WO2021241192A1 - 無機構造体及びその製造方法 - Google Patents

無機構造体及びその製造方法 Download PDF

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Publication number
WO2021241192A1
WO2021241192A1 PCT/JP2021/017819 JP2021017819W WO2021241192A1 WO 2021241192 A1 WO2021241192 A1 WO 2021241192A1 JP 2021017819 W JP2021017819 W JP 2021017819W WO 2021241192 A1 WO2021241192 A1 WO 2021241192A1
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Prior art keywords
zirconium silicate
particles
bonding portion
silicon
inorganic structure
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PCT/JP2021/017819
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English (en)
French (fr)
Japanese (ja)
Inventor
夏希 佐藤
亮介 澤
達郎 吉岡
直樹 栗副
徹 関野
知代 後藤
成訓 趙
寧浚 徐
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Panasonic Intellectual Property Management Co Ltd
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Panasonic Intellectual Property Management Co Ltd
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Priority to CN202180037781.XA priority Critical patent/CN115697908B/zh
Priority to EP21814151.3A priority patent/EP4159676A4/en
Priority to JP2022527644A priority patent/JP7432905B2/ja
Priority to US17/926,891 priority patent/US20230234855A1/en
Publication of WO2021241192A1 publication Critical patent/WO2021241192A1/ja
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/02—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
    • B28B3/025—Hot pressing, e.g. of ceramic materials
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    • C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
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Definitions

  • the present invention relates to an inorganic structure and a method for producing the same.
  • a sintering method has been conventionally known as a method for manufacturing an inorganic structure made of ceramics.
  • the sintering method is a method for obtaining a sintered body by heating an aggregate of solid powder made of an inorganic substance at a temperature lower than the melting point.
  • Patent Document 1 discloses a method for producing a polycrystalline body comprising a polycrystalline zircon phase of about 45% by weight-about 95% by weight and a polycrystalline cozy light phase of about 5% by weight-about 55% by weight. Specifically, a mixture consisting of zircon and / or ZrO 2 , Al 2 O 3 , MgO and SiO 2 and a nucleating agent is made; the above mixture is compactly molded; the compact is in the range of about 1290 ° C to about 1550 ° C. Sintered in-house to form a sintered body; the sintered body is nucleated and annealed at a temperature of about 600 ° C. to about 800 ° C.; the obtained nucleated body is converted into a nucleated body from about 1200 ° C. It discloses that it undergoes a step of crystallization annealing at a temperature below the temperature at which it is produced.
  • the sintering method requires heating the solid powder at a high temperature, there is a problem that energy consumption during manufacturing is large and cost is high. Further, it is said that the solid powders are not sufficiently bonded to each other by simply compacting the solid powders under low temperature conditions, so that the obtained molded body has many pores and the mechanical strength is insufficient. There's a problem.
  • An object of the present invention is to provide an inorganic structure which can be produced by a simple method and has higher density, and a method for producing the inorganic structure.
  • the inorganic structure according to the first aspect of the present invention covers the surface of a plurality of zirconium silicate particles and the zirconium silicate particles, and bonds between the zirconium silicate particles. And prepare.
  • the bonding portion contains an amorphous compound containing silicon, a metal element other than silicon, and oxygen, and is substantially free of alkali metals, B, V, Te, P, Bi, Pb, and Zn.
  • the method for producing an inorganic structure according to the second aspect of the present invention is to mix a plurality of zirconium silicate particles, a plurality of amorphous silicon dioxide particles, and an aqueous solution containing a metal element other than silicon. It has a step of obtaining a mixture and a step of pressurizing and heating the mixture under the conditions of a pressure of 10 to 600 MPa and a temperature of 50 to 300 ° C.
  • FIG. 1 is a cross-sectional view schematically showing an example of an inorganic structure according to the present embodiment.
  • FIG. 2 is a cross-sectional view schematically showing another example of the inorganic structure according to the present embodiment.
  • FIG. 3 is a schematic cross-sectional view for explaining a method for manufacturing an inorganic structure according to the present embodiment.
  • FIG. 4 is a graph showing the XRD pattern of zircon registered in ICSD, the XRD pattern of test sample 2 and test sample 3 in the reference example, and the XRD pattern of the sample holder.
