WO2019113973A1 - Matériau céramique diélectrique et son procédé de préparation - Google Patents

Matériau céramique diélectrique et son procédé de préparation Download PDF

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WO2019113973A1
WO2019113973A1 PCT/CN2017/116617 CN2017116617W WO2019113973A1 WO 2019113973 A1 WO2019113973 A1 WO 2019113973A1 CN 2017116617 W CN2017116617 W CN 2017116617W WO 2019113973 A1 WO2019113973 A1 WO 2019113973A1
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ceramic material
dielectric ceramic
analytically pure
powder
sintering
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PCT/CN2017/116617
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Chinese (zh)
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袁亮亮
陆正武
曾俊
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深圳市大富科技股份有限公司
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Priority to CN201780034792.6A priority Critical patent/CN109415266B/zh
Priority to PCT/CN2017/116617 priority patent/WO2019113973A1/fr
Publication of WO2019113973A1 publication Critical patent/WO2019113973A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Definitions

  • the invention belongs to the technical field of ceramic materials, and in particular relates to a dielectric ceramic material and a preparation method thereof.
  • Alumina dielectric ceramic is a new type of electronic functional ceramic used as a medium in microwave and frequency band circuits. It has high physical strength (refractive strength >300MPa), low dielectric constant ( ⁇ r value ⁇ 9), low loss (quality). Factor Q value>100000), frequency temperature coefficient ⁇ f value is small, so it can be made into chip antenna, radar substrate, resonator support and other components, widely used in mobile communication, military radar, satellite positioning navigation system and other technologies. field. However, the sintering temperature of the ceramic material is usually higher than 1700 ° C, and the Q value of the quality factor is generally not high due to the micro defects generated in the sintering process, thereby restricting the more popular promotion and application of the alumina dielectric ceramic in the communication industry. .
  • conventional alumina dielectric ceramics are mainly prepared by solid phase synthesis, and a large amount of low-melting glass phase is added to reduce the sintering temperature.
  • the inventors of the present application found that by adding a large amount of low-melting glass phase, the dielectric properties of the alumina dielectric ceramic material are impaired, and the Q value of the alumina dielectric ceramic quality factor is lowered.
  • the technical problem mainly solved by the present invention is to provide a dielectric ceramic material and a preparation method thereof, which can obtain a dielectric ceramic material with high density and high quality factor while reducing the sintering temperature.
  • a technical solution adopted by the present invention is to provide a method for preparing a dielectric ceramic material, the method comprising:
  • a ball milling medium, deionized water and a dispersing agent are added to the starting material of the analytically pure alumina and the sintering aid having an alpha crystal phase having a purity of 99.9% or more, and mechanically mixed in a planetary ball mill, and dried after mixing. Processing, obtaining a mixed powder, wherein the mass ratio of the starting material, the ball milling medium and the deionized water is 1:4:1.1 to 1.3, the ball milling time is 4 hours, and the diameter range of the ball milling medium a diameter of 2 to 3 mm, the mass percentage of the dispersant in the dielectric ceramic material is from three thousandths to six thousandths;
  • the mixed powder is placed in a nano-scale circulating sander for sanding and dispersing treatment to obtain a ceramic powder;
  • the ceramic powder is subjected to heat sintering to obtain the dielectric ceramic material.
  • the sintering aid is at least one selected from the group consisting of analytical pure boron oxide, analytically pure silica, analytically pure magnesium oxide, and analytically pure zinc oxide.
  • the molar ratio of the analytical pure alumina to each of the sintering aids contained in the dielectric ceramic material is 1:x, and the value of x ranges from 0.01 to 0.1.
  • the dielectric ceramic material has a dielectric constant ⁇ r of 9.7 to 9.8 and a quality factor Q of 150,000 to 290000 GHz.
  • the ceramic powder has a sintering temperature of 1350 to 1500 ° C and a holding time of 2 to 8 hours.
  • the mixed powder after ball milling by a planetary ball mill has a particle size of 800 nm or more.
