Material for high-frequency electronic part
A composite oxide of barium and titanium, produced via a hydrothermal reaction and calcination, addresses the limitations of conventional fillers by enhancing dielectric constant and reducing loss tangent, suitable for high-frequency electronic components.
Patent Information
- Application Number
- JP2024093730
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2024-06-10
- Publication Date
- 2025-12-22
AI Technical Summary
Conventional inorganic fillers for high-frequency electronic components are insufficient in terms of dielectric constant and dielectric loss tangent, failing to meet the requirements for high-frequency transmission properties and device miniaturization.
A composite oxide of barium and titanium with specific diffraction peaks in an XRD pattern is mixed with a resin, suppressing dielectric loss tangent while increasing the dielectric constant, achieved through a hydrothermal reaction and calcination process with an alkali metal halide.
The material effectively suppresses dielectric loss tangent and enhances dielectric constant, making it suitable for high-frequency devices by reducing transmission loss and enabling device miniaturization.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to a material for high frequency electronic components, and more particularly to a material for high frequency electronic components useful as an inorganic filler in high frequency devices and the like. [Background technology]
[0002] In recent years, the spread of AI / IoT has progressed in global markets, including Japan, with the spread of communication devices such as smartphones and tablets, IoT home appliances and manufacturing equipment, contactless IC cards, RFID automatic recognition technology, and the upcoming practical application of self-driving cars, resulting in an increase in the transmission of high-frequency signals (1 MHz and above). Because transmission loss in the high-frequency range is greater than that of conventional wavelengths, it is necessary for the materials used to have excellent high-frequency transmission properties (low dielectric loss). Dielectric loss is proportional to the product of frequency, the dielectric constant (ε or Dk) and the dielectric loss tangent (tanδ or Df) of the material, so to reduce dielectric loss, the dielectric loss tangent of the material must be small. On the other hand, the size of a dielectric device is proportional to the wavelength of the electromagnetic waves it targets, and the higher the dielectric constant, the shorter the wavelength becomes. Therefore, there is also a need for devices with a high dielectric constant from the perspective of making devices lighter and thinner.
[0003] Regarding a technique for increasing the dielectric constant while suppressing the dielectric loss tangent, Patent Document 1 discloses a resin composition comprising (A) a thermosetting resin, (B) a titanium-based inorganic filler, and (C) a siloxane compound having a reactive group. Patent Document 2 discloses a thermosetting resin composition comprising (A) an epoxy resin, (B) a curing agent, and (C) a high-dielectric-constant filler, wherein the epoxy resin (A) comprises at least one selected from the group consisting of bisphenol A-type epoxy resins, bisphenol F-type epoxy resins, naphthalene-type epoxy resins, dicyclopentadiene-type epoxy resins, glycidylamine-type epoxy resins, and naphthol aralkyl-type epoxy resins, the curing agent (B) comprises an active ester-based curing agent (B1) and / or a phenol-based curing agent (B2), and the high-dielectric-constant filler (C) comprises at least one selected from calcium titanate, strontium titanate, magnesium titanate, magnesium zirconate, strontium zirconate, bismuth titanate, zirconium titanate, zinc titanate, barium zirconate, calcium titanate zirconate, lead titanate zirconate, barium magnesium niobate, and calcium zirconate. [Prior art documents] [Patent documents]
[0004] [Patent Document 1] Japanese Patent Application Publication No. 2023-13230 [Patent Document 2] Japanese Patent Application Publication No. 2023-179419 Summary of the Invention [Problem to be solved by the invention]
[0005] As described above, various inorganic fillers have been developed to increase the dielectric constant while suppressing the dielectric loss tangent. However, the conventional inorganic fillers have been insufficient in terms of the dielectric constant.
[0006] The present invention has been made in view of the above-mentioned circumstances, and has an object to provide a material for high-frequency electronic components that can suppress the dielectric loss tangent while increasing the dielectric constant compared to conventional materials. [Means for solving the problem]
[0007] The inventors of the present invention have conducted extensive research into materials that can be used for high-frequency electronic components, and have found that when a composite oxide of barium and titanium, which has a specific diffraction peak in an XRD pattern, is mixed with a resin, the dielectric loss tangent can be suppressed while the dielectric constant can be increased compared to conventional materials. This led to the realization that the above-mentioned problems can be solved beautifully, and has led to the present invention.