  • FIG. 5A is a scanning electron microscope image of the test sample 1 of the example magnified 2000 times.
  • FIG. 5B is a scanning electron microscope image of the test sample 1 magnified 10000 times.
  • FIG. 5 (c) is a scanning electron microscope image of zircon powder magnified 2000 times.
  • FIG. 5D is a scanning electron microscope image of zircon powder magnified 10,000 times.
  • FIG. 6A is a diagram showing a backscattered electron image at position 1 in the test sample 1 of the example.
  • FIG. 6B is a diagram showing a backscattered electron image at position 2 in the test sample 1.
  • FIG. 6C is a diagram showing a backscattered electron image at position 3 in the test sample 1.
  • FIG. 7A is a diagram showing binarized data of the backscattered electron image at position 1 in the test sample 1 of the example.
  • FIG. 7B is a diagram showing binarized data of the backscattered electron image at position 2 in the test sample 1.
  • FIG. 7C is a diagram showing binarized data of the backscattered electron image at position 3 in the test sample 1.
  • the inorganic structure 1 of the present embodiment contains a plurality of zirconium silicate particles 2. Then, the adjacent zirconium silicate particles 2 are bonded to each other via the bonding portion 3 to form an inorganic structure 1 in which the zirconium silicate particles 2 are aggregated.
  • the zirconium silicate particles 2 contain zirconium silicate (zircon, ZrSiO 4 ) as a main component. That is, the zirconium silicate particles 2 preferably contain 50 mol% or more of zirconium silicate, more preferably 80 mol% or more, and particularly preferably 90 mol% or more.
  • the zirconium silicate particles 2 are preferably crystalline. Since the zirconium silicate particles 2 are crystalline particles, it is possible to obtain an inorganic structure 1 having higher durability than in the case of amorphous particles.
  • the zirconium silicate particles 2 may be single crystal particles or polycrystalline particles.
  • the average particle size of the zirconium silicate particles 2 constituting the inorganic structure 1 is not particularly limited.
  • the average particle size of the zirconium silicate particles 2 is preferably 300 nm or more and 50 ⁇ m or less, more preferably 300 nm or more and 30 ⁇ m or less, and particularly preferably 300 nm or more and 20 ⁇ m or less.
  • the average particle size of the zirconium silicate particles 2 is within this range, the zirconium silicate particles 2 can be firmly bonded to each other and the strength of the inorganic structure 1 can be increased. Further, since the average particle size of the zirconium silicate particles 2 is within this range, the proportion of pores existing inside the inorganic structure 1 is 20% or less, as will be described later.
  • the inorganic structure 1 It is possible to increase the strength of.
  • the value of the "average particle size" is several to several tens of fields using an observation means such as a scanning electron microscope (SEM) or a transmission electron microscope (TEM) unless otherwise specified. The value calculated as the average value of the particle diameters of the particles observed inside is adopted.
  • the shape of the zirconium silicate particles 2 is not particularly limited, but may be spherical, for example. Further, the zirconium silicate particles 2 may be whiskers-like (needle-like) particles or scaly particles. Since the whiskers-like particles or the scaly particles have higher contact with other particles and contact with the bonding portion 3 as compared with the spherical particles, it is possible to increase the strength of the entire inorganic structure 1.
  • the inorganic structure 1 of the present embodiment includes a bonding portion 3 that bonds between a plurality of zirconium silicate particles 2.
  • the zirconium silicate particles 2 are three-dimensionally bonded to each other, so that a bulk body having high mechanical strength can be obtained.
  • the bonding portion 3 contains an amorphous compound containing at least silicon, a metal element other than silicon, and oxygen.
  • the inorganic structure 1 is formed by heating and pressurizing a mixture of zirconium silicate particles, amorphous silicon dioxide particles, and an aqueous solution containing a metal element other than silicon. ,Obtainable. At this time, the reaction between the silicon dioxide particles and the aqueous solution forms an amorphous compound containing silicon, a metal element, and oxygen. Therefore, the bonding portion 3 contains an amorphous compound containing at least silicon, a metal element other than silicon, and oxygen.
