reacted with the surface of the particulate material with a silane compound represented by FT-IR IR spectrum measured by diffuse reflection method has a peak at 1500-1600 cm -1 , The average particle diameter (D50) by dynamic light scattering when dispersed in ethanol at a concentration of 0.1% by mass is 10 nm to 1000 nm.
  • D50 average particle diameter
  • the above-mentioned surface-modified barium titanate particle material (1) or (2) has excellent dispersibility in a dispersion medium or a resin material.
  • the surface-modified barium titanate particle material of (1) or (2) described above preferably has a zeta potential of +40 mV to +150 mV when dispersed in ethanol at a concentration of 0.1% by mass. Further, it is preferable that the surface has —SiMe 3 groups and that the surface has substantially no OH groups.
  • a barium titanate-containing resin composition of the present invention which solves the above-mentioned problems comprises the surface-modified barium titanate particle material of (1) or (2) above and the surface-modified barium titanate particle material. And a resin material to be dispersed.
  • the barium titanate dispersion liquid of the present invention for solving the above-mentioned problems disperses the surface-modified barium titanate particle material of (1) or (2) above and the surface-modified barium titanate particle material. And a dispersion medium.
  • the surface-modified barium titanate particle material of the present invention has high dispersibility in the dispersion medium or the resin material because of having the above-mentioned constitution.
  • the surface-modified barium titanate particle material of the present embodiment is not particularly limited, but it can be used for applications utilizing the high relative dielectric constant of barium titanate. Applications that utilize high relative permittivity include materials for capacitors. When barium titanate is superior to resin materials in physical properties (high strength, low coefficient of thermal expansion) and high chemical stability, it can be used as a simple filler. Can also be adopted. When the surface-modified barium titanate particle material of the present embodiment is used, other particle materials (silica, alumina, titania, zirconia, etc.) can be mixed and used.
  • the surface-modified barium titanate particle material of the present embodiment has a particle material whose main component is barium titanate, and a surface treatment layer formed by reacting the surface of the particle material with a silane compound.
  • the IR spectrum measured by the FT-IR diffuse reflection method has a peak at 1500 to 1600 cm -1 .
  • the FT-IR diffuse reflection method is herein referred to as being measured by the powder diffuse reflection method.
  • the measurement conditions were a resolution of 4 cm ⁇ 1 and a scan count of 64.
  • the surface-modified barium titanate particle material of the present embodiment has an average particle diameter (hereinafter referred to as “D50”) of 10 nm or more by dynamic light scattering when dispersed in ethanol at a concentration of 0.1% by mass. It is 1000 nm.
  • the lower limit of D50 is preferably 20 nm, 30 nm, and 50 nm.
  • the upper limit of D50 is preferably 500 nm, 300 nm, and 250 nm.
  • the main component of the particle material is barium titanate. Whether or not it is the main component is judged by whether or not the content is 50% by mass or more. In particular, 60% or more, 75% or more, 90% or more, 95% or more, 99% or more, 100% (barium titanate other than inevitable impurities) can be used.
  • Barium titanate which is a raw material of the particle material, can be produced by a general method such as a solid phase method, a hydrothermal method, an alkoxide method, an oxalate method, and a sol-gel method. Then, if necessary, the particle size distribution can be adjusted by a crushing operation. The particle size of the particulate material is determined according to the particle size of the final surface modified barium titanate particulate material.
  • the surface treatment layer is chemically bonded to the surface of the particle material.
  • the surface treatment layer is formed by reacting the silane compound with the reactive groups present on the surface of the above-mentioned particle material.
  • the method of reacting the silane compound on the surface of the particle material is not particularly limited. For example, it can be carried out by contacting the surface of the particle material with a silane compound or by contacting a silane compound solution in which the silane compound is dissolved in an appropriate solvent.
  • When contacting the silane compound or the silane compound solution directly add to the particle material, atomize a liquid material and add it, or add it in a state of being heated and vaporized, and then stir and mix. be able to. Stirring and mixing can be performed with a stirrer or a crusher.