  • the method further comprises:
  • Spray granulation to form the ceramic powder into powder particles having spherical fluidity Spray granulation to form the ceramic powder into powder particles having spherical fluidity.
  • the powder particles obtained by the spray granulation have a size distribution of 200 to 250 mesh.
  • the method further comprises:
  • Dry compression molding to form the spherical fluid powder particles into a ceramic green compact of a desired shape.
  • the method further comprises:
  • the dielectric properties of the obtained dielectric ceramic material were tested using a network analyzer, wherein the test frequency was 9 to 10 GHz.
  • the ceramic powder obtained by the sanding dispersion treatment has a particle size distribution in the range of 50 to 100 nm.
  • another technical solution adopted by the present invention is to provide a dielectric ceramic material comprising an analytically pure alumina of ⁇ phase and a sintering aid, and the molecular formula of Al 2 O 3 —xMO Wherein MO represents a sintering aid, and x has a value in the range of 0.01 to 0.1.
  • the dielectric ceramic material has a grain size distribution ranging from 50 to 100 nanometers.
  • the sintering aid is at least one selected from the group consisting of analytical pure boron oxide, analytically pure silica, analytically pure magnesium oxide, and analytically pure zinc oxide.
  • the dielectric ceramic material has a dielectric constant ⁇ r of 9.7 to 9.8 and a quality factor Q of 150,000 to 290000 GHz.
  • the invention has the beneficial effects that, in the preparation method of the dielectric ceramic material provided by the prior art, since the ceramic powder is a powder with high microscopic uniformity obtained after the nano-scale ultrafine grinding treatment, That is, the ceramic powder is finer and the particle size distribution is uniform, so that the growth of the crystal grains is uniform, the grain size is uniform, the grain arrangement is dense, and the crystal grains, the grain boundaries and the combination therebetween are all in the nanometer order, and finally the obtained material.
  • High quality factor Q high compactness, high physical strength, microscopic defects The probability of trapping is greatly reduced.
  • the ceramic powder that has been refined into smaller particles has a smaller surface activation energy, and the temperature at the time of heating and sintering is also lowered, and at the same time, the industrial system of the material system can be effectively reduced. Energy consumption and production costs.
  • 1 is an SEM image of an embodiment of a dielectric ceramic material provided by the present invention
  • FIG. 2 is a schematic flow chart of an embodiment of a method for preparing a dielectric ceramic material of the present invention.
  • Figure 1 is an SEM image of an embodiment of a dielectric ceramic material provided by the present invention.
  • a dielectric ceramic material according to an embodiment of the present invention wherein the dielectric ceramic material may be, but not limited to, a millimeter wave dielectric ceramic material, and the dielectric ceramic material includes an analytically pure alumina having an alpha crystal phase having a purity of 99.9% or more and a sintering aid.
  • the dielectric ceramic material is a composite material of an analytically pure alumina and a sintering aid containing an ⁇ crystal phase having a purity of 99.9% or more.
  • the dielectric ceramic material has a grain size distribution in the range of 50 to 100 nanometers, for example, 50 nanometers, 75 nanometers, or 100 nanometers.
  • the dielectric ceramic material is prepared by at least high-temperature calcination of the ceramic powder, and the ceramic powder is obtained by a sand-dispersion treatment of a nano-scale circulating sander, so that the ceramic powder has a particle size distribution ranging from 50 to 100 nm. Internal, and has a high degree of dispersion.
  • High-efficiency centrifugal separation systems for nano-scale circulating sanders are commonly used in wet grinding and dispersion processes, especially for obtaining powders with high dispersibility and nanometer size.
  • the high-efficiency centrifugal separation system can use a minimum diameter of 30 ⁇ m to 300 ⁇ m.
  • the grinding media is subjected to continuous grinding to grind the raw material into nano-powders having a uniform particle size, a high degree of dispersion, and a particle size diameter of less than 200 nm.
  • the analytically pure alumina and the sintering aid are contained in an alpha phase having a purity of 99.9% or more.
  • the mixed material is also mechanically mixed before being subjected to the scrub dispersion treatment of the nano-scale circulating sander.