  • the binding portion 3 preferably contains an amorphous compound as a main component. Specifically, the binding portion 3 preferably contains 50 mol% or more of the amorphous compound, more preferably 70 mol% or more, and further preferably 90 mol% or more.
  • the metal element other than silicon contained in the amorphous compound of the bonding portion 3 can be at least one selected from the group consisting of alkali metals, alkaline earth metals, transition metals, base metals and metalloids.
  • an alkaline earth metal includes beryllium and magnesium in addition to calcium, strontium, barium and radium.
  • Base metals include aluminum, zinc, gallium, cadmium, indium, tin, mercury, thallium, lead, bismuth and polonium.
  • Metalloids include boron, silicon, germanium, arsenic, antimony and tellurium.
  • the metal element other than silicon is preferably zirconium.
  • the inorganic structure 1 can be obtained by heating and pressurizing a mixture of zirconium silicate particles, amorphous silicon dioxide particles, and an aqueous solution containing zirconium. can. At this time, the reaction between the silicon dioxide particles and the aqueous solution containing zirconium forms an amorphous compound containing silicon, oxygen, and zirconium. Therefore, the bonding portion 3 preferably contains an amorphous compound containing silicon, oxygen, and zirconium.
  • the bonding portion 3 does not substantially contain alkali metal, B, V, Te, P, Bi, Pb and Zn. Further, it is preferable that the binding portion 3 does not substantially contain Ca, Sr and Ba.
  • the bonding portion substantially does not contain alkali metal, B, V, Te, P, Bi, Pb and Zn means that the bonding portion 3 intentionally contains alkali metal, B, V, Te. , P, Bi, Pb and Zn are not contained. Therefore, when alkali metal, B, V, Te, P, Bi, Pb and Zn are mixed as unavoidable impurities in the bonding portion 3, "the bonding portion is an alkali metal, B, V, Te, P, Bi, Pb.
  • the binding portion substantially does not contain Ca, Sr and Ba means that the binding portion 3 does not intentionally contain Ca, Sr and Ba. .. Therefore, when Ca, Sr and Ba are mixed in the binding portion 3 as unavoidable impurities, the condition that "the binding portion does not substantially contain Ca, Sr and Ba" is satisfied.
  • the bonding portion 3 is in direct contact with the zirconium silicate particles 2. Further, the bonding portion 3 preferably covers at least a part of the surface of the zirconium silicate particles 2, and more preferably covers the entire surface of the zirconium silicate particles 2. As a result, the zirconium silicate particles 2 and the bonding portion 3 are firmly bonded to each other, so that an inorganic structure 1 having excellent denseness and mechanical strength can be obtained.
  • the bonding portion 3 may contain fine particles 4 having an average particle size of 100 nm or less. Since the bonding portion 3 contains a plurality of fine particles 4, the bonding portion 3 has a more dense structure, so that the strength of the inorganic structure 1A can be increased.
  • the bonding portion 3 is formed by reacting the amorphous silicon dioxide particles with an aqueous solution containing a metal element other than silicon by heating and pressurizing. Therefore, the inside of the bonding portion 3 may contain particulate matter derived from silicon dioxide particles. Further, as will be described later, the particle size of the amorphous silicon dioxide particles is preferably 100 nm or less. Therefore, the bonding portion 3 may contain fine particles 4 derived from silicon dioxide particles and having an average particle size of 100 nm or less. The particle size of the fine particles 4 contained in the bonding portion 3 can be measured using a scanning electron microscope or a transmission electron microscope.
  • the fine particles 4 contained in the bonding portion 3 may be particles made of an amorphous compound containing silicon, oxygen, and a metal element other than silicon. Further, the fine particles 4 may be particles made of a crystalline compound containing silicon, oxygen, and a metal element other than silicon. The fine particles 4 contained in the bonding portion 3 may be particles made of an amorphous compound containing silicon, oxygen, and zirconium. Further, the fine particles 4 may be particles made of a crystalline compound containing silicon, oxygen and zirconium. The fine particles 4 may contain silicon dioxide that has not reacted with an aqueous solution containing a metal element other than silicon.
  • the volume ratio of the zirconium silicate particles 2 is larger than the volume ratio of the bonding portion 3.