[0008] The present invention includes the following materials for high-frequency electronic components. [1] A material for high-frequency electronic components, comprising a composite oxide of barium and titanium, the composite oxide having diffraction peaks at 2θ=30.7±0.3° and 2θ=38.6±0.2° in an XRD pattern when analyzed by powder X-ray diffraction. [2] The material for high-frequency electronic components according to the above [1], wherein the composite oxide has a molar ratio of barium element to titanium element (Ba / Ti) of 0.34 to 0.40. [3] A composite oxide of barium and titanium, The composite oxide has diffraction peaks at 2θ=30.7±0.3° and 2θ=38.6±0.2° in the XRD pattern when analyzed by powder X-ray diffraction, and has a specific surface area of 0.1 to 2.0 m 2 / g of a composite oxide of barium and titanium. [4] The composite oxide of barium and titanium according to the above [3], wherein the composite oxide has a molar ratio of barium element to titanium element (Ba / Ti) of 0.34 to 0.40. [5] A resin composition comprising the composite oxide according to [3] or [4] above and a resin. [6] A method for producing a composite oxide of barium and titanium, comprising: The production method includes a step of hydrothermally reacting a titanium compound with a barium compound; and a step of mixing the product obtained in the hydrothermal reaction step with an alkali metal halide and calcining the mixture. [7] The method for producing a composite oxide of barium and titanium according to [6] above, wherein the titanium compound is titanium oxide and / or titanium hydroxide. [8] The method for producing a composite oxide of barium and titanium according to [6] or [7] above, wherein the barium compound is barium hydroxide and / or barium oxide. [9] The method for producing a composite oxide of barium and titanium according to any one of the above [6] to [8], wherein the alkali metal halide is sodium chloride.
[10] The method for producing a barium and titanium composite oxide according to any one of [6] to [9] above, wherein the ratio of the titanium compound to the barium compound used in the hydrothermal reaction step is 0.34 to 0.40 in terms of the molar ratio of barium element to titanium element (Ba / Ti).
[11] The method for producing a composite oxide of barium and titanium according to any one of the above [6] to
[10] , wherein the reaction temperature in the hydrothermal reaction step is 80 to 250°C. [Effects of the Invention]
[0009] The material for high-frequency electronic components of the present invention has the above-mentioned configuration, and when mixed with a resin, can suppress the dielectric loss tangent while increasing the dielectric constant compared to conventional materials, and therefore can be suitably used as an inorganic filler in high-frequency devices, etc. [Brief explanation of the drawings]
[0010] [Figure 1] 1 is an SEM image of the material for high-frequency electronic components obtained in Example 1. [Figure 2] FIG. 1 is a diagram showing an XRD pattern of the material for high-frequency electronic components obtained in Example 1. [Figure 3] FIG. 2 is a diagram showing a peak observed at a diffraction angle (2θ) of 30.7±0.3° in the XRD pattern of the material for high-frequency electronic components obtained in Example 1. [Figure 4] FIG. 2 is a diagram showing a peak observed at a diffraction angle (2θ) of 38.6±0.2° in the XRD pattern of the material for high-frequency electronic components obtained in Example 1. [Figure 5]1 is an SEM image of the material for high-frequency electronic components obtained in Example 2. [Figure 6] FIG. 2 is a diagram showing an XRD pattern of the material for high-frequency electronic components obtained in Example 2. [Figure 7] FIG. 2 is a diagram showing a peak observed at a diffraction angle (2θ) of 30.7±0.3° in the XRD pattern of the material for high-frequency electronic components obtained in Example 2. [Figure 8] FIG. 2 is a diagram showing a peak observed at a diffraction angle (2θ) of 38.6±0.2° in the XRD pattern of the material for high-frequency electronic components obtained in Example 2. DETAILED DESCRIPTION OF THE INVENTION
[0011] Preferred embodiments of the present invention will be specifically described below, but the present invention is not limited to the following description and can be appropriately modified and applied within the scope of the present invention. Note that combinations of two or more of the individual preferred embodiments of the present invention described below also fall within the scope of preferred embodiments of the present invention.
