WO2017113224A1 - 陶瓷材料及其制备方法、谐振器、滤波器及射频拉远设备 - Google Patents

陶瓷材料及其制备方法、谐振器、滤波器及射频拉远设备 Download PDF

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WO2017113224A1
WO2017113224A1 PCT/CN2015/099954 CN2015099954W WO2017113224A1 WO 2017113224 A1 WO2017113224 A1 WO 2017113224A1 CN 2015099954 W CN2015099954 W CN 2015099954W WO 2017113224 A1 WO2017113224 A1 WO 2017113224A1
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organic binder
zinc
degreasing
green body
cerium
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PCT/CN2015/099954
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English (en)
French (fr)
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庄后荣
陆正武
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深圳市大富科技股份有限公司
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Priority to CN201580079830.0A priority Critical patent/CN107614461A/zh
Priority to PCT/CN2015/099954 priority patent/WO2017113224A1/zh
Publication of WO2017113224A1 publication Critical patent/WO2017113224A1/zh

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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
    • C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers

Definitions

  • the invention relates to the technical field of preparation of resonators, in particular to a ceramic material and a preparation method thereof, a resonator, a filter and a radio remote device.
  • the dielectric resonator is a basic microwave component.
  • the dielectric resonator can be used to form microwave circuits such as filters, oscillators and antennas. It is widely used in mobile communication, satellite communication, military radar, global positioning system, Bluetooth technology, wireless LAN, etc. In modern communication, it is the key infrastructure of modern communication technology.
  • dielectric resonators used in microwave circuits must meet the following dielectric performance requirements: (1) have a relatively high dielectric constant ⁇ r at microwave frequencies, and generally require ⁇ r >20 In order to miniaturize and integrate the microwave device; (2) have a very low dielectric loss at the microwave resonant frequency, that is, a high quality factor (Q ⁇ f), to ensure excellent frequency selection characteristics and reduce device Insertion loss at high frequencies; (3) Temperature coefficient of resonance frequency ( ⁇ f ) close to zero to ensure high stability of the resonant frequency of the device in a temperature changing environment.
  • ⁇ Zn-cerium ceramics (Ba(Zn 1/3 Nb 2/3 )O 3 , BZN) has a complex perovskite structure and is a microwave dielectric ceramic with a high Q value in the X-band (7-8 GHz). An extremely important dielectric material in the field of microwave high frequencies such as satellite communications.
  • BZN ceramics have a relatively high value of ⁇ f ( ⁇ 30 ppm/°C) which limits their practical application. Many researchers have reduced the ⁇ f value of BZN to zero by exploring various chemical formulations.
  • the disordered temperature of Ba(Ni 1/3 Nb 2/3 )O 3 has contradictory values in the literature, varying from 1400 ° C to > 1500 ° C.
  • the X-ray pattern of this phase usually has a secondary heterophase, which may be related to the partial melting or volatilization of NiO at high temperatures.
  • the uneven mixing of the components of the traditional solid phase method and the volatilization of Ni at high temperatures may be the cause of the inconsistency of the order of the system.
  • the ceramic is sintered dense at 1500 ° C
  • the Q value is ⁇ 5700 (10 GHz).
  • the molding process in the prior art is mainly dry press molding.
  • the principle of dry pressing is as follows: the dielectric ceramic powder is granulated by a binder, pressed and formed by a die, and then sintered.
  • the preparation of the dielectric resonator by this process has the following disadvantages: (1) During the press forming process, internal and external friction between the particles and between the particles and the mold wall causes pressure loss to cause uneven force in various portions of the green compact, so green body and sintering The sample density distribution is not uniform. The degree of unevenness is related to the selected pressing method.
  • the common pressing methods are unidirectional pressing and bidirectional pressing.
  • the density distribution is shown in Figures 1a and 1b.
  • the uniformity of density affects the dielectric properties of the dielectric resonator. It also affects the performance of the filter; (2) limited by the pressing method, the dielectric resonator is mostly columnar (or similar), not all shape sizes can be prepared by dry pressing, such as complex shaped resonators.
  • Demolding is difficult to achieve, and resonators with large aspect ratios cannot be produced by pressing, because low density regions are likely to occur due to uneven density, which causes distortion of the resonator during sintering, resulting in poor precision in order to obtain a desired shape. Or the size also needs to be machined.
  • the density of the resonators of the prepared microwave dielectric ceramic material is not uniform, resulting in poor dielectric properties of the microwave dielectric ceramic resonator;
  • the dry pressing method cannot prepare a resonator with a complicated shape.
  • the invention provides a ceramic material and a preparation method thereof, a resonator, a filter and a radio remote device,
  • the invention can solve the uneven density distribution, low dimensional precision, low quality factor Q ⁇ f value, unstable performance and the shape of the prepared shape which are easy to occur in the dry press forming process of the prior art bismuth zinc bismuth based dielectric resonator. Limited problem.
  • a technical solution adopted by the present invention is to provide a raw material formulation of a bismuth-zinc ruthenium-based dielectric resonator, the raw material formulation comprising the following components by weight:
  • the organic binder comprises a binder, a surfactant and a plasticizer; the binder is 50%-90% by weight in the organic binder; the surfactant is The weight percentage in the organic binder is from 1% to 5%; the weight percentage of the plasticizer in the organic binder is from 3% to 22%.
  • the binder is at least one selected from the group consisting of paraffin wax, ethylene-vinyl acetate copolymer, polypropylene, atactic polypropylene, polystyrene, polymethacrylate, and ethylene ethyl acrylate copolymer.
  • the surfactant is at least one selected from the group consisting of stearic acid, octanoic acid and microcrystalline paraffin.
  • the plasticizer is a low melting point plasticizer.
  • the plasticizer is at least one selected from the group consisting of dibutyl phthalate, diethyl phthalate and dioctyl phthalate.
  • another technical solution adopted by the present invention is to provide a method for preparing a bismuth-zinc-based ruthenium-based dielectric resonator, the preparation method comprising the steps of: bismuth-zinc-based ceramic powder and an organic binder Mixing to obtain a mixed material, wherein the cerium zinc cerium-based ceramic powder has a weight percentage of 76%-85%, and the organic binder has a weight percentage of 15%-24%;
  • the mixture is heated to form the melt into a melt; the melt is injection molded using an injection molding machine to obtain a green body; the green body is degreased to remove the organic binder; and the degreased blank is The body is sintered to obtain a dielectric resonator.
  • the cerium-zinc-cerium-based ceramic powder is mixed with the organic binder on a mixer, and the mixing time is 4-8 hour.
  • the mixture is heated to cause the mixture to form a melt, and the heating temperature is from 150 ° C to 250 ° C.
  • the melt is injected into a metal mold, and after 2 to 5 minutes, the mold is cooled and released to obtain the green body.
  • the step of degreasing the green body comprises: oil extracting and degreasing the green body; and thermally degreasing the oil body after oil extraction and degreasing.
  • the step of oil extracting and degreasing the green body comprises: placing the green body in a non-polar solvent, the non-polar solvent having a temperature of 30-50 ° C and a degreasing time of 12-36 hours; The green body is taken out from the non-polar solvent and dried in an oven, wherein the drying temperature is 50-70 ° C and the drying time is 4-12 hours.
  • non-polar solvent is at least one selected from the group consisting of gasoline, carbon disulfide, xylene, diethyl ether, benzene, chloroform, carbon tetrachloride and naphtha.
  • the body in the step of thermally degreasing the body after degreasing the oil, the body is placed in an electric heating furnace, and is heated to a temperature of 500-600 ° C at a heating rate of 0.5-5 ° C / min, and the heat preservation 2 -3 hours.
  • the sintering temperature is 900-1400 ° C and the temperature is maintained for 2-6 hours.
  • the organic binder comprises a binder, a surfactant and a plasticizer; the binder is 50%-90% by weight in the organic binder; the surfactant is The weight percentage in the organic binder is from 1% to 5%; the weight percentage of the plasticizer in the organic binder is from 3% to 22%.
  • another technical solution adopted by the present invention is to provide a bismuth-zinc ruthenium-based dielectric resonator, which is obtained by the following preparation method: ⁇ Zn-based ceramic powder And mixing with an organic binder to obtain a mixture material, wherein the cerium zinc cerium-based ceramic powder has a weight percentage of 76%-85%, and the organic binder has a weight percentage of 15%-24 %; heating the mixture to form the mixture into a melt; using an injection molding machine to melt the mixture The green body is obtained by injection molding; the green body is degreased to remove the organic binder; and the degreased green body is sintered to obtain a dielectric resonator.
  • the organic binder comprises a binder, a surfactant and a plasticizer; the binder is 50%-90% by weight in the organic binder; the surfactant is The weight percentage in the organic binder is from 1% to 5%; the weight percentage of the plasticizer in the organic binder is from 3% to 22%.
  • the step of degreasing the green body comprises: oil extracting and degreasing the green body; and thermally degreasing the oil body after oil extraction and degreasing.