  • the silane compound can be promptly reacted with the new surface of the particulate material generated by the pulverization.
  • the stirring/mixing may be performed at room temperature or while heating.
  • the surface treatment layer has at least one of the following features (1) and (2).
  • the surface-modified barium titanate particle material of the present embodiment has a surface-treated layer formed by the reaction of the silane compound on the surface, and “Ti—O existing on the surface of the original particle material.
  • the “structure” and the “Ba—O” structure can properly interact with the dispersion medium and the resin material, respectively, and high dispersibility can be realized.
  • the type of silane compound is not particularly limited. Examples thereof include hexamethyldisilazane (HMDS), epoxysilane, vinylsilane, phenylsilane, methacrylsilane, phenylaminosilane, and alkenylsilane (having about 2 to 8 carbon atoms).
  • HMDS hexamethyldisilazane
  • the lower limit of the reaction of the silane compound 0.05 ⁇ mol / m 2, 0.2 ⁇ mol / m 2, can be employed is 0.5 [mu] mol / m 2, the upper limit value, 4.0 ⁇ mol / m 2, 5.0 ⁇ mol / m 2 can be adopted.
  • the upper limit value and the lower limit value can be arbitrarily combined.
  • the zeta potential in ethanol is +40 mV to +150 mV because the dispersibility becomes high.
  • the zeta potential can be controlled by changing the type of silane compound and the amount of reaction.
  • —SiMe 3 groups on the surface and substantially no OH groups on the surface. Specifically, it can be realized by surface-treating a particle material (including one treated with another silane compound) with a compound having a —SiMe 3 group as a silane compound forming a surface treatment layer.
  • the barium titanate-containing resin composition of this embodiment has the above-described surface-modified barium titanate particle material of this embodiment and a resin material in which the surface-modified barium titanate particle material is dispersed.
  • the resin material is not particularly limited. Examples thereof include epoxy resin, polyphenylene sulfide, polyethylene terephthalate, polyvinylidene fluoride, and acrylic resin.
  • the mixing ratio of the surface-modified barium titanate particle material and the resin material is not particularly limited, but it is preferable that the surface-modified barium titanate particle material is as large as possible, and the surface-modified barium titanate particles based on the total mass.
  • the content of the material may be about 2% to 60%.
  • the barium titanate dispersion liquid of the present embodiment has the surface-modified barium titanate particle material of the present embodiment described above and a dispersion medium in which the surface-modified barium titanate particle material is dispersed. Then, the resin material described in the section of the barium titanate-containing resin composition described above can be dissolved in the dispersion medium or can be made into fine particles and dispersed. When dispersed, a dispersant such as a surfactant can be contained.
  • the dispersion medium is not particularly limited. Examples thereof include ethanol, toluene, isopropanol, ethyl methyl ketone, methyl isobutyl ketone, cyclohexanone, dimethylformamide, propylene glycol monomethyl ether, and mixed solvents thereof.
  • the mixing ratio of the surface-modified barium titanate particle material and the dispersion medium is not particularly limited, but it is preferable that the surface-modified barium titanate particle material is as large as possible, and the surface-modified barium titanate particle material is based on the total mass.
  • the content of 2% to 60% can be exemplified.
  • the surface-modified barium titanate particle material, barium titanate-containing resin composition, and barium titanate dispersion liquid of the present invention will be described in detail based on examples.
  • Test 1 Examination of surface treatment of barium titanate particle material: Table 1
  • ⁇ Test example 1 10 parts by mass of barium titanate (specific surface area 16 m 2 /g), 90 parts by mass of ethanol, 0.03 parts by mass of HMDS (1 ⁇ mol/m 2 : surface area standard of barium titanate, the same applies hereinafter), 0.3 mm zirconia
  • the beads were mixed and dispersed for 60 minutes at a rotation speed of 3000 rpm with a bead mill. Thereafter, the zirconia beads were removed, and a barium titanate dispersion liquid of this test example was obtained in which the surface-modified barium titanate particle material was dispersed in ethanol as a dispersion medium.