  • a ball milling medium, deionized water, and a dispersing agent are added to the starting material of the analytically pure alumina and the sintering aid having an alpha crystal phase having a purity of 99.9% or more, and mechanically mixed in a planetary ball mill. Drying is carried out to obtain a mixed powder in which the mass ratio of the starting material, the ball milling medium and the deionized water is 1:4:1.1 to 1.3, for example, 1:4:1.1, 1:4:1.2 or 1:4: 1.3, etc., the ball milling time is 4 hours, and the diameter of the ball milling medium ranges from 2 to 3 mm in diameter, for example, 2 mm, 2.5 mm or 3 mm.
  • the mixed powder obtained by ball milling usually has a particle size of 800 nm or more.
  • the ball-milled mixed powder is placed in a nano-scale circulating sander for sanding and dispersion treatment, and a ceramic powder having a high dispersibility and a particle size distribution in the range of 50 to 100 nm can be obtained. Since the ceramic powder is a high-micro-uniformity powder obtained after nano-scale ultra-fine grinding treatment, that is, the ceramic powder is fine and the particle size distribution is uniform, so that the crystal grains are uniformly distributed, the crystal grain size is uniform, and the crystal is uniform.
  • the grain arrangement is dense and the grain, the grain boundary and the combination between them are in the nanometer order, so that the material quality factor Q obtained at the end is higher, the compactness is higher, the physical strength is high, and the probability of microscopic defects is greatly reduced.
  • the refined ceramic powder has a small particle size, and the activated surface activation energy is low, so that the temperature during heating and sintering is also lowered, and at the same time, the industrial energy consumption and production cost of the material system can be effectively reduced.
  • the dielectric ceramic material has a molecular formula of Al 2 O 3 —xMO, wherein MO represents a sintering aid, and the sintering aid is selected from at least one of analytical pure boron oxide, analytically pure silica, analytically pure magnesium oxide, and analytically pure zinc oxide.
  • the molar ratio of the pure alumina to each of the sintering aids contained in the material is 1:x, and the value of x ranges from 0.01 to 0.1, such as 0.01, 0.05 or 0.1.
  • the molecular ceramic material may have a molecular formula of Al 2 O. 3 —0.07 ⁇ SiO 2 —(1-y)ZnO—yMgO ⁇ , which means that the analytical pure alumina, analytically pure silica, analytically pure zinc oxide, and analytical pure magnesium oxide have a molar ratio of 1:0.07:0.07 (1).
  • the selected sintering aid comprises analytically pure silica and analytically pure Zinc oxide, when the value of y is greater than 0 and less than 1, the selected sintering aid is composed of analytically pure silica, analytically pure zinc oxide and analytically pure magnesium oxide.
  • the auxiliaries include analytically pure silica and analytically pure magnesium oxide.
  • the material type and content of the sintering aid can be adjusted according to requirements.
  • the ceramic powder can be effectively improved during the sintering process. Problems such as abnormal grain growth, such as avoiding the phenomenon that a plurality of crystal grains are agglomerated, thereby effectively improving the Q value of the material quality factor.
  • the sintering temperature of the material of the present embodiment is 1350 to 1500 ° C, for example, 1350 ° C, 1425 ° C or 1500 ° C; the dielectric constant ⁇ r is 9.7 to 9.8, for example, 9.7, 9.75, 9.8, etc.; the quality factor Q is 150,000. 290000 GHz, for example, 150,000 GHz, 200000 GHz, 290,000 GHz, and the like.
  • the present embodiment provides a dielectric ceramic material which is a composite material of analytically pure alumina and a sintering aid containing an ⁇ crystal phase having a purity of 99.9% or more.
  • a sintering aid to the analysis of pure alumina, problems such as abnormal growth of crystal grains in the sintering process can be effectively avoided, thereby effectively improving the Q value of the quality factor of the material.
  • FIG. 2 is a schematic flow chart of an embodiment of a method for preparing a dielectric ceramic material according to the present invention.