[0012] 1. Materials for high-frequency electronic components The material for high-frequency electronic components of the present invention contains a composite oxide of barium and titanium, which has diffraction peaks at 2θ=30.7±0.3° and 2θ=38.6±0.2° in an XRD pattern when analyzed by powder X-ray diffraction. The composite oxide of barium and titanium contained in the material for high-frequency electronic components of the present invention has a crystalline structure with a diffraction peak at such a predetermined position in the XRD pattern, thereby achieving excellent dielectric properties, namely, a low dielectric loss tangent and a high dielectric constant. The composite oxide of barium and titanium contained in the material for high-frequency electronic components is hereinafter also referred to as composite oxide (α).
[0013] The composite oxide (α) may have any of the above-mentioned predetermined diffraction peaks in the XRD pattern, but preferably has a molar ratio of barium to titanium (Ba / Ti) of 0.34 to 0.40, which allows the composite oxide (α) to exhibit better dielectric properties.
[0014] The composite oxide (α) is not particularly limited as long as it has the above-mentioned predetermined diffraction peaks in the XRD pattern, but may be selected from the group consisting of compounds represented by the following formula (1); Ba x Ti y O z (1) In this case, the configuration where x=11, y=28, and z=66.5 is one of the preferred embodiments of the present invention.
[0015] The shape of the composite oxide (α) is not particularly limited, but it is preferably plate-like. When the composite oxide (α) is plate-shaped, the plate diameter is preferably 0.1 to 100 μm, more preferably 0.2 to 50 μm, even more preferably 0.5 to 20 μm, and particularly preferably 1 to 5 μm. The plate surface diameter can be measured by the method described in the Examples.
[0016] The specific surface area of the composite oxide (α) is not particularly limited, but is preferably within the same range as the preferred range of the specific surface area of the composite oxide (β) described below.
[0017] The composite oxide (α) preferably has a dielectric loss tangent (tan δ) at 1 GHz of 0.01 or less, more preferably 0.005 or less, and even more preferably 0.001 or less. The dielectric loss tangent at 1 GHz can be measured by the method described in the examples.
[0018] The composite oxide (α) preferably has a dielectric constant of 13 or more at 1 GHz. The dielectric constant at 1 GHz can be measured by the method described in the Examples.
[0019] The material for high-frequency electronic components may contain the composite oxide (α), and the content of the composite oxide (α) is preferably 80 to 100 mass %, more preferably 90 to 100 mass %, and most preferably 100 mass %, relative to 100 mass % of the material for high-frequency electronic components.
[0020] The material for high-frequency electronic components may contain other components in addition to the composite oxide (α). Examples of the other components include alkali metal elements such as Li, Na, K, Rb, and Cs, and compounds containing oxygen atoms thereof; alkali metal halides; and elements other than alkali metals such as Al, Si, Ca, Zr, Nb, and Sn, and compounds containing oxygen atoms thereof. The content of the other components is preferably 1% by mass or less, more preferably 0.07% by mass or less, and even more preferably 0.05% by mass or less, relative to 100% by mass of the composite oxide (α).
[0021] 2. Barium and titanium composite oxide The present invention relates to a powder of 1000 kJ / cm2 or 1000 kJ / cm2, which has diffraction peaks at 2θ=30.7±0.3° and 2θ=38.6±0.2° in an XRD pattern when analyzed by powder X-ray diffraction, and has a specific surface area of 0.1 to 2.0 m 2 / g (hereinafter also referred to as composite oxide (β)).
[0022] The composite oxide (β) has a specific surface area of 0.1 to 2.0 m 2 This makes it possible to sufficiently suppress thickening when the composite oxide (β) is mixed with a resin. The specific surface area is preferably 0.2 to 1.5 m 2 / g, and more preferably 0.2 to 1.0 m 2 / g. The specific surface area can be measured by the method described in the Examples.
[0023] The composite oxide (β) has a specific surface area of 0.1 to 2.0 m 2 / g, but other than this, the composite oxide (β) is common to the composite oxide (α). Furthermore, the material for high-frequency electronic components of the present invention may contain the composite oxide (β). Hereinafter, when the term "composite oxide" is simply used, it means the matters common to the composite oxide (α) and the composite oxide (β).