  • the obtained inorganic structures 1, 1A are structures that can easily utilize the characteristics of the zirconium silicate particles 2.
  • the zirconium silicate particles 2 are materials having a low thermal conductivity of about 1.3 W / m ⁇ K and excellent heat insulating properties. Therefore, by making the volume ratio of the zirconium silicate particles 2 larger than the volume ratio of the bonding portion 3, the heat insulating property of the entire inorganic structures 1, 1A can be improved.
  • the bonding portion 3 further contains crystalline zirconium silicate.
  • the bonding portion 3 contains an amorphous compound containing silicon, oxygen, and zirconium, and more preferably contains an amorphous compound containing silicon, oxygen, and zirconium. Therefore, the crystal structure of the bonding portion 3 is at least partially amorphous.
  • the bonding portion 3 preferably contains crystalline zirconium silicate in addition to the amorphous compound.
  • the bonding portion 3 preferably contains an amorphous compound containing silicon, oxygen, and zirconium.
  • the ratio of silicon to zirconium in the amorphous compound is not particularly limited.
  • the fine particles 4 may be particles made of an amorphous compound containing silicon, oxygen, and zirconium, or may be particles made of crystalline zirconium silicate. good.
  • the fine particles 4 may contain silica derived from silicon dioxide particles as a raw material.
  • the bonding portion 3 may contain zirconium silicate as a crystalline compound.
  • the bonding portion 3 is formed by the reaction of amorphous silicon dioxide particles and an aqueous solution containing a metal element other than silicon by heating and pressurizing, so that the bonding portion 3 has a dense phase.
  • pores may be present inside the bonding portion 3 and at least one position between the bonding portion 3 and the zirconium silicate particles 2.
  • the porosity of the inorganic structures 1, 1A in the cross section is preferably 20% or less. That is, when observing the cross section of the inorganic structure 1, 1A, it is preferable that the average value of the ratio of pores per unit area is 20% or less. When the porosity is 20% or less, the ratio of the zirconium silicate particles 2 bonded to each other by the bonding portion 3 increases, so that the inorganic structures 1 and 1A become dense and the strength increases. Therefore, it is possible to improve the machinability of the inorganic structures 1, 1A. Further, when the porosity is 20% or less, cracks are suppressed from occurring in the inorganic structures 1, 1A starting from the pores, so that the bending strength of the inorganic structures 1, 1A can be increased.
  • the porosity in the cross section of the inorganic structure 1, 1A is preferably 10% or less, more preferably 8% or less, and further preferably 5% or less. The smaller the porosity in the cross section of the inorganic structures 1, 1A, the more the cracks originating from the pores are suppressed, so that the strength of the inorganic structures 1, 1A can be increased.
  • the porosity can be determined as follows. First, the cross section of the inorganic structures 1, 1A is observed to discriminate the zirconium silicate particles 2, the bonding portion 3, and the pores. Then, the unit area and the area of the pores in the unit area are measured, the ratio of the pores per unit area is obtained, and the value is used as the porosity. It is more preferable to determine the ratio of pores per unit area at a plurality of locations with respect to the cross section of the inorganic structures 1, 1A, and then use the average value of the ratio of pores per unit area as the porosity. When observing the cross section of the inorganic structures 1, 1A, an optical microscope, a scanning electron microscope (SEM), or a transmission electron microscope (TEM) can be used. Further, the unit area and the area of the pores in the unit area may be measured by binarizing the image observed with a microscope.
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • the size of the pores existing inside the inorganic structures 1, 1A is not particularly limited, but it is preferably as small as possible. Since the size of the pores is small, cracks originating from the pores are suppressed, so that the strength of the inorganic structures 1, 1A can be increased and the machinability of the inorganic structures 1, 1A can be improved. ..
  • the pore size of the inorganic structures 1, 1A is preferably 5 ⁇ m or less, more preferably 1 ⁇ m or less, and even more preferably 100 nm or less.
  • the size of the pores existing inside the inorganic structures 1, 1A can be determined by observing the cross section of the inorganic structures 1, 1A with a microscope in the same manner as the above-mentioned porosity.