  • a method for preparing a dielectric ceramic material according to an embodiment of the present invention, the preparation method comprising:
  • Step S101 adding a ball milling medium, deionized water and a dispersing agent to the starting material of the analytically pure alumina and the sintering aid having an ⁇ crystal phase having a purity of 99.9% or more, and mechanically mixing in a planetary ball mill, and mixing is completed. Thereafter, drying treatment is carried out to obtain a mixed powder.
  • the molecular formula is Al 2 O 3 —xMO, wherein MO represents a sintering aid, and the sintering aid is selected from at least one of analytical pure boron oxide, analytically pure silica, analytically pure magnesium oxide, and analytically pure zinc oxide.
  • the molar ratio of alumina to each of the sintering aids contained in the material is 1:x, and the value of x ranges from 0.01 to 0.1, such as 0.01, 0.05 or 0.1.
  • the molecular ceramic material may have a molecular formula of Al 2 O. 3 —0.07 ⁇ SiO 2 —(1-y)ZnO—yMgO ⁇ , which means that the analytical pure alumina, analytically pure silica, analytically pure zinc oxide, and analytical pure magnesium oxide have a molar ratio of 1:0.07:0.07 (1).
  • the selected sintering aid comprises analytically pure silica and analytically pure Zinc oxide, when the value of y is greater than 0 and less than 1, the selected sintering aid is composed of analytically pure silica, analytically pure zinc oxide and analytically pure magnesium oxide.
  • the auxiliaries include analytically pure silica and analytically pure magnesium oxide.
  • the material type and content of the sintering aid can be adjusted according to requirements.
  • the mass ratio of the starting material, the ball milling medium and the deionized water is 1:4:1.1 to 1.3, for example, 1:4:1.1, 1:4:1.2 or 1:4:1.3, etc.
  • the ball milling time is 4 hours.
  • the diameter of the ball milling medium ranges from 2 to 3 mm in diameter, for example 2 mm, 2.5 mm or 3 mm, etc.
  • the mass percentage of the dispersant in the material is from three thousandths to six thousandths, for example, three thousandths, one thousandths Five or six thousandths, etc.
  • the particle size of the mixed powder after ball milling by a planetary ball mill is greater than or equal to 800 nm.
  • step S102 the mixed powder is placed in a nano-scale circulating sander for sanding and dispersion treatment to obtain a ceramic powder.
  • the starting material is placed in a nano-scale circulating sander for sanding and dispersing treatment, a highly dispersible ceramic powder is obtained, and the particle size distribution of the ceramic powder is in the range of 50 to 100 nm, for example, 50 nm, 75 nm, 100 nm, etc. .
  • the ceramic powder is a high-micro-uniformity powder obtained after nano-scale ultra-fine grinding treatment, that is, the ceramic powder is fine and the particle size distribution is uniform, so that the crystal grains are uniformly distributed, the crystal grain size is uniform, and the crystal is uniform.
  • the grain arrangement is dense and the grain, the grain boundary and the combination between them are in the nanometer order, so that the material quality factor Q obtained at the end is higher, the compactness is higher, the physical strength is high, and the probability of microscopic defects is greatly reduced.
  • the refined ceramic powder has a small particle size, and the activated surface activation energy is low, so that the temperature during heating and sintering is also lowered, and at the same time, the industrial energy consumption and production cost of the material system can be effectively reduced.
  • step S103 the ceramic powder is heated and sintered to obtain a dielectric ceramic material.
  • the ceramic powder is placed in a muffle furnace for sintering, and the sintering temperature is 1350 to 1500 ° C, for example, 1350 ° C, 1425 ° C, 1500 ° C, etc., and the holding time is 2 to 8 hours, for example, 2 hours, 5 hours, After 8 hours, etc., a dielectric ceramic material was obtained.
  • the dielectric constant ⁇ r of the material is 9.7 to 9.8, for example, 9.7, 9.75, 9.8, etc.; the quality factor Q is 150,000 to 290000 GHz, for example, 150,000 GHz, 200,000 GHz, 290,000 GHz, and the like.
  • the dispersing agent volatilizes in a high temperature environment, that is, the formed dielectric ceramic material does not contain a dispersing agent.