[0024] The composite oxide (β) preferably has a viscosity of 0.1 to 5.0 Pa·s at 20° C. when mixed with a resin under the following conditions: The viscosity is more preferably 0.1 to 2.0 Pa·s, and even more preferably 0.1 to 0.5 Pa·s. <Mixing conditions with resin> Resin type: Epoxy resin (Daicel Celloxide 2021P) Ratio of complex oxide (β): 15% by volume relative to 100% by volume of resin
[0025] 3. Method for manufacturing materials for high-frequency electronic components or composite oxides of barium and titanium The method for producing the material for high-frequency electronic components of the present invention is not particularly limited, but it is preferable to produce it by carrying out a step of hydrothermally reacting a titanium compound with a barium compound, and a step of mixing the product obtained in the hydrothermal reaction step with an alkali metal halide and firing the mixture. In the above manufacturing method, the hydrothermal reaction process partially converts the raw material titanium compound into barium titanate, which is then mixed with an alkali metal halide and fired, thereby sufficiently preventing the presence of fine powder of the complex oxide in the material for high-frequency electronic components, and making it possible to obtain a material for high-frequency electronic components that has a low dielectric tangent and a higher dielectric constant than conventional materials. The present invention also provides a method for producing a composite oxide of barium and titanium, which comprises the steps of hydrothermally reacting a titanium compound with a barium compound, and mixing the product obtained in the hydrothermal reaction with an alkali metal halide and firing the mixture.
[0026] The titanium compound used in the hydrothermal reaction step is not particularly limited as long as it contains titanium element, and examples thereof include sulfates, hydrochlorides, oxides, hydroxides, organic acid salts, etc. One or more of these may be used. Among these, titanium oxide, titanium sulfate, and titanium hydroxide are preferred, titanium oxide and titanium hydroxide are more preferred, and titanium oxide is particularly preferred.
[0027] The barium compound used in the hydrothermal reaction step is not particularly limited as long as it contains barium element, and examples thereof include nitrates, hydrochlorides, oxides, hydroxides, carbonates, fatty acid salts, organic acid salts, etc. One or more of these can be used. Among these, compounds such as barium hydroxide and barium oxide, whose aqueous solutions are basic, are preferred, with barium hydroxide being more preferred.
[0028] The ratio of the titanium compound to the barium compound used in the hydrothermal reaction step is not particularly limited, but the molar ratio of barium element to titanium element (Ba / Ti) is preferably 0.34 to 0.40.
[0029] The reaction temperature in the hydrothermal reaction step is not particularly limited, but is preferably 80 to 250°C, more preferably 100 to 200°C, and even more preferably 120 to 180°C.
[0030] The reaction time in the hydrothermal reaction step is not particularly limited, but is preferably 0.5 to 72 hours, more preferably 1 to 48 hours, and even more preferably 3 to 24 hours.
[0031] In the hydrothermal reaction step, a mixed slurry containing water, a titanium compound, and a barium compound is preferably heated.
[0032] The method for producing the composite oxide may include a step of purifying the product obtained after the hydrothermal reaction step by filtering, washing with water, or the like, and a step of drying the product.
[0033] The calcination step may be any step in which the product obtained in the hydrothermal reaction step is mixed with an alkali metal halide and calcined. However, if a purification step or a drying step is performed after the hydrothermal reaction step, it is preferable to mix the product after these steps with an alkali metal halide and calcinate the mixture.
[0034] The alkali metal halide used in the calcination step is not particularly limited, but is preferably a chloride such as sodium chloride or potassium chloride, more preferably sodium chloride.
[0035] The proportion of the alkali metal halide used in the calcination step is not particularly limited, but is preferably 50 to 500 mass% relative to 100 mass% of the product obtained in the hydrothermal reaction step. This allows the particle size of the resulting composite oxide to fall within a suitable range. The proportion of the alkali metal halide is more preferably 100 to 300 mass%, and even more preferably 150 to 250 mass%.
[0036] The firing temperature in the firing step is not particularly limited, but is preferably 800 to 1400°C, more preferably 900 to 1300°C, and even more preferably 1000 to 1200°C.
[0037] The firing time in the firing step is not particularly limited, but is preferably 0.5 to 24 hours, more preferably 1 to 12 hours, and even more preferably 3 to 8 hours.
[0038] The method for producing the composite oxide may include a step of purifying the product obtained after the calcination step by filtering, washing with water, or the like, and a step of drying the product.