  • the step of oil extracting and degreasing the green body comprises: placing the green body in a non-polar solvent, the non-polar solvent having a temperature of 30-50 ° C and a degreasing time of 12-36 hours; The green body is taken out from the non-polar solvent and dried in an oven, wherein the drying temperature is 50-70 ° C and the drying time is 4-12 hours.
  • a technical solution adopted by the present invention is to provide a cavity filter including a cavity, a cover plate, and the dielectric resonator described in the above embodiment, the cover A plate covers the cavity to form a resonant cavity, and the dielectric resonator is mounted within the cavity.
  • the present invention also adopts a technical solution for providing a radio remote device, which includes: a radio frequency transceiver module, a power amplifier module, and a cavity filter according to the fourth aspect.
  • the radio frequency transceiver module is connected to the power amplifier module, and the power amplifier module is connected to the cavity filter.
  • the beneficial effects of the present invention are: different from the prior art, the zinc-zinc-based dielectric resonator of the present invention and the raw material formula and preparation method thereof, the zinc-cerium-based ceramic powder is added by adding more organic binder The mixture of the body and the organic binder forms a viscous melt after heating, so that the dielectric resonator can be formed by injection molding, thereby obtaining a dielectric resonator having uniform density distribution and high dimensional accuracy, and the material cost is low.
  • the preparation process is simple.
  • the Q value of the zinc-zinc-based dielectric resonator prepared by injection molding of the present invention is about 20,000 to 26,000 (higher than dry pressing molding 15000 to 25000), in addition, Injection molding can realize complex zinc bismuth Mass production of based dielectric resonators.
  • Figure 1a is a density distribution diagram of a unidirectionally pressed sample prepared by dry pressing
  • Figure 1b is a density distribution diagram of a biaxially compressed sample prepared by dry pressing
  • FIG. 2 is a schematic flow chart of an embodiment of a method for preparing a bismuth-zinc-based dielectric resonator according to the present invention
  • 3a is an electron microscope scan of the port of the Zn-Zn-based dielectric resonator prepared by dry pressing;
  • Figure 3b is an electron microscope scan of the port of the bismuth-zinc-based ruthenium dielectric resonator prepared by injection molding;
  • FIG. 4 is a block diagram showing the structural composition of a preferred embodiment of the radio remote device of the present invention.
  • the invention provides a molding raw material formula of a bismuth-zinc bismuth-based dielectric resonator, the molding raw material formula comprising the following components by weight: 76%-85% of lanthanum-cerium-based ceramic powder and 15%-24 % organic binder.
  • the content of the organic binder is 15% to 24% by weight, and the weight percentage of the organic binder in the conventional dielectric resonator is 5%.
  • the organic binder in the present invention has a large percentage by weight, and the organic binder having a large content can make the zinc-cerium-based ceramic powder and the organic bond.
  • the mixture of the agents forms a viscous melt upon heating, thereby allowing the molding material formulation of the present invention to form a dielectric resonator by injection molding.
  • the chemical expression of the bismuth-zinc-based composite microwave dielectric ceramic is:
  • the organic binder of this embodiment includes a binder, a surfactant, and a plasticizer.
  • the binder is mainly used for bonding the lanthanum zinc cerium-based ceramic powder, the binder is 50%-90% by weight in the organic binder, and the binder is selected from the group consisting of paraffin wax and ethylene-acetic acid. At least one of a vinyl ester copolymer, polypropylene, atactic polypropylene, polystyrene, polymethacrylate, and ethylene ethyl acrylate copolymer.
  • the surfactant is selected from at least one of stearic acid, octanoic acid and microcrystalline paraffin, and the surfactant is present in an amount of from 1% to 5% by weight based on the organic binder.
  • the plasticizer is 3%-22% by weight in the organic binder, and the plasticizer acts to increase flexibility and increase viscosity.
  • the plasticizer is a low melting plasticizer, thereby Melt at a lower temperature to mix well with the molten mixture.
  • the plasticizer is at least one selected from the group consisting of dibutyl phthalate, diethyl phthalate, and dioctyl phthalate.
  • the zinc-germanium-based ceramic powder in the molding material formulation of the dielectric resonator has a weight percentage of 76% and an organic binder content of 24% by weight.
  • the weight percentage of the binder is 50%, the weight percentage of the surfactant is 5%, and the weight percentage of the plasticizer is 22%.
  • the bismuth zinc cerium-based ceramic powder in the molding material formulation of the dielectric resonator has a weight percentage of 85% and an organic binder content of 15% by weight.
  • the weight percentage of the binder is 90%, the weight percentage of the surfactant is 1%, and the weight percentage of the plasticizer is 3%.
  • the bismuth zinc cerium-based ceramic powder in the molding material formulation of the dielectric resonator has a weight percentage of 80% and an organic binder content of 20% by weight.
  • the weight percentage of the binder is 80%, the weight percentage of the surfactant is 3%, and the weight percentage of the plasticizer is 15%.
  • the zinc-zinc-based dielectric resonator of the present invention and the raw material formula and preparation method thereof, by adding more organic binder, make the zinc-cerium-based ceramic powder and the organic binder The mixture is heated to form a viscous melt, so that the dielectric resonance can be formed by injection molding. Therefore, a dielectric resonator having uniform density distribution and high dimensional accuracy can be obtained, and the material cost is low and the preparation process is simple.
  • FIG. 2 is a schematic flow chart of an embodiment of a method for preparing a bismuth-zinc-based dielectric resonator according to the present invention. Specifically, the preparation method includes the following steps:
  • the chemical expression of the bismuth zinc bismuth based dielectric ceramic is:
  • the formula of bismuth zinc bismuth is determined mainly by solid phase preparation.
  • the ball milling medium is zirconia balls, and the ball milling time is 4-12 hours. Calcination is then carried out at a calcination temperature of from 1000 ° C to 1200 ° C.
  • the calcined powder is then placed in a ball mill for ball milling.
  • the ball milled medium is still zirconia balls, the ball milling time is still 4-12 hours, and 2%-5% PVA binder is added during the ball milling process.
  • the granulation is carried out on the spray tower, and the granulated powder is put into a mold for press molding, and the pressure is 100 MPa-200 MPa. After the press molding, the properties of the test material itself are sintered, thereby obtaining the desired dielectric material--zinc-zinc bismuth base.
  • Ceramic powder is made by solid phase preparation.
  • the organic binder of this embodiment includes a binder, a surfactant, and a plasticizer.
  • the binder is mainly used for bonding the lanthanum zinc cerium-based ceramic powder, the binder is 50%-90% by weight in the organic binder, and the binder is selected from the group consisting of paraffin wax and ethylene-acetic acid.
  • the binder is selected from the group consisting of paraffin wax and ethylene-acetic acid.
  • the surfactant is selected from at least one of stearic acid, octanoic acid and microcrystalline paraffin, and the surfactant is present in an amount of from 1% to 5% by weight based on the organic binder.
  • the plasticizer is 3%-22% by weight in the organic binder, and the plasticizer acts to increase flexibility and increase viscosity.
  • the plasticizer is a low melting plasticizer, thereby At lower Melt at temperature to mix well with the molten mixture.
  • the plasticizer is at least one selected from the group consisting of dibutyl phthalate, diethyl phthalate, and dioctyl phthalate.
  • the mixing of the cerium zinc cerium-based ceramic powder and the organic binder is carried out on a mixer for a mixing time of 4-8 hours.
  • the melt formed in the step S102 is viscous, which facilitates subsequent injection molding.
  • the heating temperature is from 150 ° C to 250 ° C.
  • the melt is injection molded using an injection molding machine to obtain a green body.
  • step S103 the melt is poured into a metal mold of an injection molding machine, and after 2 to 5 minutes, the mold is cooled and released to obtain a green body.
  • a dielectric resonator is formed by injection molding, and mass production of a zinc-zinc-based dielectric resonator having uniform density distribution, high dimensional accuracy, and complicated shape can be realized.
  • step S104 the organic binder in the green body is removed to prevent the organic binder from affecting the efficiency of the dielectric resonator.
  • the step of degreasing specifically comprises subjecting the body to a non-polar solvent extraction degreasing and thermal degreasing.
  • the non-polar volume extraction degreasing process is as follows: the injection-molded body is placed in a non-polar solvent such as gasoline, carbon disulfide, xylene, diethyl ether, really, chloroform, carbon tetrachloride or naphtha to dissolve Remove some organic binder, the temperature of the non-polar solvent is 30-50 ° C, the degreasing time is 12-36 hours, then the blank is taken out from the non-polar solvent, and placed in an oven for drying, drying temperature It is 50-70 ° C and the drying time is 4-12 hours.
  • the non-polar solvent extraction degreasing process in this step is very necessary because if the direct thermal desorption occurs, the sample is decomposed during the degreasing process due to the excessively high organic binder component in the embryo body.
  • the thermal degreasing process is as follows: the dried body is placed in an electric heating furnace for thermal degreasing to remove the remaining organic binder. In this process, the embryo body is heated to 550 ° C at a temperature increase rate of 0.5 to 5 ° C / min, and then kept for 2 to 3 hours.