  • the inorganic structures 1 and 1A may have a structure in which the zirconium silicate particles 2 are bonded to each other via the bonding portion 3. Therefore, as long as the inorganic structures 1, 1A have such a structure, the shape thereof is not limited.
  • the shapes of the inorganic structures 1, 1A can be, for example, a plate shape, a film shape, a rectangular shape, a lump shape, a rod shape, or a spherical shape.
  • the thickness t thereof is not particularly limited, but may be, for example, 50 ⁇ m or more.
  • the inorganic structures 1, 1A of the present embodiment are formed by a pressure heating method, as will be described later.
  • the thickness t of the inorganic structures 1, 1A can be 500 ⁇ m or more, 1 mm or more, or 1 cm or more.
  • the upper limit of the thickness t of the inorganic structures 1, 1A is not particularly limited, but may be, for example, 50 cm.
  • the inorganic structures 1, 1A are structures that retain the characteristics of the zirconium silicate particles 2 and the bonding portion 3. For example, since the zirconium silicate particles 2 have high heat insulating properties, the obtained inorganic structures 1 and 1A also have excellent heat insulating properties.
  • the inorganic structures 1 and 1A of the present embodiment include the plurality of zirconium silicate particles 2 and the bonding portion 3 that covers the surface of the zirconium silicate particles 2 and bonds between the zirconium silicate particles 2.
  • the bonding portion 3 contains an amorphous compound containing silicon, a metal element other than silicon, and oxygen.
  • the coupling portion 3 is substantially free of alkali metals, B, V, Te, P, Bi, Pb and Zn.
  • a plurality of zirconium silicate particles 2 are bonded via a highly dense bonding portion 3. Therefore, the inorganic structures 1, 1A having excellent denseness and mechanical strength can be obtained.
  • zirconium silicate has a thermal conductivity of about 1.3 W / m ⁇ K, and is known to have a low thermal conductivity among ceramic materials. Therefore, by using zirconium silicate particles 2 and forming the bonding portion 3 as an amorphous compound containing silicon, oxygen, and zirconium, an inorganic structure 1, 1A having excellent heat insulating properties in addition to mechanical strength can be obtained. ..
  • the inorganic structures 1, 1A preferably have a thermal conductivity of 1 W / m ⁇ K or less. At this time, the thermal conductivity can be measured in accordance with Japanese Industrial Standards JIS R1611 (measurement method of thermal diffusion rate, specific heat capacity, and thermal conductivity by the flash method of fine ceramics).
  • the inorganic structures 1 and 1A of the present embodiment can be a structure in which only the zirconium silicate particles 2 are bonded via the bonding portion 3.
  • the inorganic structures 1,1A can be obtained by pressurizing while heating at 50 to 300 ° C.
  • a member having low heat resistance can be added to the inorganic structures 1,1A. ..
  • the inorganic structures 1, 1A may contain organic substances and resin particles in addition to the zirconium silicate particles 2 and the bonding portion 3.
  • the inorganic structure 1, 1A is not limited to a member having low heat resistance such as an organic substance, and may contain particles made of an inorganic compound other than the zirconium silicate particles 2 and the bonding portion 3.
  • the inorganic structure includes a step of obtaining a mixture by mixing a plurality of zirconium silicate particles, a plurality of amorphous silicon dioxide particles, and an aqueous solution, and a step of pressurizing and heating the mixture.
  • a method for producing the inorganic structures 1, 1A includes a step of obtaining a mixture by mixing a plurality of zirconium silicate particles, a plurality of amorphous silicon dioxide particles, and an aqueous solution, and a step of pressurizing and heating the mixture.
  • the zirconium silicate particles preferably contain 50 mol% or more of zirconium silicate, more preferably 80 mol% or more, and particularly preferably 90 mol% or more.
  • Silicon dioxide particles are particles made of amorphous silicon dioxide.
  • the silicon dioxide particles are preferably fumed particles, that is, fumed silica.
  • Fused silica is an amorphous silica particle having a particle size of primary particles of about 5 nm to 50 nm.
  • This fumed silica is a particle produced by combustion hydrolysis of silicon tetrachloride, and the primary particles are aggregated and agglomerated to form bulky secondary particles. Therefore, fumed silica has high reactivity with an aqueous solution, and an amorphous compound containing silicon and oxygen can be easily formed.