[0039] <Resin composition> The present invention also relates to a resin composition containing the above-mentioned material for high-frequency electronic components and a resin. The present invention also relates to a resin composition containing the above composite oxide (β) and a resin. The above composite oxide can suppress the viscosity increase of the resin composition when mixed with a resin, and therefore can sufficiently suppress the occurrence of voids and the like in the resin composition, thereby more sufficiently suppressing the dielectric loss tangent of the resin composition.
[0040] The proportion of the composite oxide in the resin composition is not particularly limited, but is preferably 0.1 to 99% by volume, more preferably 1 to 50% by volume, and even more preferably 2 to 30% by volume, relative to 100% by volume of the resin composition. As described above, the complex oxide (β) has a predetermined specific surface area, and therefore can suppress the viscosity increase of the resin composition, and therefore the amount of complex oxide can be increased compared to when conventional materials are used.
[0041] The resin contained in the resin composition is not particularly limited, and various resins such as thermoplastic resins, thermosetting resins, room temperature curable resins, ultraviolet curable resins, and radiation curable resins can be used. Specific examples include polyethylene resin, epoxy resin, phenol resin, polyphenylene sulfide (PPS) resin, polyester resin, polyamide, polyimide, polystyrene, polypropylene, polyvinyl chloride, polyvinylidene chloride, fluororesin, polymethyl methacrylate, ethylene-ethyl acrylate copolymer (EEA) resin, polycarbonate, polyurethane, polyacetal, polyphenylene ether, polyetherimide, acrylonitrile-butadiene-styrene copolymer (ABS) resin, liquid crystal resin (LCP), silicone resin, acrylic resin, etc. Among these, polyethylene resin is preferred.
[0042] The resin composition may contain other components in addition to the material for high-frequency electronic components and resin. The other components are not particularly limited, but examples thereof include inorganic particles other than the materials for high-frequency electronic components, curing agents, cure accelerators, stress reducing agents, silane coupling agents, surface treatment agents, flame retardant assistants, flame retardants, colorants, and mold release agents. The content of the other components is preferably 0 to 10% by mass, more preferably 0 to 5% by mass, and even more preferably 0 to 2% by mass, relative to 100% by mass of the resin composition.
[0043] The inorganic particles other than the materials for high-frequency electronic components are not particularly limited, but examples thereof include titanium compounds such as barium titanate, strontium titanate, calcium titanate, magnesium titanate, bismuth titanate, zirconium titanate, zinc titanate, and titanium dioxide. The curing agent is not particularly limited, but examples thereof include thiol-based curing agents, phenol-based curing agents, amine-based curing agents, and acid anhydride-based curing agents. The curing accelerator is not particularly limited, but examples thereof include amine-based curing accelerators, guanidine-based curing accelerators, imidazole-based curing accelerators, phosphonium-based curing accelerators, and metal-based curing accelerators.
[0044] <Applications for materials for high-frequency electronic components and resin compositions> The material for high-frequency electronic components of the present invention has a high dielectric constant and a low dielectric dissipation factor, and therefore the material for high-frequency electronic components and the resin composition of the present invention can be suitably used for circuit boards, sealing materials, insulating materials, underfills, resist inks, etc. for high-frequency devices and the like. The frequency band of high-frequency devices is preferably 1 MHz or higher, more preferably 10 MHz or higher, even more preferably 100 MHz or higher, and particularly preferably 1 GHz or higher. Also, the frequency band of high-frequency devices is preferably 500 GHz or lower. [Example]
[0045] Examples are given below to explain the present invention in more detail, but the present invention is not limited to only these examples. Unless otherwise specified, “%” means “mass %”.
[0046] ≪Physical Property Evaluation≫ <0Fifty particles were randomly extracted from the composite oxide observed by a scanning electron microscope (SEM), and the diameter of the planar part thereof was measured and averaged to obtain the plate surface diameter.