  • step S105 the sintering temperature is between 900 and 1400 ° C and the temperature is maintained for 2 to 6 hours.
  • the dielectric resonator of BZN-based material was prepared by dry pressing method and injection molding method respectively.
  • the Q resonator value of the dielectric resonator prepared by dry pressing method was 15000-25000, the frequency was 2.3-2.6G, and the Q value of the dielectric resonator prepared by injection molding was From 20000 to 26000, the frequency is 2.3 to 2.7G (Note: samples prepared in the same batch (60) are used as inspection and comparison data).
  • the dielectric resonator prepared by injection molding has more stable performance.
  • the preparation method of the bismuth-zinc-cerium-based dielectric resonator provided by the invention can make the produced bismuth-zinc bismuth-based dielectric resonator have uniform density distribution and high dimensional precision, and also has high dielectric constant and high performance. It has stability, and also has high dielectric constant and performance stability.
  • mass production of a complex-shaped zinc-cerium-based dielectric resonator can be realized by injection molding.
  • the injection molding process has the following advantages: (1) The molding process has high mechanization and automation, high production efficiency, short molding cycle, high strength of the green body, convenient management and control in the production process, and easy to realize large-scale and large-scale production; (2) Nearly net forming small parts with complicated geometric shapes and special requirements, so that the sintered ceramic products do not need to be machined or processed less; (3) the molded products have extremely high dimensional accuracy and Surface finish.
  • the main material formulation of the present embodiment adopts a chemical formula: 0.5Ba(Ni 0.5 Co 0.5 ) 1/3 Nb 2/3 O 3 as a chemical composition, and compares the performance of the dielectric resonator prepared by the dry pressing method and the injection molding method, respectively.
  • the dielectric material itself has a dielectric property relative permittivity ⁇ r of 35, a quality factor (Q ⁇ f) value of 100800 GHz, and a resonance frequency temperature coefficient ⁇ f of +4.8 ppm/°C.
  • the dry pressing method mainly obtains a dielectric resonator by granulation, press molding, and sintering, and the process is simple.
  • the BZN-based dielectric resonator prepared by the injection molding process is realized by the following process steps:
  • (1) Mixed ceramic powder and organic binder The BZN-based ceramic powder and the organic binder are uniformly mixed to obtain an injection molding mixture, and the content of different components in the mixture is related to the particle size, morphology and density of the powder. Therefore, different powders have different mixture formulations; for BZN-based dielectric ceramics, injection molding In the mixture, the weight percentage of the BZN-based ceramic powder is 78%, and the weight percentage of the organic binder is 22%; the organic binder is composed of a binder, a surfactant, and a plasticizer, each of which The weight percentage of the components is: binder 80%; surfactant 5%; plasticizer: 15%.
  • injection molding The injection molding mixture was injection molded on an injection molding machine to obtain a green body, and the injection temperature was 180 ° C. After injection into the mold, the molded body was released in 2 minutes.
  • Oil extraction degreasing the body obtained by injection molding is placed in oil, and some organic binder is dissolved and dissolved.
  • the temperature of the oil is 30 ° C, the degreasing time is 24 hours, and the oil body after degreasing is in an oven. Fully dry, direct thermal release will cause the sample to break during the degreasing process.
  • the injection molding has a uniform grain size and a small particle size compared with that prepared by dry pressing, which is positively correlated with the final performance and stability of the BZN based dielectric resonator product. .
  • the main material formulation of this embodiment adopts the chemical formula: [0.3Ba(Zn 0.99 ⁇ 0.01 ) 1/3 (Nb 0.99 Mo 0.01 ) 2/3 O 3 +0.7Ba(Ni 0.7 Co 0.3 ) 1/3 Nb 2/3 O 3
  • the performance of the dielectric resonator prepared by the dry pressing method and the injection molding method is compared, and the dielectric property relative dielectric constant ⁇ r of the main material itself in this embodiment is 32, and the quality factor (Q ⁇ f) value is At 91200 GHz, the temperature coefficient ⁇ f of the resonant frequency is -2.5 ppm/°C.
  • the dry pressing method mainly obtains a dielectric resonator by granulation, press molding, and sintering, and the process is simple.
  • the BZN-based dielectric resonator prepared by the injection molding process is realized by the following process steps:
  • (1) Mixed ceramic powder and organic binder The BZN-based ceramic powder and the organic binder are uniformly mixed to obtain an injection molding mixture, and the content of different components in the mixture is related to the particle size, morphology and density of the powder. Therefore, different mixtures of different powder formulations; BZN group is directed to a dielectric ceramic, injection molding mix, the weight percentage of Ba 2 Ti 9 O 20 based ceramic powder was 75%, the weight percentage of organic binder It is 25%; the organic binder is composed of a binder, a surfactant and a plasticizer, and the weight percentage of each component is: binder 80%; surfactant 5%; plasticizer: 15%.
  • injection molding The injection molding mixture is injection-molded on an injection molding machine to obtain a green body, and the injection temperature is between 180 ° C. After injection into the mold, the mold is released in 2 minutes.
  • Oil extraction degreasing the body obtained by injection molding is placed in oil, and some organic binder is dissolved and dissolved.
  • the temperature of the oil is 30 ° C, the degreasing time is 24 hours, and the oil body after degreasing is in an oven. Fully dry, direct thermal release will cause the sample to break during the degreasing process.
  • the main material formulation of this embodiment adopts the chemical formula: [0.3Ba(Zn 0.99 ⁇ 0.01 ) 1/3 (Nb 0.99 Mo 0.01 ) 2/3 O 3 +0.7Ba(Ni 0.7 Co 0.3 ) 1/3 Nb 2/3 O 3 ] +0.5 mol% B 2 O 3 , comparing the performance of the dielectric resonator prepared by the dry pressing method and the injection molding method, respectively, the dielectric property relative dielectric constant ⁇ r of the main material itself in this example is 33, and the quality factor (Q)
  • the ⁇ f) value is 83,000 GHz, and the temperature coefficient ⁇ f of the resonance frequency is 0 ppm/°C.
  • the dry pressing method mainly obtains a dielectric resonator by granulation, press molding, and sintering, and the process is simple.
  • the BZN-based dielectric resonator prepared by the injection molding process is realized by the following process steps:
  • (1) Mixed ceramic powder and organic binder The BZN-based ceramic powder and the organic binder are uniformly mixed to obtain an injection molding mixture, and the content of different components in the mixture is related to the particle size, morphology and density of the powder. Therefore, the different powders have different mixture formulations; for the BZN-based dielectric ceramics, the BZN-based ceramic powder has a weight percentage of 75% and the organic binder has a weight percentage of 25%;
  • the binder is composed of a binder, a surfactant and a plasticizer, and the weight percentage of each component is: binder 80%; surfactant 5%; plasticizer: 15%.
  • injection molding The injection molding mixture is injection-molded on an injection molding machine to obtain a green body, and the injection temperature is between 180 ° C. After injection into the mold, the mold is released in 2 minutes.
  • Oil extraction degreasing the body obtained by injection molding is placed in oil, and some organic binder is dissolved and dissolved.
  • the temperature of the oil is 30 ° C, the degreasing time is 24 hours, and the oil body after degreasing is in an oven. Fully dry, direct thermal release will cause the sample to break during the degreasing process.
  • the main material formulation of this embodiment adopts a chemical formula: 0.5Ba(Ni 0.5 Co 0.5 ) 1/3 Nb 2/3 O 3 as a chemical composition, and the BZN-based dielectric resonator prepared by the injection molding process is realized by the following process steps:
  • BZN-based ceramic powder and organic binder are mixed on a mixer, and mixed for 4 minutes to obtain a uniformly mixed injection molding mixture, in the injection molding mixture,
  • the weight percentage of the BZN-based ceramic powder is 76%, and the weight percentage of the organic binder is 24%;
  • the organic binder is composed of a binder, a surfactant and a plasticizer, and the weight of each component is 100%.
  • the content of the fraction is: binder 50%; surfactant 5%; plasticizer: 22%.
  • injection molding The injection molding mixture was injection-molded on an injection molding machine to obtain a green body, and the injection temperature was 250 ° C. After injection into the mold, the molded body was released in 2 minutes.
  • Oil extraction degreasing the blank obtained by injection molding is placed in oil, and some organic binder is dissolved and dissolved, the temperature of the oil is 30 ° C, the degreasing time is 12 hours, and the oil body after degreasing is in an oven. It was dried at a temperature of 50 ° C for 12 hours to make it sufficiently dry, and direct heat removal caused the sample to be broken during the degreasing process.
  • the main material formulation of this embodiment adopts the chemical formula: [0.3Ba(Zn 0.99 ⁇ 0.01 ) 1/3 (Nb 0.99 Mo 0.01 ) 2/3 O 3 +0.7Ba(Ni 0.7 Co 0.3 ) 1/3 Nb 2/3 O 3
  • the BZN-based dielectric resonator prepared by the injection molding process is realized by the following process steps:
  • BZN-based ceramic powder and organic binder are mixed on a kneader, mixed for 8 minutes to obtain a uniformly mixed injection molding mixture, in the injection molding mixture,
  • the weight percentage of the BZN-based ceramic powder is 85%, and the weight percentage of the organic binder is 15;
  • the organic binder is composed of a binder, a surfactant and a plasticizer, and the weight percentage of each component
  • the content is: binder 90%; surfactant 1%; plasticizer: 3%.