  • an aqueous solution containing a metal element other than silicon is used as the aqueous solution.
  • the aqueous solution containing a metal element other than silicon is an aqueous solution containing the metal element as an ion.
  • the metal element other than silicon can be at least one selected from the group consisting of alkali metals, alkaline earth metals, transition metals, base metals and metalloids.
  • the solvent for dissolving the metal element is preferably pure water or ion-exchanged water. However, the solvent may contain an acidic substance or an alkaline substance in addition to water, or may contain an organic solvent (for example, alcohol).
  • the "aqueous solution containing a metal element other than silicon" is also referred to as a "metal element-containing aqueous solution”.
  • aqueous solution it is preferable to use an aqueous solution containing zirconium.
  • the aqueous solution containing zirconium is an aqueous solution containing zirconium as an ion, and for example, an aqueous solution of zirconium oxyacetate can be used.
  • zirconium-containing aqueous solution is also referred to as a "zirconium-containing aqueous solution”.
  • a mixture of zirconium silicate particles 11, silicon dioxide particles 12, and a metal element-containing aqueous solution 13 is filled inside the mold 14.
  • the mold 14 is heated if necessary. Then, by applying pressure to the mixture inside the mold 14, the inside of the mold 14 becomes a high pressure state.
  • the silicon dioxide particles 12 are amorphous and highly reactive, the silicon dioxide particles 12 and the metal element-containing aqueous solution 13 react with each other, and the bonding portion 3 containing silicon, oxygen, and a metal element other than silicon is contained. Is formed.
  • the fumed silica when used as the silicon dioxide particles 12, the fumed silica has a nano-level particle size, so that the fumed silica is filled between the zirconium silicate particles 11 without any gaps. Therefore, the obtained bonding portion 3 has a dense structure, and the zirconium silicate particles 11 can be firmly bonded to each other.
  • the zirconium silicate particles 11 and the zirconium-containing aqueous solution both contain zirconium, so that the zirconiums easily diffuse from each other.
  • a compound 15 containing silicon, oxygen, and zirconium, for example, zirconium silicate is likely to be formed on the surface of the zirconium silicate particles 11. Therefore, since the obtained bonding portion 3 firmly bonds while covering the zirconium silicate particles 11, it is possible to increase the mechanical strength of the inorganic structures 1, 1A.
  • the heating and pressurizing conditions of the mixture obtained by mixing the zirconium silicate particles 11, the silicon dioxide particles 12, and the metal element-containing aqueous solution 13 are such that the reaction between the silicon dioxide particles 12 and the metal element-containing aqueous solution 13 proceeds.
  • the conditions are not particularly limited. For example, it is preferable to pressurize the mixture at a pressure of 10 to 600 MPa while heating the mixture to 50 to 300 ° C.
  • the temperature at which the mixture is heated is more preferably 80 to 250 ° C, further preferably 100 to 200 ° C.
  • the pressure when pressurizing the mixture is more preferably 50 to 600 MPa, further preferably 200 to 600 MPa.
  • the amorphous silicon dioxide particles 12 may completely react with the metal element-containing aqueous solution 13 to become a compound containing silicon, oxygen, and zirconium. Further, the silicon dioxide particles 12 may not completely react with the metal element-containing aqueous solution 13 and may remain as silicon dioxide in the bonding portion 3.
  • the bonding portion 3 is formed by the reaction between the silicon dioxide particles 12 and the metal element-containing aqueous solution 13, the bonding portion 3 is derived from the silicon dioxide particles and contains fine particles 4 having an average particle diameter of 100 nm or less. It may be included.
  • the fine particles 4 may contain silicon dioxide that has not reacted with the metal element-containing aqueous solution 13.
  • the inorganic structures 1, 1A are formed by pressurizing a mixture of zirconium silicate particles 11, silicon dioxide particles 12, and a metal element-containing aqueous solution 13 at 10 to 600 MPa and 50 to 300 ° C. It can be obtained by heating. Then, by such a heating and pressurizing step, the bonding portion 3 containing the amorphous compound can be formed. However, by lengthening the heating and pressurizing time of the mixture, a part of the amorphous compound crystallizes.