[0051] <Dielectric constant, dielectric loss tangent> [Dielectric properties of powder] The dielectric properties of the powder were determined for the dielectric constant ε and dielectric loss tangent tanδ of the powder at 1 GHz in the TM mode using a cavity resonator ADMS01Nc1 manufactured by AET Co., Ltd. and a vector network analyzer P9373A manufactured by Keysight Technologies, Inc. [Dielectric properties of resin composition] The oxide powder and polyethylene powder (manufactured by Tosoh Corporation, trade name: Petrothene 217-1) were weighed so that the filling amount of the powder was 8% by volume, and mixed at 30 rpm for 10 minutes using a Laboplastmill manufactured by Toyo Seiki Co., Ltd. The obtained mixture was weighed by a predetermined volume, placed in a 7 cm square gold frame, and sheeted under the conditions of 150 °C, 5 minutes, and 7 MPa using a heating press (Mini Test Press MP-WCH). The thickness of the sheet was about 0.9 mm, and a strip obtained by cutting the sheet into a width of 3 mm was used as an evaluation sample. The dielectric properties of the resin composition were determined for the dielectric constant ε and dielectric loss tangent tanδ at 10 GHz in the TM mode using a cavity resonator ADMS01Nc1 manufactured by AET Co., Ltd. and a vector network analyzer P9373A manufactured by Keysight Technologies, Inc.
[0052] <Ba / Ti ratio> The Ba / Ti ratio was determined by the calibration curve method using a fluorescence X-ray analyzer (ZSX PrimusII manufactured by Rigaku Corporation). For the preparation of the calibration curve at this time, a mixed powder of barium titanate and titanium oxide with a known Ba / Ti ratio was used in advance.
[0053] <Example 1> Step 1: Preparation of partially BT-modified titanium oxide 54.5 g of titanium dioxide (SSP-N, Sakai Chemical Industry Co., Ltd.) and 75.0 g of barium hydroxide octahydrate (Fujifilm Wako Pure Chemical Industries, Ltd.) were added to 500 ml of ion-exchanged water and stirred for 30 minutes. The resulting mixed slurry was then placed in a hydrothermal reactor, sealed, and heated at 120°C for 3 hours. After cooling to room temperature, the reactor was opened and the reaction slurry was removed, filtered, and washed with water. When the filtrate's conductivity reached 100 μS / cm or less, washing was stopped. The resulting filter cake was dried at 105°C for 12 hours to obtain a partially titanium dioxide-modified powder. Powder X-ray diffraction analysis of the resulting powder revealed only peaks for barium titanate (BaTiO3) and anatase-type titanium dioxide (TiO2).
[0054] Step 2: Plate-shaped Ba 11 Ti 28 O 66.5 Preparation of compounds 70 g of the partially BT titanium oxide powder obtained in step 1 was placed in an alumina crucible, 140 g of sodium chloride (Fujifilm Wako Pure Chemical Industries, Ltd.) was added, and the mixture was fired at 1150°C for 4 hours. The fired sintered body was repulped with ion-exchanged water, filtered, and washed with water. When the conductivity of the filtrate reached 50 μs / cm or less, the washing was stopped, and the resulting filter cake was dried at 105°C for 12 hours to obtain a powder.
[0055] [Powder property evaluation] The particle shape of the obtained powder was confirmed by scanning electron microscopy, and it was found to be plate-like particles with a plate diameter of 4.4 μm. Furthermore, powder X-ray diffraction analysis showed peaks at 2θ = 30.68° and 2θ = 38.60°. The specific surface area was 0.86 m 2 The molar ratio of barium to titanium (Ba / Ti) determined by fluorescent X-ray analysis was 0.35. [Dielectric property evaluation] The powder dielectric properties of the obtained powder were a dielectric constant of 13.1 and a dielectric loss tangent of 0.0005 at 1 GHz, and the resin composition dielectric properties were a dielectric constant of 3.70 and a dielectric loss tangent of 0.00025 at 10 GHz.
[0056] <Example 2> A powder was obtained in the same manner as in Example 1, except that step 1 was not performed in Example 1, and step 2 was performed using a mixed powder of 52 g of titanium oxide (SA-120 manufactured by Sakai Chemical Industry Co., Ltd.) and 88 g of barium titanate (BT-01 manufactured by Sakai Chemical Industry Co., Ltd.) instead of the partially BT-treated titanium oxide powder. [Powder property evaluation] The particle shape of the obtained powder SA-120 was confirmed by scanning electron microscopy, and it was found to be plate-like particles with a plate diameter of 41.5 μm. Furthermore, powder X-ray diffraction analysis showed peaks at 2θ = 30.68° and 2θ = 38.62°. The specific surface area was 0.23 m 2 The molar ratio of barium to titanium (Ba / Ti) determined by fluorescent X-ray analysis was 0.37. [Dielectric property evaluation] The powder dielectric properties of the obtained powder were a dielectric constant of 15.6 and a dielectric loss tangent of 0.0018 at 1 GHz.