  • injection molding The injection molding mixture was injection-molded on an injection molding machine to obtain a green body, and the injection temperature was 150 ° C. After injection into the mold, the molded body was released in 3 minutes.
  • Oil extraction degreasing the body obtained by injection molding is placed in oil, and some organic binder is dissolved and dissolved, the temperature of the oil is 40 ° C, the degreasing time is 36 hours, and the oil body after degreasing is in an oven. It was dried at 60 ° C for 8 hours to make it sufficiently dry. Direct heat removal caused the sample to break during the degreasing process.
  • Example formulations of the present embodiment uses the main material of the formula: [0.3Ba (Zn 0.99 ⁇ 0.01 ) 1/3 (Nb 0.99 Mo 0.01) 2/3 O 3 + 0.7Ba (Ni 0.7 Co 0.3) 1/3 Nb 2/3 O 3 ] +0.5 mol% B 2 O 3 is a chemical composition, and a BZN-based dielectric resonator prepared by an injection molding process is realized by the following process steps:
  • BZN-based ceramic powder and organic binder are mixed on a mixer, and mixed for 6 minutes to obtain a uniformly mixed injection molding mixture, in the injection molding mixture,
  • the weight percentage of the BZN-based ceramic powder is 80%, and the weight percentage of the organic binder is 15%;
  • the organic binder is composed of a binder, a surfactant and a plasticizer, and the weight of each component is 100%.
  • the content of the fraction is: binder 80%; surfactant 3%; plasticizer: 15%.
  • injection molding The injection molding mixture was injection-molded on an injection molding machine to obtain a green body, and the injection temperature was 200 ° C. After injection into the mold, the molded body was released in 5 minutes.
  • Oil extraction degreasing the body obtained by injection molding is placed in oil, and the organic part is dissolved and removed.
  • the temperature of the oil is 50 ° C
  • the degreasing time is 25 hours
  • the oil body after degreasing by oil extraction is dried in an oven at 70 ° C for 4 hours to make it fully dry, and the direct heat removal will cause the sample to be broken during the degreasing process. crack.
  • the preparation method of the bismuth-zinc-based germanium dielectric resonator provided by the embodiment of the invention can make the produced bismuth-zinc bismuth-based dielectric resonator have uniform density distribution and high dimensional precision, and also has high dielectric constant and high performance stability, and It also has high dielectric constant and performance stability.
  • large-scale production of zinc-silicon-based dielectric resonators with complex shapes can be realized by injection molding.
  • the present invention provides a dielectric resonator and a cavity filter which are produced by the production method of any of the above embodiments.
  • the technical features of the parameters such as the shape and structure of the resonant device are within the understanding of those skilled in the art, and are not described herein again.
  • the cavity filter includes the resonator in the above embodiment, and the cavity has a higher quality factor Q ⁇ f value and a lower temperature coefficient of resonance frequency ( ⁇ f), so that the cavity filter is prepared.
  • the device has better dielectric properties and stability. The technical features of the structure and parameters of other parts of the cavity filter are within the understanding of those skilled in the art, and are not described herein again.
  • FIG. 4 is a structural block diagram of a preferred embodiment of the radio remote device of the present invention.
  • the radio remote device includes but is not limited to the following structural units: a radio frequency transceiver module 510, a power amplifier module 520, and a cavity filter. 530.
  • the radio frequency transceiver module 510 is connected to the power amplifier module 520, and the power amplifier module 520 is further connected to the cavity filter 530.