  • the average particle diameter (D50) by dynamic light scattering was 125 nm, and the zeta potential was 82 mV.
  • the measurement result of the particle size distribution is shown in FIG.
  • the barium titanate dispersion liquid of this test example did not cause coagulation sedimentation even when left standing for 1 week. Whether or not coagulation sedimentation occurred, when the slurry concentration was allowed to stand for 24 hours in a glass container having a liquid surface height of 10 cm, 10 mm or more from the liquid surface was transparent and a sedimentation layer of 1 mm or more from the bottom surface of the container was formed. When it did, it was judged that cohesive sedimentation had occurred.
  • the barium titanate dispersion liquid of this test example was subjected to centrifugal sedimentation, the obtained precipitate was washed with methyl ethyl ketone (MEK), and then dried at 120° C. to obtain a sample after washing. It can be inferred that the HMDS physically adsorbed on the surface of the surface-modified barium titanate particle material in the barium titanate dispersion can be washed by this washing and drying.
  • MEK methyl ethyl ketone
  • Test Example 2 All the HMDS of Test Example 1 were replaced by 0.09 parts by mass of 2-glycidyloxypropyltrimethoxysilane (KBM403) (2 ⁇ mol/m 2 ) and prepared in the same manner as the test sample of this Test Example. did. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • HMDS HMDS 0.03 parts by mass (1 ⁇ mol/m 2 ).
  • a test sample of this test example was prepared by the same procedure except for the above. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • ⁇ Test Example 5 Combined use of all two types of HMDS of Test Example 1, 0.09 parts by mass (2 ⁇ mol/m 2 ) of N-phenylaminopropyltrimethoxysilane (KBM573) and 0.03 parts by mass of HMDS (1 ⁇ mol/m 2 ).
  • a test sample of this test example was prepared by the same procedure except that the treatment was changed. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • HMDS ⁇ Test Example 7 All of the HMDS of Test Example 1 was replaced with a combined treatment using two types of octenyltrimethoxysilane (KBM1083) 0.08 parts by mass (2 ⁇ mol/m 2 ) and HMDS 0.03 parts by mass (1 ⁇ mol/m 2 ).
  • KBM1083 octenyltrimethoxysilane
  • HMDS HMDS 0.03 parts by mass (1 ⁇ mol/m 2 ).
  • a test sample of this test example was prepared by the same procedure except for the above. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • Test Example 9 A test sample of this test example was prepared by the same operation except that 90 parts by mass of ethanol in Test Example 1 was replaced with 45 parts by mass of ethanol and 45 parts by mass of toluene. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • Test Example 10 A test sample of this test example was prepared by the same operation except that 90 parts by mass of ethanol in Test Example 5 was replaced with 45 parts by mass of ethanol and 45 parts by mass of MEK. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • Test Example 11 A test sample of this test example was prepared by the same operation except that 90 parts by mass of ethanol in Test Example 1 was replaced with 45 parts by mass of ethanol and 45 parts by mass of MEK. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • ⁇ Test Example 12 10 parts by mass of barium titanate (specific surface area: 16 m 2 /g) and 0.03 parts by mass of hexamethyldisilazane (1 ⁇ mol/m 2 ) were mixed for surface modification. Then, 90 parts by mass of ethanol was mixed with 0.3 mm zirconia beads, and the mixture was dispersed by a bead mill at a rotation speed of 3000 rpm for 60 minutes. Thereafter, the zirconia beads were removed, and a barium titanate dispersion liquid of this test example was obtained in which the surface-modified barium titanate particle material was dispersed in ethanol as a dispersion medium. The same evaluation as in Test Example 1 was performed on the test sample of this test example. Similar to the test sample of Test Example 1, no cohesive sedimentation was observed even after standing for 1 week. The results are shown in Table 2.