  • the method before the step of subjecting the raw material of the analytically pure alumina and the sintering aid having an alpha crystal phase having a purity of 99.9% or more to the nano-scale circulating sander for the sanding dispersion treatment, the method further comprises:
  • the method before the step of heating and sintering the ceramic powder, the method further comprises:
  • Spray granulation to form the ceramic powder into powder particles having spherical fluidity Spray granulation to form the ceramic powder into powder particles having spherical fluidity.
  • polyvinyl alcohol having a mass percentage of 10% is added to the ceramic powder, and spray granulation is carried out to obtain powder particles having spherical fluidity.
  • the powder particles obtained by spray granulation have a size distribution of 200 to 250 mesh, for example, 200 mesh, 225 mesh or 250 mesh.
  • the method further comprises:
  • Dry pressing to form spherical powdery powder particles into a ceramic compact of a desired shape, wherein The pressure during dry pressing is in the range of 140 to 160 MPa, for example, 140 MPa, 150 MPa or 160 MPa.
  • the powder particles are dry-formed under a pressure of 150 MPa to obtain a green wafer having a diameter of 12 mm and a thickness of 6 mm.
  • the shape of the ceramic green compact depends on the shape and size of the mold, and can be adjusted accordingly according to requirements, which is not limited herein.
  • the method further comprises:
  • the dielectric properties of the obtained materials were tested using a network analyzer, wherein the test frequency was 9 to 10 GHz.
  • the material of the present embodiment was tested to have a dielectric constant ⁇ r of 9.7 to 9.8 and a quality factor Q of 150,000 to 290000 GHz.
  • the method for preparing a dielectric ceramic material includes: adding a ball milling medium, deionized water, and a dispersing agent to a starting material of an analytically pure alumina and a sintering aid having an ⁇ crystal phase having a purity of 99.9% or more, And mechanically mixing in a planetary ball mill, and after drying, drying treatment is performed to obtain a mixed powder, wherein the mass ratio of the starting material, the ball milling medium and the deionized water is 1:4:1.1-1.3 a ball milling time of 4 hours, a diameter of the ball milling medium ranging from 2 to 3 mm, and a mass percentage of the dispersing agent in the dielectric ceramic material of from three thousandths to six thousandths; The powder is placed in a nano-scale circulating sander for sanding and dispersing treatment to obtain a ceramic powder; the ceramic powder is heated and sintered to obtain the dielectric ceramic material.
  • the ceramic powder is a high-micro-uniformity powder obtained after nano-scale ultra-fine grinding treatment, that is, the ceramic powder is fine and the particle size distribution is uniform, so that the crystal grains are uniformly distributed, the crystal grain size is uniform, and the crystal is uniform.
  • the grain arrangement is dense and the grain, the grain boundary and the combination between them are in the nanometer order, so that the material quality factor Q obtained at the end is higher, the compactness is higher, the physical strength is high, and the probability of microscopic defects is greatly reduced.
  • the refined ceramic powder has a small particle size, and the activated surface activation energy is low, so that the temperature during heating and sintering is also lowered, and at the same time, the industrial energy consumption and production cost of the material system can be effectively reduced.
  • the starting material of Example 1 is compounded according to the formula Al 2 O 3 —xMO, wherein MO represents one of B 2 O 3 , SiO 2 , MgO, ZnO, and the molar ratio of the analytical pure alumina to the sintering aid is 1: x, where x ranges from 0.01 to 0.1.
  • Analytically pure alumina having a purity of 99.9% of the ⁇ crystal phase and a mixed material of analytically pure boron oxide, analytically pure silica, analytically pure magnesium oxide or analytically pure zinc oxide were respectively used as starting materials, and were obtained by the following process steps.