  • the transmit signals from the two channels of the radio transceiver module 510 enter the cavity filter 530 through the power amplifier module 520, and the cavity filter 530 filters the transmit signal, and then the power is synthesized.
  • the RF remote device operates in the uplink time slot, and the signal received from the antenna port is filtered by the cavity filter 530 and then enters the power amplifier module 520, and is amplified by the power amplifier module 520 and output to the RF transceiver.
  • the receiving channel corresponding to module 510.
  • the radio remote device may further include a power module 540, and the power module 540 is configured to supply power to each module of the radio remote device.

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Abstract

本发明提供了一种陶瓷材料及其制备方法、谐振器、滤波器及射频拉远设备。该原料配方包括重量百分含量为76％-85％的钡锌铌基陶瓷粉体和15％-24％有机粘结剂；该制备方法包括以下步骤：将上述配方的钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料；加热混合物料以形成熔体；将熔体注射成型得到坯体；对坯体进行脱脂；对脱脂后的坯体进行烧结。本发明的钡锌铌基介质谐振器密度均匀、尺寸精度高，具有高介电常数和性能稳定性并可成型形状复杂的介质谐振器。

Description

陶瓷材料及其制备方法、谐振器、滤波器及射频拉远设备 【技术领域】
本发明涉及谐振器的制备技术领域，特别是涉及一种陶瓷材料及其制备方法、谐振器、滤波器及射频拉远设备。
【背景技术】
介质谐振器是一个最基本的微波元件，利用介质谐振器可以构成滤波器、振荡器和天线等微波电路，广泛应用于移动通讯、卫星通信、军用雷达、全球定位系统、蓝牙技术、无线局域网等现代通信中，是现代通信技术的关键基础器件。应用于微波电路的介质谐振器，除了必备的机械强度外，还需满足如下介电性能要求：(1)在微波频率下具有相对较高的介电常数εr，一般要求εr＞20，以便于微波器件小型化、集成化；(2)在微波谐振频率下具有极低的介电损耗，即很高的品质因数(Q×f)，以保证优良的选频特性和降低器件在高频下的插入损耗；(3)接近零的谐振频率温度系数(τf)，以保证器件在温度变化环境中谐振频率的高度稳定性。
钡锌铌陶瓷(Ba(Zn1/3Nb2/3)O3，BZN)具有复合钙钛矿结构，是一种在X波段(7～8GHz)Q值很高的微波介质陶瓷，它是卫星通讯等微波高频领域中极其重要的介质材料。然而，BZN陶瓷具有相对高的τf值(～30ppm/℃)限制了其实际应用。至今已有许多研究者通过探索各种不同的化学配方来降低BZN的τf值到零。比如，在固溶物(1-x)Ba(Zn1/3Nb2/3)O3-xSr(Zn1/3Nb2/3)O3中用部分Sr取代Ba实现τf值为零，此时x＝0.7，然而随着τf值的降低Qf值也随之变小。降低τf的研究也在(1-x)Ba(Zn1/3Nb2/3)O3-(x)Ba(Ni1/3Nb2/3)O3(BZN-BNN)和(1-x)Ba(Zn1/3Nb2/3)O3-(x)Ba(Co1/3Nb2/3)O3(BZN-BCoN)系统中进行。纯相Ba(Co1/3Nb2/3)O3在1425℃发生结构转变，从1：2有序结构转变成无序 结构，其转变温度要比纯BZN稍高(～1375℃)。所以，通过1300～1400℃长时间退火处理在BZN-BCoN中形成有序固溶相；尽管文献上所报道的τf为零的成分值不太一致，从x＝0.4到x＝0.7。Ba(Ni1/3Nb2/3)O3的无序化温度文献上存在相矛盾的值，从1400℃变化到＞1500℃。该相的X射线图谱通常存在二次杂相，可能与高温下NiO部分熔解或挥发有关。传统固相法组分混合不均匀和高温下Ni的挥发可能是该系统有序性不一致的原因。对于(1-x)BZN-xBNN其tf为零的成分值为x＝0.7，该陶瓷在1500℃烧结致密，Q值为～5700(10GHz)。
虽然注射成型的研究和应用在不断的发展，从聚合物到金属再到陶瓷(主要应用于结构陶瓷，氧化铝、氧化锆等)。但对于钡锌铌基介质陶瓷谐振器的注射成型研究和生产几乎没有。现有技术中的成型工艺主要是干压成型。干压成型的原理是：对介质陶瓷粉末加粘结剂造粒、通过模具进行压制成型后进行烧结。此工艺制备介质谐振器存在如下缺点：(1)压制成型过程中，颗粒间以及颗粒与模壁间存在的内、外摩擦引起压力损失使压坯各部位受力不均，因此生坯、烧结样品密度分布不均匀。不均匀的程度与选用的压制方式有关，常用的压制方式有单向压制和双向压制，其密度分布情况如图1a和1b所示，密度的均匀性会影响介质谐振器的介电性能，进而也会影响滤波器的工作性能；(2)受限于压制方式，介质谐振器大部分是柱状(或类似形状)，并不是所有形状尺寸能用干压法进行制备，比如形状复杂的谐振器脱模难以实现，长径比大的谐振器也无法通过压制制得，因为容易因密度不均匀而出现低密度区，进而导致烧结过程中谐振器变形，制作精度差，为了得到想要的形状或尺寸还需要进行机加工获得。
综上所述，现有技术中通常采用的干压法制备的微波介质陶瓷，存在所制备微波介质陶瓷材料谐振器的密度不均匀，导致微波介质陶瓷材料谐振器介电性能较差；同时，干压法无法制备形状复杂的谐振器。
【发明内容】
本发明提供一种陶瓷材料及其制备方法、谐振器、滤波器及射频拉远设备， 能够解决现有技术中钡锌铌基介质谐振器在干压成型过程中容易出现的密度分布不均匀、尺寸精度低、品质因数Q×f值较低、性能不稳定以及所能制备的成型形状有限的问题。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种钡锌铌基介质谐振器的原料配方，该原料配方包括以下重量百分含量的组分：
钡锌铌基陶瓷粉体  76％-85％；
有机粘结剂        15％-24％。
其中，所述有机粘结剂包括粘结剂、表面活性剂和增塑剂；所述粘结剂在所述有机粘结剂中的重量百分比为50％-90％；所述表面活性剂在所述有机粘结剂中的重量百分比为1％-5％；所述增塑剂在所述有机粘结剂中的重量百分比为3％-22％。
其中，所述粘结剂选自石蜡、乙烯-乙酸乙烯脂共聚物、聚丙烯、无规聚丙烯、聚苯乙烯、聚甲基丙烯酸酯和乙烯丙烯酸乙酯共聚物中的至少一种。
其中，所述表面活性剂选自硬脂酸、辛酸和微晶石蜡中的至少一种。
其中，所述增塑剂为低熔点增塑剂。
其中，所述增塑剂选自邻苯二甲酸二丁酯、邻苯二甲酸二乙酯和邻苯二甲酸二辛脂中的至少一种。
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种钡锌铌基介质谐振器的制备方法，该制备方法包括以下步骤：将钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料，其中，所述钡锌铌基陶瓷粉体的重量百分含量为76％-85％，所述有机粘结剂的重量百分含量为15％-24％；对所述混合物料加热，以使所述混合物料形成熔体；使用注射成型机将所述熔体注射成型得到坯体；对所述坯体进行脱脂，以脱除有机粘结剂；对脱脂后的坯体进行烧结以获得介质谐振器。
其中，将钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料的步骤中，所述钡锌铌基陶瓷粉体与所述有机粘结剂在混炼机上进行混合，混合时间为4-8 小时。
其中，将所述混合物料加热，以使所述混合物料形成熔体的步骤中，所述加热温度为150℃-250℃。
其中，使用注射成型机将所述熔体注射成型得到坯体的步骤中，将所述熔体注入金属模具中，2-5分钟后冷却脱模得到所述坯体。
其中，对所述坯体进行脱脂的步骤包括：对所述坯体进行油萃取脱脂；对油萃取脱脂后的所述坯体进行热脱脂。
其中，对所述坯体进行油萃取脱脂的步骤包括：将所述坯体放入非极性溶剂中，所述非极性溶剂的温度为30-50℃，脱脂时间12-36小时；将所述坯体从非极性溶剂中取出，并置于烘箱中进行干燥，其中，干燥温度为50-70℃，干燥时间4-12小时。
其中，所述非极性溶剂选自汽油、二硫化碳、二甲苯、乙醚、苯、氯仿、四氯化碳和石脑油中的至少一种。
其中，对油萃取脱脂后的所述坯体进行热脱脂的步骤中，将所述坯体置于电加热炉内，以0.5-5℃/min的升温速率升温至500-600℃，保温2-3小时。
其中，对热脱脂后的坯体进行烧结以获得介质谐振器的步骤中，所述烧结温度为900-1400℃，保温2-6小时。
其中，所述有机粘结剂包括粘结剂、表面活性剂和增塑剂；所述粘结剂在所述有机粘结剂中的重量百分比为50％-90％；所述表面活性剂在所述有机粘结剂中的重量百分比为1％-5％；所述增塑剂在所述有机粘结剂中的重量百分比为3％-22％。