[0057] <Comparative Example 1> Instead of the plate-like compound obtained in step 2 of Example 1, granular barium titanate particles (BT-05 manufactured by Sakai Chemical Industry Co., Ltd.) having a particle size of 0.5 μm were used to evaluate the powder properties and dielectric characteristics. [Powder property evaluation] Powder X-ray diffraction analysis showed no diffraction peaks at 30.7±0.3° and 2θ=38.6±0.2°. The specific surface area was 2.20 m 2 The molar ratio of barium to titanium (Ba / Ti) determined by fluorescent X-ray analysis was 1.00. [Dielectric property evaluation] The dielectric properties of the powder were a dielectric constant of 18.0 and a dielectric dissipation factor of 0.0500 at 1 GHz, and the dielectric properties of the resin composition were a dielectric constant of 3.45 and a dielectric dissipation factor of 0.01750 at 10 GHz.
[0058] <Comparative Example 2> Instead of the plate-like compound obtained in step 2 of Example 1, granular calcium titanate particles (CT-03 manufactured by Sakai Chemical Industry Co., Ltd.) having a particle size of 0.3 μm were used to evaluate the powder properties and dielectric characteristics. [Powder property evaluation] Powder X-ray diffraction analysis showed no diffraction peaks at 30.7±0.3° and 2θ=38.6±0.2°. The specific surface area was 5.00 m 2 The molar ratio of barium to titanium (Ba / Ti) determined by fluorescent X-ray analysis was 0.00. [Dielectric property evaluation] The powder dielectric properties were a dielectric constant of 12.8 and a dielectric loss tangent of 0.0070 at 1 GHz. The dielectric properties of the resin composition were a dielectric constant of 3.20 and a dielectric loss tangent of 0.00047 at 10 GHz.
Claims
1. Contains a composite oxide of barium and titanium, The composite oxide is a material for high-frequency electronic components, which has diffraction peaks at 2θ=30.7±0.3° and 2θ=38.6±0.2° in an XRD pattern when analyzed by powder X-ray diffraction.
2. 2. The material for high frequency electronic components according to claim 1, wherein the composite oxide has a molar ratio of barium element to titanium element (Ba / Ti) of 0.34 to 0.
40.
3. A composite oxide of barium and titanium, The composite oxide has diffraction peaks at 2θ=30.7±0.3° and 2θ=38.6±0.2° in an XRD pattern analyzed by powder X-ray diffraction, and has a specific surface area of 0.1 to 2.0 m 2 / g of a composite oxide of barium and titanium.
4. 4. The composite oxide of barium and titanium according to claim 3, wherein the composite oxide has a molar ratio of barium element to titanium element (Ba / Ti) of 0.34 to 0.
40.
5. A resin composition comprising the composite oxide according to claim 3 or 4 and a resin.
6. A method for producing a composite oxide of barium and titanium, comprising the steps of: The production method includes a step of hydrothermally reacting a titanium compound with a barium compound; and a step of mixing the product obtained in the hydrothermal reaction step with an alkali metal halide and calcining the mixture.
7. 7. The method for producing a composite oxide of barium and titanium according to claim 6, wherein the titanium compound is titanium oxide and / or titanium hydroxide.
8. 8. The method for producing a composite oxide of barium and titanium according to claim 6 or 7, wherein the barium compound is barium hydroxide and / or barium oxide.
9. 8. The method for producing a composite oxide of barium and titanium according to claim 6 or 7, wherein the alkali metal halide is sodium chloride.
10. The method for producing a barium and titanium composite oxide according to claim 6 or 7, wherein the ratio of the titanium compound to the barium compound used in the hydrothermal reaction step is 0.34 to 0.40 in terms of a molar ratio of barium element to titanium element (Ba / Ti).
11. The method for producing a composite oxide of barium and titanium according to claim 6 or 7, wherein the reaction temperature in the hydrothermal reaction step is 80 to 250°C.
Citation Information
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