  • the polyurethane ball mill can be ball milled in a planetary ball mill for 4 hours;
  • step 3 transferring the ball-milled mixed powder in step 2 to a nano-scale circulating sand mill, and performing sanding dispersion treatment until a ceramic powder having a particle size ranging from 50 to 100 nm and having high dispersibility is obtained;
  • step 3 adding the ceramic powder after the sanding in step 3 to a polyvinyl alcohol having a mass percentage of 10% for spray granulation to obtain powder particles having a size ranging from 250 to 300 mesh;
  • the powder particles obtained in the step 4 are dry-formed, and a green wafer having a diameter of 12 mm and a thickness of 6 mm is obtained under a pressure of 150 MPa;
  • the green compact wafer in the step 5 is placed in a muffle furnace for sintering, the sintering temperature is 1400 to 1500 ° C, and the sintering holding time is 4 hours to obtain an alumina ceramic sample.
  • the dielectric properties of the alumina ceramic samples obtained above were tested using a network analyzer (Agilient 5071C) at a test frequency of 9.46 GHz and a Q factor of up to 194,000 GHz. See Table 1 for detailed results.
  • Example 2 The starting material of Example 2 was formulated according to the formula Al 2 O 3 —0.07 ⁇ SiO 2 —(1-y)ZnO—yMgO ⁇ , wherein pure alumina, analytically pure silica, analytically pure zinc oxide and analytical analysis were analyzed.
  • the molar ratio of pure magnesium oxide is 1:0.07:0.07 (1-y): 0.07y, wherein y ranges from 0 to 1.
  • a mixed material of analytically pure alumina, analytically pure silica and analytically pure magnesium oxide or/and analytically pure zinc oxide having a purity of 99.9% of ⁇ phase was used as a starting material, and was achieved by the following process steps.
  • the polyurethane ball mill can be ball milled in a planetary ball mill for 4 hours;
  • step 3 transferring the ball-milled mixed powder in step 2 to a nano-scale circulating sand mill, and performing sanding dispersion treatment until a ceramic powder having a particle size ranging from 50 to 100 nm and having high dispersibility is obtained;
  • step 3 adding the ceramic powder after the sanding in step 3 to a polyvinyl alcohol having a mass percentage of 10% for spray granulation to obtain powder particles having a size ranging from 250 to 300 mesh;
  • the powder particles obtained in the step 4 are dry-formed, and a green wafer having a diameter of 12 mm and a thickness of 6 mm is obtained under a pressure of 150 MPa;
  • the green compact wafer in the step 5 is placed in a muffle furnace for sintering, the sintering temperature is 1300 to 1450 ° C, and the sintering holding time is 6 hours to obtain an alumina ceramic sample.
  • the dielectric properties of the alumina ceramic samples obtained above were tested by a network analyzer (Agilient 5071C) at a test frequency of 9.53 GHz, a dielectric constant ⁇ r of 9.7, and a Q factor of up to 297000 GHz.
  • a network analyzer Agilient 5071C

Abstract

La présente invention concerne un matériau céramique diélectrique et son procédé de préparation. Le procédé comprend : l'ajout d'un milieu de broyage à billes, d'eau déionisée et d'un agent de dispersion à un matériau de départ constitué d'α-alumine analytiquement pure, présentant une pureté de 99,9 % ou plus, et d'auxiliaires de frittage, le mélange mécanique du tout dans un broyeur à billes planétaire et le séchage de l'ensemble pour obtenir une poudre mélangée, le rapport pondéral entre le matériau de départ, le milieu de broyage à billes et l'eau déionisée étant de 1/4/1,1-1,3, la durée du broyage à billes étant de 4 heures, la plage de diamètre du milieu de broyage à billes variant de 2 à 3 mm et la teneur en pourcentage en masse du matériau céramique diélectrique en agent de dispersion variant de trois millièmes à six millièmes ; l'introduction de la poudre mélangée dans un broyeur à sable nanométrique à circulation pour un traitement de broyage et de dispersion afin d'obtenir une poudre céramique ; et le chauffage et le frittage de la poudre céramique pour obtenir le matériau céramique diélectrique.
PCT/CN2017/116617 2017-12-15 2017-12-15 Matériau céramique diélectrique et son procédé de préparation WO2019113973A1 (fr)

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CN114550977A (zh) * 2022-03-03 2022-05-27 太原理工大学 一种低温共烧陶瓷介质材料及其制备方法
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