为解决上述技术问题，本发明采用的又一个技术方案是：提供一种钡锌铌基介质谐振器，其特征在于，该介质谐振器通过以下制备方法制得：将钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料，其中，所述钡锌铌基陶瓷粉体的重量百分含量为76％-85％，所述有机粘结剂的重量百分含量为15％-24％；对所述混合物料加热，以使所述混合物料形成熔体；使用注射成型机将所述熔体 注射成型得到坯体；对所述坯体进行脱脂，以脱除有机粘结剂；对脱脂后的坯体进行烧结以获得介质谐振器。
其中，所述有机粘结剂包括粘结剂、表面活性剂和增塑剂；所述粘结剂在所述有机粘结剂中的重量百分比为50％-90％；所述表面活性剂在所述有机粘结剂中的重量百分比为1％-5％；所述增塑剂在所述有机粘结剂中的重量百分比为3％-22％。
其中，对所述坯体进行脱脂的步骤包括：对所述坯体进行油萃取脱脂；对油萃取脱脂后的所述坯体进行热脱脂。
其中，对所述坯体进行油萃取脱脂的步骤包括：将所述坯体放入非极性溶剂中，所述非极性溶剂的温度为30-50℃，脱脂时间12-36小时；将所述坯体从非极性溶剂中取出，并置于烘箱中进行干燥，其中，干燥温度为50-70℃，干燥时间4-12小时。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种腔体滤波器，所述腔体滤波器包括腔体、盖板以及上述实施例中所述的介质谐振器，所述盖板封盖所述腔体以形成谐振腔，所述介质谐振器安装在所述腔体内。
为解决上述技术问题，本发明还采用的一个技术方案是：提供一种射频拉远设备，所述射频拉远设备包括：射频收发信机模块、功放模块以及第四方面所述的腔体滤波器，所述射频收发信机模块与所述功放模块连接，所述功放模块与所述腔体滤波器连接。
本发明的有益效果是：区别于现有技术的情况，本发明的钡锌铌基介质谐振器及其原料配方和制备方法，通过添加较多的有机粘结剂，使钡锌铌基陶瓷粉体和有机粘结剂的混合物料在加热后形成粘稠性熔体，从而可以通过注射成型的方法形成介质谐振器，因而可以得到密度分布均匀、尺寸精度高的介质谐振器，且材料成本低，制备工艺简单。并且还具有高品质因数Q×f值和性能稳定性，本发明注射成型制备的钡锌铌基介质谐振器Q值为20000～26000左右(高于干压成型的15000～25000)，另外，通过注射成型可以实现形状复杂的钡锌铌 基介质谐振器的大批量生产。
【附图说明】
图1a是干压法中的单向压制制备样品的密度分布图；
图1b是干压法中的双向压制制备样品的密度分布图；
图2是本发明钡锌铌基介质谐振器的制备方法实施例的流程示意图；
图3a是干压成型制备的钡锌铌基介质谐振器端口腐蚀后的电子显微镜扫描图；
图3b是注射成型制备的钡锌铌基介质谐振器端口腐蚀后的电子显微镜扫描图；以及
图4是本发明射频拉远设备一优选实施例的结构组成框图。
【具体实施方式】
下面结合附图和实施例对本发明进行详细说明。
本发明提供了一种钡锌铌基介质谐振器的成型原料配方，该成型原料配方包括以下重量百分含量的组分：76％-85％的钡锌铌基陶瓷粉体和15％-24％的有机粘结剂。
本发明的介质谐振器的成型原料配方中，有机粘结剂的重量百分比含量为15％-24％，传统的介质谐振器的压制成型原料配方中，有机粘结剂的重量百分比含量为5％以下，相比较与干压成型的原料配方而言，本发明中的有机粘结剂的重量百分比含量较多，含量较多的有机粘结剂能够使得钡锌铌基陶瓷粉体和有机粘结剂的混合物料在加热后能形成粘稠性熔体，因而使本发明的成型原料配方可以通过注射成型的方式形成介质谐振器。
具体而言，钡锌铌基复合微波介质陶瓷的化学表达式为：
[(1-x)Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+xBa(Ni1-yCoy)1/3Nb2/3O3]+aB2O3+bCuO，其中□表示原子空位，0≤x≤0.7，0≤y≤1.0，0≤a≤0.5mol％，0≤b≤1.0mol％。
本实施例的有机粘结剂包括粘结剂、表面活性剂和增塑剂。
其中，粘结剂主要用于将钡锌铌基陶瓷粉体粘结起来，该粘结剂在有机粘结剂中的重量百分比为50％-90％，粘结剂选自石蜡、乙烯-乙酸乙烯脂共聚物、聚丙烯、无规聚丙烯、聚苯乙烯、聚甲基丙烯酸酯和乙烯丙烯酸乙酯共聚物中的至少一种。
表面活性剂选自硬脂酸、辛酸和微晶石蜡中的至少一种，表面活性剂在有机粘结剂中的重量百分比为1％-5％。
增塑剂在有机粘结剂中的重量百分比为3％-22％，增塑剂的作用是增加柔韧性以及增加粘度，在本实施例中，增塑剂为低熔点增塑剂，从而可以在较低的温度下熔化，以与熔化的混合物料混合均匀。具体地，增塑剂选自邻苯二甲酸二丁酯、邻苯二甲酸二乙酯和邻苯二甲酸二辛脂中的至少一种。
举例而言，在一个实施例中，介质谐振器的成型原料配方中的钡锌铌基陶瓷粉体的重量百分含量为76％，有机粘结剂的重量百分含量为24％。
具体地，在有机粘结剂中，粘结剂的重量百分比为50％，表面活性剂的重量百分比为5％，增塑剂的重量百分比为22％。
在另一个实施例中，介质谐振器的成型原料配方中的钡锌铌基陶瓷粉体的重量百分含量为85％，有机粘结剂的重量百分含量为15％。
具体地，在有机粘结剂中，粘结剂的重量百分比为90％，表面活性剂的重量百分比为1％，增塑剂的重量百分比为3％。
在另一个实施例中，介质谐振器的成型原料配方中的钡锌铌基陶瓷粉体的重量百分含量为80％，有机粘结剂的重量百分含量为20％。
具体地，在有机粘结剂中，粘结剂的重量百分比为80％，表面活性剂的重量百分比为3％，增塑剂的重量百分比为15％。
区别于现有技术的情况，本发明的钡锌铌基介质谐振器及其原料配方和制备方法，通过添加较多的有机粘结剂，使钡锌铌基陶瓷粉体和有机粘结剂的混合物料在加热后形成粘稠性熔体，从而可以通过注射成型的方法形成介质谐振 器，因而可以得到密度分布均匀、尺寸精度高的介质谐振器，且材料成本低，制备工艺简单。
本发明还提供了一种钡锌铌基介质谐振器的制备方法。请参阅图2，图2是本发明钡锌铌基介质谐振器的制备方法实施例的流程示意图，具体地，该制备方法包括以下步骤：
S101、将钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料，其中，钡锌铌基陶瓷粉体的重量百分含量为76％-85％，有机粘结剂的重量百分含量为15％-24％。
具体地，该钡锌铌基介质陶瓷的化学表达式为：
[(1-x)Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+xBa(Ni1-yCoy)1/3Nb2/3O3]+aB2O3+bCuO，其中□表示原子空位，0≤x≤0.7，0≤y≤1.0，0≤a≤0.5mol％，0≤b≤1.0mol％。
钡锌铌基的配方确定主要通过固相法制备进行研究，在配好料之后，首先经过球磨，球磨介质为氧化锆球，球磨时间为4-12小时。然后进行煅烧，煅烧温度为1000℃-1200℃。然后对煅烧好的粉末放入球磨机进行球磨，此次球磨的介质仍然是氧化锆球，球磨时间仍为4-12小时，并且，在球磨过程中加入2％-5％的PVA粘结剂。然后在喷雾塔上进行造粒，再将造粒粉末放入模具进行压制成型，压力为100MPa-200MPa，压制成型之后再烧结测试材料本身性能，从而得到所需要的介质材料--钡锌铌基陶瓷粉体。
本实施例的有机粘结剂包括粘结剂、表面活性剂和增塑剂。其中，粘结剂主要用于将钡锌铌基陶瓷粉体粘结起来，该粘结剂在有机粘结剂中的重量百分比为50％-90％，粘结剂选自石蜡、乙烯-乙酸乙烯脂共聚物、聚丙烯、无规聚丙烯、聚苯乙烯、聚甲基丙烯酸酯和乙烯丙烯酸乙酯共聚物中的至少一种。
表面活性剂选自硬脂酸、辛酸和微晶石蜡中的至少一种，表面活性剂在有机粘结剂中的重量百分比为1％-5％。
增塑剂在有机粘结剂中的重量百分比为3％-22％，增塑剂的作用是增加柔韧性以及增加粘度，在本实施例中，增塑剂为低熔点增塑剂，从而可以在较低的 温度下熔化，以与熔化的混合物料混合均匀。具体地，增塑剂选自邻苯二甲酸二丁酯、邻苯二甲酸二乙酯和邻苯二甲酸二辛脂中的至少一种。
在该步骤中，钡锌铌基陶瓷粉体和有机粘结剂的混合在混炼机上进行，混合时间4-8小时。
S102、对混合物料加热，以使混合物料形成熔体。
由于混合物料中的有机粘结剂的含量较多，因而步骤S102中形成的熔体具有粘稠性，利于后续注射成型。其中，加热的温度为150℃-250℃。
S103、使用注射成型机将熔体注射成型得到坯体。
步骤S103中，将熔体注入注射成型机的金属模具中，2-5分钟后冷却脱模得到坯体。本步骤通过注射成型的方式来形成介质谐振器，可以实现密度分布均匀、尺寸精度高、形状复杂的钡锌铌基介质谐振器的大批量生产。
S104、对坯体进行脱脂，以脱除有机粘结剂。
步骤S104中，将坯体中的有机粘结剂脱除，以防止有机粘结剂对介质谐振器的功效产生影响。脱脂的步骤具体包括将坯体先后进行非极性溶剂萃取脱脂和热脱脂。
其中，非极性容积萃取脱脂过程如下：将注射成型得到的坯体放入汽油、二硫化碳、二甲苯、乙醚、笨、氯仿、四氯化碳、石脑油等非极性溶剂中，以溶解脱除部分有机粘结剂，非极性溶剂的温度为30-50℃，脱脂时间为12-36小时，再将坯体从非极性溶剂中取出，并置于烘箱中进行干燥，干燥温度为50-70℃，干燥时间为4-12小时。该步骤中的非极性溶剂萃取脱脂过程是非常必要的，因为如果直接进行热脱会由于胚体中有机粘结剂成分过高，而导致样品在脱脂过程中的碎裂。
热脱脂的过程如下：将干燥后的坯体放入电加热炉内进行热脱脂，以脱除剩余的有机粘结剂。该过程中，将胚体以0.5～5℃/min的升温速率升温至550℃，然后保温2～3小时。
S105、对脱脂后的坯体进行烧结以获得介质谐振器。
在步骤S105中，烧结温度在900-1400℃之间，保温2-6小时。