  • the bonding portion 3 further contains crystalline zirconium silicate, it is preferable to lengthen the heating and pressurizing time of the mixture of the zirconium silicate particles, the silicon dioxide particles, and the zirconium-containing aqueous solution.
  • fumed particles that is, fumed silica
  • alumina Al 2 O 3
  • titania TIO 2
  • at least one of fumed alumina and fumed titania may be further mixed with the mixture formed by mixing the zirconium silicate particles 11, the silicon dioxide particles 12, and the metal element-containing aqueous solution 13.
  • the fused alumina and / or the fused titania reacts with the metal element-containing aqueous solution 13, and the reaction product can be contained in the bonding portion 3.
  • a method of pressing only the powder of zirconium silicate particles can be considered.
  • the powder of the zirconium silicate particles is put into a mold and pressurized at room temperature, the particles of the zirconium silicate particles do not easily react with each other, and it is difficult to firmly bond the particles to each other. Therefore, the obtained green compact has many pores, and the mechanical strength is insufficient.
  • a method of forming an aggregate of zirconium silicate particles a method of pressing only the powder of zirconium silicate particles to form a green compact and then firing at a high temperature (for example, 1700 ° C. or higher) can be considered.
  • a high temperature for example, 1700 ° C. or higher
  • the zirconium silicate particles are sintered together to form a structure.
  • the zirconium silicate particles even if the green compact of zirconium silicate particles is fired at a high temperature, it is difficult for the zirconium silicate particles to sinter with each other. Therefore, the obtained structure has many pores and the mechanical strength is insufficient. Will be. Further, when the zirconium silicate particles are fired at a high temperature, precise temperature control is required, which increases the manufacturing cost.
  • a mixture of zirconium silicate particles 11, amorphous silicon dioxide particles 12, and a metal element-containing aqueous solution 13 is heated and pressurized. Therefore, it is possible to obtain a structure that is dense and has excellent strength. Further, since the manufacturing method of the present embodiment can be obtained by pressurizing while heating at 50 to 300 ° C., precise temperature control becomes unnecessary and the manufacturing cost can be reduced.
  • the method for producing the inorganic structures 1, 1A of the present embodiment is an aqueous solution 13 containing a plurality of zirconium silicate particles 11, a plurality of amorphous silicon dioxide particles 12, and a metal element other than silicon. It has a step of obtaining a mixture by mixing with and.
  • the production method further comprises a step of pressurizing and heating the mixture under conditions of a pressure of 10 to 600 MPa and a temperature of 50 to 300 ° C. Therefore, in the production method of the present embodiment, an inorganic structure having high density can be produced by a simple method.
  • the inorganic structure 1 can be in the shape of a plate having a large thickness, and is also excellent in stability because it is dense. Further, the inorganic structure 1 has high mechanical strength and can be cut in the same manner as a general ceramic member, and can also be surface-treated. Therefore, the inorganic structure 1 can be suitably used as a building member.
  • the building member is not particularly limited, and examples thereof include an outer wall material (siding) and a roofing material. Moreover, as a building member, a material for a road and a material for an outer groove can also be mentioned.
  • the inorganic structure 1 can also be suitably used as a member for electronic devices.
  • members for electronic devices include structural materials, heat-resistant members, insulating members, heat insulating members, sealing materials, circuit boards, optical members, and the like.
  • zirconium oxyacetate powder ZrO (CH 3 COO) 2 , manufactured by Mitsuwa Chemical Co., Ltd.
  • ZrO (CH 3 COO) 2 zirconium oxyacetate powder
  • the entire amount of the mixed powder was put into the inside of the cylindrical molding die ( ⁇ 10) having an internal space. Further, 400 ⁇ l of a zirconium oxyacetate aqueous solution was added to the inside of the molding die, and the mixture was mixed with a plastic spatula. In the mixed powder containing the zirconium oxyacetate aqueous solution, SiO 2 was 250 mol% with respect to Zr (CH 3 COO) 2.
  • the mixed powder containing the zirconium oxyacetate aqueous solution was heated and pressurized at 150 ° C., 400 MPa and 60 minutes. In this way, the test sample 1 of this example having a columnar shape was obtained.