  • Test Example 2 All the HMDS of Test Example 1 were replaced by 0.34 parts by mass (6 ⁇ mol/m 2 ) of 8-methacryloxyoctyltrimethoxysilane (KBM5803) to prepare a test sample of the same test example. The same evaluation as in Test Example 1 was performed on the test sample of this test example. After standing for 1 day, aggregation and sedimentation was observed. The results are shown in Table 2.
  • test sample of this test example was prepared by the same procedure except that 0.27 parts by mass (6 ⁇ mol/m 2 ) of 8-octenyltrimethoxysilane (KBM1083) was used for all of the HMDS of Test Example 1.
  • KBM1083 8-octenyltrimethoxysilane
  • the same evaluation as in Test Example 1 was performed on the test sample of this test example. After standing for 1 day, aggregation and sedimentation was observed. The results are shown in Table 2.
  • the barium titanate dispersions of the test samples of Test Examples 1 to 13 did not show the occurrence of aggregation and sedimentation, whereas the barium titanate dispersions of the test samples of Comparative Examples 1 to 3 did. Occurrence of aggregation and sedimentation was observed. It can be inferred that agglomeration occurred because the addition amount of the silane compound was excessive. It has been found that the treatment amount of the silane compound is preferably smaller than 6 ⁇ mol/m 2 .
  • Test Example 3 D50 was slightly higher than that in the other test examples, and the zeta potential was 38 mV, which was lower than that in the other test examples. Therefore, the preferable range of the zeta potential was 40 mV which was higher than that in Test example 3. It turned out that it was above.

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Abstract

L'invention concerne un matériau particulaire de titanate de baryum à surface modifiée qui présente une dispersibilité élevée dans des milieux de dispersion et une résine.　Ce matériau particulaire de titanate de baryum à surface modifiée qui résout le problème ci-dessus comprend (1) un matériau particulaire composé principalement de titanate de baryum, et une couche traitée en surface qui est un composé de silane ayant réagi avec la surface du matériau particulaire en une quantité de 0,05 à 6,0 μmol/m2 sur la base de la surface, ou (2) un matériau particulaire composé principalement de titanate de baryum, et une couche traitée en surface qui est un composé de silane ayant réagi avec la surface du matériau particulaire, le composé de silane représenté par X-(CH2)n-Si(OR)3 (dans la formule générale (1), X est un groupe vinyle, un groupe phényle, un groupe méthacryloxy, un groupe N-phénylamino, un groupe glycidyloxy, ou un groupe amino, R est un groupe hydrocarboné ayant 1 à 3 atomes de carbone, et n est de 4 à 10). Le spectre IR Mesuré par le procédé de réflectance diffuse FTIR a un pic de 1500 à 1600 cm-1, et la taille moyenne de particule (D50) en fonction de la diffusion dynamique de la lumière lorsqu'elle est dispersée dans de l'éthanol à une concentration de 0,1 % en masse est de 10 à 300 nm.
PCT/JP2018/043461 2018-11-27 2018-11-27 Matériau particulaire de titanate de baryum à surface modifiée, composition de résine contenant du titanate de baryum et dispersion de titanate de baryum WO2020110183A1 (fr)

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PCT/JP2018/043461 WO2020110183A1 (fr) 2018-11-27 2018-11-27 Matériau particulaire de titanate de baryum à surface modifiée, composition de résine contenant du titanate de baryum et dispersion de titanate de baryum

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CN114878032A (zh) * 2022-04-02 2022-08-09 华南理工大学 一种柔性自供电压力传感器及其制备方法与应用
WO2024009948A1 (fr) * 2022-07-07 2024-01-11 テイカ株式会社 Poudre de titanate de métal alcalino-terreux de type mtio3 et composition de résine l'utilisant

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114878032A (zh) * 2022-04-02 2022-08-09 华南理工大学 一种柔性自供电压力传感器及其制备方法与应用
WO2024009948A1 (fr) * 2022-07-07 2024-01-11 テイカ株式会社 Poudre de titanate de métal alcalino-terreux de type mtio3 et composition de résine l'utilisant

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