分别用干压法和注射成型方法制备BZN基材料的介质谐振器，干压法制备的介质谐振器Q值为15000～25000，频率为2.3～2.6G，注射成型制备的介质谐振器Q值为20000～26000左右，频率为2.3～2.7G(注：是以同一批制备的样品(60个)作为检查和对比数据)。注射成型制备的介质谐振器性能更为稳定。
相对于现有技术，本发明提供的钡锌铌基介质谐振器的制备方法，能够使得生产的钡锌铌基介质谐振器密度分布均匀、尺寸精度高，同时还具备高介电常数和高性能稳定性，并且还具有高介电常数和性能稳定性，另外，通过注射成型可以实现形状复杂的钡锌铌基介质谐振器的大批量生产。
注射成型工艺具有以下优势：(1)成型过程具有机械化和自动化程度高、生产效率高、成型周期短、坯体强度高，生产过程中的管理和控制方便，易于实现大批量、规模化生产；(2)可近净成形各种几何形状复杂的及有特殊要求的小型零部件，使烧结后的陶瓷产品无需进行机加工或少加工；(3)成型出的产品具有极高的尺寸精度和表面光洁度。
下面几个具体实施例来详细说明本发明中钡锌铌基介质谐振器件制作过程和成品谐振器件的性能参数。
实施例一
本实施例主材料配方采用化学式：0.5Ba(Ni0.5Co0.5)1/3Nb2/3O3为化学组成，分别比较干压法和注射成型法制备的介质谐振器的性能，本实施例主材料本身的介电性能相对介电常数εr为35，品质因数(Q×f)值为100800GHz，谐振频率温度系数τf为+4.8ppm/℃。干压法主要通过造粒、压制成型后，进行烧结得到介质谐振器，工艺简单。注射成型工艺制备BZN基介质谐振器通过以下工艺步骤实现：
(1)混合陶瓷粉体和有机粘结剂：将BZN基陶瓷粉体和有机粘结剂混合均匀得到注射成型混合料，混料中不同成分的含量跟粉末的粒度、形貌、密度有关，所以不同的粉末其混合物配方不同；针对于BZN基介质陶瓷，注射成型 混合料中，BZN基陶瓷粉体的重量百分含量为78％，有机粘结剂的重量百分含量为22％；有机粘结剂由粘结剂、表面活性剂和增塑剂组成，各组分重量百分含量为：粘结剂80％；表面活性剂5％；增塑剂：15％。
(2)注射成型：注射成型混合料在注射成型机上注射成型得到坯体，注射温度为180℃，注入模具后在2分钟内脱模得到成型坯体。
(3)油萃取脱脂：将注射成型得到的坯体放入油中，溶解脱除部分有机粘结剂，油的温度在30℃，脱脂时间在24小时，油萃取脱脂后的坯体在烘箱中充分干燥，直接热脱会导致样品在脱脂过程中碎裂。
(4)热脱脂：将干燥后的坯体放入电加热炉内，进行热脱脂，脱除剩余的有机粘结剂，以0.5℃/min的升温速率升温至550℃，保温2小时。
(5)烧结：热脱脂后的坯体进行烧结，烧结温度为1300℃，保温2小时，得到介质谐振器。
分别用干压和注射成型工艺制备60个介质谐振器，并对他们的性能进行了测试，性能如表1：
Figure PCTCN2015099954-appb-000001
表1：注射成型和干压成型制备介质谐振器的性能
从表1可以看出注射成型制备的介质谐振器比传统干压法制备的性能更优，且性能稳定。
从图3a和图3b中可以看出，注射成型与干压成型法制备的相比，晶粒尺寸均匀，颗粒尺寸小，这对于BZN基介质谐振器产品最终的性能和稳定性影响呈正相关关系。
实施例二
本实施例主材料配方采用化学式：[0.3Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3]为化学组成，分别比较干压法和注射成型法制备的介 质谐振器的性能，本实施例主材料本身的介电性能相对介电常数εr为32，品质因数(Q×f)值为91200GHz，谐振频率温度系数τf为-2.5ppm/℃。干压法主要通过造粒、压制成型后，进行烧结得到介质谐振器，工艺简单。注射成型工艺制备BZN基介质谐振器通过以下工艺步骤实现：
(1)混合陶瓷粉体和有机粘结剂：将BZN基陶瓷粉体和有机粘结剂混合均匀得到注射成型混合料，混料中不同成分的含量跟粉末的粒度、形貌、密度有关，所以不同的粉末其混合物配方不同；针对于BZN基介质陶瓷，注射成型混合料中，Ba2Ti9O20基陶瓷粉体的重量百分含量为75％，有机粘结剂的重量百分含量为25％；有机粘结剂由粘结剂、表面活性剂和增塑剂组成，各组分重量百分含量为：粘结剂80％；表面活性剂5％；增塑剂：15％。
(2)注射成型：注射成型混合料在注射成型机上注射成型得到坯体，注射温度在180℃之间，注入模具后在2分钟内脱模得到成型坯体。
(3)油萃取脱脂：将注射成型得到的坯体放入油中，溶解脱除部分有机粘结剂，油的温度在30℃，脱脂时间在24小时，油萃取脱脂后的坯体在烘箱中充分干燥，直接热脱会导致样品在脱脂过程中碎裂。
(4)热脱脂：将干燥后的坯体放入电加热炉内，进行热脱脂，脱除剩余的有机粘结剂，以0.5℃/min的升温速率升温至550℃，保温2小时。
(5)烧结：热脱脂后的坯体进行烧结，烧结温度为1280℃，保温4小时，得到介质谐振器。
分别用干压和注射成型工艺制备60个介质谐振器，并对他们的性能进行了测试，性能如表2：
Figure PCTCN2015099954-appb-000002
表2：注射成型和干压成型制备介质谐振器的性能
从表2可以看出注射成型制备的介质谐振器比传统干压法制备的性能更优， 且性能稳定。
实施例三
本实施例主材料配方采用化学式：[0.3Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3]+0.5mol％B2O3，分别比较干压法和注射成型法制备的介质谐振器的性能，本实施例主材料本身的介电性能相对介电常数εr为33，品质因数(Q×f)值为83000GHz，谐振频率温度系数τf为0ppm/℃。干压法主要通过造粒、压制成型后，进行烧结得到介质谐振器，工艺简单。注射成型工艺制备BZN基介质谐振器通过以下工艺步骤实现：
(1)混合陶瓷粉体和有机粘结剂：将BZN基陶瓷粉体和有机粘结剂混合均匀得到注射成型混合料，混料中不同成分的含量跟粉末的粒度、形貌、密度有关，所以不同的粉末其混合物配方不同；针对于BZN基介质陶瓷，注射成型混合料中，BZN基陶瓷粉体的重量百分含量为75％，有机粘结剂的重量百分含量为25％；有机粘结剂由粘结剂、表面活性剂和增塑剂组成，各组分重量百分含量为：粘结剂80％；表面活性剂5％；增塑剂：15％。
(2)注射成型：注射成型混合料在注射成型机上注射成型得到坯体，注射温度在180℃之间，注入模具后在2分钟内脱模得到成型坯体。
(3)油萃取脱脂：将注射成型得到的坯体放入油中，溶解脱除部分有机粘结剂，油的温度在30℃，脱脂时间在24小时，油萃取脱脂后的坯体在烘箱中充分干燥，直接热脱会导致样品在脱脂过程中碎裂。
(4)热脱脂：将干燥后的坯体放入电加热炉内，进行热脱脂，脱除剩余的有机粘结剂，以0.5℃/min的升温速率升温至550℃，保温2小时。
(5)烧结：热脱脂后的坯体进行烧结，烧结温度为1100℃，保温3小时，得到介质谐振器。
分别用干压和注射成型工艺制备60个介质谐振器，并对他们的性能进行了测试，性能如表3：
Figure PCTCN2015099954-appb-000003
Figure PCTCN2015099954-appb-000004
表3：注射成型和干压成型制备介质谐振器的性能
从表3可以看出注射成型制备的介质谐振器比传统干压法制备的性能更优，且性能稳定。
实施例四
本实施例主材料配方采用化学式：0.5Ba(Ni0.5Co0.5)1/3Nb2/3O3为化学组成，注射成型工艺制备BZN基介质谐振器通过以下工艺步骤实现：
(1)混合陶瓷粉体和有机粘结剂：将BZN基陶瓷粉体和有机粘结剂在混炼机上进行混合，混合4分钟得到混合均匀的注射成型混合料，该注射成型混合料中，BZN基陶瓷粉体的重量百分含量为76％，有机粘结剂的重量百分含量为24％；有机粘结剂由粘结剂、表面活性剂和增塑剂组成，各组分重量百分含量为：粘结剂50％；表面活性剂5％；增塑剂：22％。
(2)注射成型：注射成型混合料在注射成型机上注射成型得到坯体，注射温度为250℃，注入模具后在2分钟内脱模得到成型坯体。
(3)油萃取脱脂：将注射成型得到的坯体放入油中，溶解脱除部分有机粘结剂，油的温度在30℃，脱脂时间12小时，油萃取脱脂后的坯体在烘箱中，50℃的温度下干燥12小时，使其充分干燥，直接热脱会导致样品在脱脂过程中碎裂。
(4)热脱脂：将干燥后的坯体放入电加热炉内，进行热脱脂，脱除剩余的有机粘结剂，以0.5℃/min的升温速率升温至500℃，保温3小时。
(5)烧结：热脱脂后的坯体进行烧结，烧结温度为900℃，保温6小时，得到介质谐振器。
实施例五
本实施例主材料配方采用化学式：[0.3Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3]为化学组成，注射成型工艺制备BZN基介质谐振器通过以下工艺步骤实现：
(1)混合陶瓷粉体和有机粘结剂：将BZN基陶瓷粉体和有机粘结剂在混炼机上进行混合，混合8分钟得到混合均匀的注射成型混合料，该注射成型混合料中，BZN基陶瓷粉体的重量百分含量为85％，有机粘结剂的重量百分含量为15；有机粘结剂由粘结剂、表面活性剂和增塑剂组成，各组分重量百分含量为：粘结剂90％；表面活性剂1％；增塑剂：3％。
(2)注射成型：注射成型混合料在注射成型机上注射成型得到坯体，注射温度为150℃，注入模具后在3分钟内脱模得到成型坯体。
(3)油萃取脱脂：将注射成型得到的坯体放入油中，溶解脱除部分有机粘结剂，油的温度在40℃，脱脂时间36小时，油萃取脱脂后的坯体在烘箱中，60℃的温度下干燥8小时，使其充分干燥，直接热脱会导致样品在脱脂过程中碎裂。