  • a test sample containing no zircon powder was prepared. First, 0.2 g of the same silica powder as in the examples was put into the inside of a cylindrical molding die ( ⁇ 10) having an internal space. Further, 300 ⁇ l of the zirconium oxyacetate aqueous solution prepared in the example was added to the inside of the molding die, and the mixture was mixed with a plastic spatula.
  • the silica powder containing the zirconium oxyacetate aqueous solution was heated and pressurized under the conditions of 150 ° C., 400 MPa and 60 minutes to obtain a test sample 2 containing no zircon powder. Further, separately, the silica powder containing the zirconium oxyacetate aqueous solution was heated and pressurized under the conditions of 150 ° C., 400 MPa and 240 minutes to obtain a test sample 3 containing no zircon powder.
  • test sample 2 prepared with a heating / pressurizing time of 60 minutes was prepared under the same conditions as the test sample 1 of the example except that it did not contain zircon powder. Therefore, it is considered that the test sample 2 of the reference example has the same crystal structure as the silicon-containing compound (silicon-containing compound) in the test sample 1 of the example. Further, the test sample 3 containing no zircon powder prepared with a heating / pressurizing time of 240 minutes has a crystal structure similar to that of the silicon-containing compound when the test sample 1 of the example is heated and pressurized for 240 minutes. It is thought that it is.
  • FIG. 4 shows an XRD pattern of zircon registered in ICSD, an XRD pattern of test sample 2 and test sample 3 containing no zircon powder, and an XRD pattern of a sample holder.
  • the silicon-containing compound contained in the test sample 1 of the example is amorphous. It is conceivable that. That is, the silicon-containing compound constituting the bond 3 in the test sample 1 is considered to be amorphous.
  • the silicon-containing compound constituting the bond 3 in the test sample 1 is considered to be amorphous.
  • the silicon-containing compound is composed of crystalline zircon and an amorphous compound. That is, when the heating / pressurizing time of the test sample 1 is set to 240 minutes, it is considered that the silicon-containing compound constituting the bonding portion 3 is composed of crystalline zircon and an amorphous compound.
  • FIG. 5A shows an SEM image of the test sample 1 magnified 2000 times
  • FIG. 5B shows an SEM image of the test sample 1 magnified 10000 times
  • FIG. 5 (c) shows an SEM image of the zircon powder magnified 2000 times
  • FIG. 5 (d) shows an SEM image of the zircon powder magnified 10000 times.
  • the zircon powders (zirconium silicate particles 2) are bonded to each other via the bonding portion 3. Further, in the test sample 1, a precise structure can be confirmed. Further, as shown by reference numeral A in FIG. 5B, it can be confirmed that the inside of the coupling portion 3 contains fine fine particles 4 having a particle size of 100 nm or less.
  • a cross-section polisher processing (CP processing) was applied to a cross section of the test sample 1 of the example having a columnar shape.
  • SEM scanning electron microscope
  • a backscattered electron image was observed with respect to the cross section of the test sample 1 at a magnification of 50,000 times.
  • the reflected electron images obtained by observing three places (positions 1 to 3) on the cross section of the test sample 1 are shown in FIGS. 6 (a), 6 (b), and 6 (c).
  • the white portion 22 is zircon
  • the gray portion 23 is a silicon-containing compound
  • the black portion 25 is a pore.
  • the pores were clarified by binarizing each of the SEM images in the three fields of view.
  • the binarized images of the backscattered electron images of FIGS. 6 (a), 6 (b), and 6 (c) are shown in FIGS. 7 (a), 7 (b), and 7 (c), respectively.
  • the area ratio of the pore portion was calculated from the binarized image, and the average value was taken as the porosity. Specifically, from FIG. 7A, the area ratio of the pore portion at position 1 was 7.4%. From FIG. 7B, the area ratio of the pore portion at position 2 was 5.9%. From FIG. 7 (c), the area ratio of the pore portion at position 3 was 7.3%. Therefore, the porosity of the test sample 1 produced this time was 6.8%, which is the average value of the area ratio of the pore portions at positions 1 to 3.
  • an inorganic structure having a higher density and a method for producing the inorganic structure, which can be produced by a simple method.

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