(4)热脱脂：将干燥后的坯体放入电加热炉内，进行热脱脂，脱除剩余的有机粘结剂，以3℃/min的升温速率升温至550℃，保温2.5小时。
(5)烧结：热脱脂后的坯体进行烧结，烧结温度为1400℃，保温2小时，得到介质谐振器。
实施例六
本实施例主材料配方采用化学式：[0.3Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3]+0.5mol％B2O3为化学组成，注射成型工艺制备BZN基介质谐振器通过以下工艺步骤实现：
(1)混合陶瓷粉体和有机粘结剂：将BZN基陶瓷粉体和有机粘结剂在混炼机上进行混合，混合6分钟得到混合均匀的注射成型混合料，该注射成型混合料中，BZN基陶瓷粉体的重量百分含量为80％，有机粘结剂的重量百分含量为15％；有机粘结剂由粘结剂、表面活性剂和增塑剂组成，各组分重量百分含量为：粘结剂80％；表面活性剂3％；增塑剂：15％。
(2)注射成型：注射成型混合料在注射成型机上注射成型得到坯体，注射温度为200℃，注入模具后在5分钟内脱模得到成型坯体。
(3)油萃取脱脂：将注射成型得到的坯体放入油中，溶解脱除部分有机粘 结剂，油的温度在50℃，脱脂时间25小时，油萃取脱脂后的坯体在烘箱中，70℃的温度下干燥4小时，使其充分干燥，直接热脱会导致样品在脱脂过程中碎裂。
(4)热脱脂：将干燥后的坯体放入电加热炉内，进行热脱脂，脱除剩余的有机粘结剂，以5℃/min的升温速率升温至600℃，保温2小时。
(5)烧结：热脱脂后的坯体进行烧结，烧结温度为1200℃，保温4小时，得到介质谐振器。
本发明实施例提供的钡锌铌基介质谐振器的制备方法，能够使得生产的钡锌铌基介质谐振器密度分布均匀、尺寸精度高，同时还具备高介电常数和高性能稳定性，并且还具有高介电常数和性能稳定性，另外，通过注射成型可以实现形状复杂的钡锌铌基介质谐振器的大批量生产。
另外，本发明还提供了一种介质谐振器和一种腔体滤波器，该介质谐振器由上述任一实施例的制备方法制得。而关于谐振器件形状、结构等参数的技术特征在本领域技术人员的理解范围内，此处不再赘述。
腔体滤波器则包括上述实施例中的谐振器，由该谐振器具有较高的品质因数Q×f值和较低的谐振频率温度系数(τf)等优点，使之制备得到的腔体滤波器具有较佳的介电性能和稳定性。而关于腔体滤波器的其他部分的结构及参数的技术特征在本领域技术人员的理解范围内，此处不再赘述。
请参阅图4，图4是本发明射频拉远设备一优选实施例的结构组成框图，该射频拉远设备包括但不限于以下结构单元：射频收发信机模块510、功放模块520以及腔体滤波器530。其中，射频收发信机模块510与功放模块520连接，功放模块520进一步与腔体滤波器530连接。
射频拉远设备工作在下行时隙时，来自射频收发信机模块510的两个通道的发射信号通过功放模块520进入腔体滤波器530，腔体滤波器530对发射信号完成滤波，然后功率合成后发射到天线口；射频拉远设备工作在上行时隙时，从天线口接收到的信号通过腔体滤波器530滤波后进入功放模块520，在经功放模块520放大后输出给射频收发信机模块510对应的接收通道。
进一步地，该射频拉远设备还可以包括电源模块540，该电源模块540用于对该射频拉远设备的各个模块供电。
以上所述仅为本发明的部分实施例，并非因此限制本发明的保护范围，凡是利用本发明说明书及附图内容所作的等效装置或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (22)

  1. 一种钡锌铌基介质陶瓷材料的原料配方，其特征在于，包括以下重量百分含量的组分：
    钡锌铌基陶瓷粉体  76％-85％；
    有机粘结剂        15％-24％。
  2. 根据权利要求1所述的原料配方，其特征在于，所述有机粘结剂包括粘结剂、表面活性剂和增塑剂；
    所述粘结剂在所述有机粘结剂中的重量百分比为50％-90％；
    所述表面活性剂在所述有机粘结剂中的重量百分比为1％-5％；
    所述增塑剂在所述有机粘结剂中的重量百分比为3％-22％。
  3. 根据权利要求2所述的原料配方，其特征在于，所述粘结剂选自石蜡、乙烯-乙酸乙烯脂共聚物、聚丙烯、无规聚丙烯、聚苯乙烯、聚甲基丙烯酸酯和乙烯丙烯酸乙酯共聚物中的至少一种。
  4. 根据权利要求3所述的原料配方，其特征在于，所述表面活性剂选自硬脂酸、辛酸和微晶石蜡中的至少一种。
  5. 根据权利要求4所述的原料配方，其特征在于，所述增塑剂为低熔点增塑剂。
  6. 根据权利要求5所述的原料配方，其特征在于，所述增塑剂选自邻苯二甲酸二丁酯、邻苯二甲酸二乙酯和邻苯二甲酸二辛脂中的至少一种。
  7. 一种钡锌铌基介质陶瓷材料的制备方法，其特征在于，包括以下步骤：
    将钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料，其中，所述钡锌铌基陶瓷粉体的重量百分含量为76％-85％，所述有机粘结剂的重量百分含量为15％-24％；
    对所述混合物料加热，以使所述混合物料形成熔体；
    使用注射成型机将所述熔体注射成型得到坯体；
    对所述坯体进行脱脂，以脱除有机粘结剂；
    对脱脂后的坯体进行烧结以获得介质谐振器。
  8. 根据权利要求7所述的制备方法，其特征在于，将钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料的步骤中，所述钡锌铌基陶瓷粉体与所述有机粘结剂在混炼机上进行混合，混合时间为4-8小时。
  9. 根据权利要求8所述的制备方法，其特征在于，将所述混合物料加热，以使所述混合物料形成熔体的步骤中，所述加热温度为150℃-250℃。
  10. 根据权利要求9所述的制备方法，其特征在于，使用注射成型机将所述熔体注射成型得到坯体的步骤中，将所述熔体注入金属模具中，2-5分钟后冷却脱模得到所述坯体。
  11. 根据权利要求10所述的制备方法，其特征在于，对所述坯体进行脱脂的步骤包括：
    对所述坯体进行油萃取脱脂；
    对油萃取脱脂后的所述坯体进行热脱脂。
  12. 根据权利要求11所述的制备方法，其特征在于，对所述坯体进行油萃取脱脂的步骤包括：
    将所述坯体放入非极性溶剂中，所述非极性溶剂的温度为30-50℃，脱脂时间12-36小时；
    将所述坯体从非极性溶剂中取出，并置于烘箱中进行干燥，其中，干燥温度为50-70℃，干燥时间4-12小时。
  13. 根据权利要求12所述的制备方法，其特征在于，所述非极性溶剂选自汽油、二硫化碳、二甲苯、乙醚、苯、氯仿、四氯化碳和石脑油中的至少一种。
  14. 根据权利要求13所述的制备方法，其特征在于，对油萃取脱脂后的所述坯体进行热脱脂的步骤中，将所述坯体置于电加热炉内，以0.5-5℃/min的升温速率升温至500-600℃，保温2-3小时。
  15. 根据权利要求14所述的制备方法，其特征在于，对热脱脂后的坯体进 行烧结以获得介质谐振器的步骤中，所述烧结温度为900-1400℃，保温2-6小时。
  16. 根据权利要求15所述的制备方法，其特征在于，所述有机粘结剂包括粘结剂、表面活性剂和增塑剂；
    所述粘结剂在所述有机粘结剂中的重量百分比为50％-90％；
    所述表面活性剂在所述有机粘结剂中的重量百分比为1％-5％；
    所述增塑剂在所述有机粘结剂中的重量百分比为3％-22％。
  17. 一种钡锌铌基介质谐振器，其特征在于，该介质谐振器通过以下制备方法制得：
    将钡锌铌基陶瓷粉体和有机粘结剂混合以获得混合物料，其中，所述钡锌铌基陶瓷粉体的重量百分含量为76％-85％，所述有机粘结剂的重量百分含量为15％-24％；
    对所述混合物料加热，以使所述混合物料形成熔体；
    使用注射成型机将所述熔体注射成型得到坯体；
    对所述坯体进行脱脂，以脱除有机粘结剂；
    对脱脂后的坯体进行烧结以获得介质谐振器。
  18. 根据权利要求17所述的钡锌铌基介质谐振器，其特征在于，所述有机粘结剂包括粘结剂、表面活性剂和增塑剂；
    所述粘结剂在所述有机粘结剂中的重量百分比为50％-90％；
    所述表面活性剂在所述有机粘结剂中的重量百分比为1％-5％；
    所述增塑剂在所述有机粘结剂中的重量百分比为3％-22％。
  19. 根据权利要求18所述的钡锌铌基介质谐振器，其特征在于，对所述坯体进行脱脂的步骤包括：
    对所述坯体进行油萃取脱脂；
    对油萃取脱脂后的所述坯体进行热脱脂。
  20. 根据权利要求19所述的钡锌铌基介质谐振器，其特征在于，对所述坯体进行油萃取脱脂的步骤包括：
    将所述坯体放入非极性溶剂中，所述非极性溶剂的温度为30-50℃，脱脂时间12-36小时；
    将所述坯体从非极性溶剂中取出，并置于烘箱中进行干燥，其中，干燥温度为50-70℃，干燥时间4-12小时。
  21. 一种腔体滤波器，其特征在于，所述腔体滤波器包括腔体、盖板以及权利要求17-20任一项所述的介质谐振器，所述盖板封盖所述腔体以形成谐振腔，所述介质谐振器安装在所述腔体内。
  22. 一种射频拉远设备，其特征在于，所述射频拉远设备包括：射频收发信机模块、功放模块以及权利要求21所述的腔体滤波器，所述射频收发信机模块与所述功放模块连接，所述功放模块与所述腔体滤波器连接。
PCT/CN2015/099954 2015-12-30 2015-12-30 陶瓷材料及其制备方法、谐振器、滤波器及射频拉远设备 WO2017113224A1 (zh)

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