CN105622093B - Ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment - Google Patents

Ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment Download PDF

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CN105622093B
CN105622093B CN201511019803.2A CN201511019803A CN105622093B CN 105622093 B CN105622093 B CN 105622093B CN 201511019803 A CN201511019803 A CN 201511019803A CN 105622093 B CN105622093 B CN 105622093B
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preparation
resonator
green body
nonpolar solvent
temperature
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CN105622093A (en
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庄后荣
陆正武
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Anhui Tatfook Technology Co Ltd
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Shenzhen Tatfook Technology Co Ltd
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46Shaped 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 titanium oxides or titanates
    • C04B35/462Shaped 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 titanium oxides or titanates based on titanates
    • C04B35/465Shaped 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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C04B35/468Shaped 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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing 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
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    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing 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
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01PWAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
    • H01P1/00Auxiliary devices
    • H01P1/20Frequency-selective devices, e.g. filters
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms

Abstract

The present invention provides a kind of Ba2Ti9O20Base microwave medium ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment, wherein the preparation method of medium ceramic material is comprising steps of prepare mixture, including at least Ba in mixture2Ti9O20Based ceramic powder body and organic binder;Material injection forming will be mixed, green body is obtained;Idiosome is successively subjected to nonpolar solvent extraction degreasing and thermal debinding;Green body after thermal debinding is sintered, to obtain Ba2Ti9O20Base microwave dielectric ceramics.The preparation method, by by Ba2Ti9O20The injection moulding of base media ceramic, the available medium ceramic material high with dimensional accuracy after density and even size distribution, sintering, and the cost of material is low, preparation process is simple.Compared with the resonator of dry-pressing preparation, there is high quality factor q × f value and stability.

Description

Ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment
Technical field
The present invention relates to the technical field of dielectric resonator, it is specifically related to a kind of microwave dielectric ceramic materials and its preparation Method, resonator, cavity body filter and radio frequency remote equipment.
Background technique
Dielectric resonator is a most basic microwave component, may be constructed filter, oscillator using dielectric resonator With the microwave circuits such as antenna, be widely used in mobile communication, satellite communication, military radar, global positioning system, Bluetooth technology, It is the key foundation device of modern communication technology in the modern communications such as WLAN.Dielectric resonance applied to microwave circuit Device also needs to meet following dielectric properties requirement other than indispensable mechanical strength: (1) having at microwave frequencies relatively high Permittivity εr, generally require εr> 20, in order to microwave device miniaturization, it is integrated;(2) have under microwave resonance frequency Extremely low dielectric loss, i.e., very high quality factor (Q × f), to guarantee excellent selecting frequency characteristic and reduce device in high frequency Insertion loss;(3) close to zero temperature coefficient of resonance frequency (τf), to guarantee device resonance frequency in temperature change environment High stability.
Ba2Ti9O20The dielectric properties of material: εr=39, Q × f=32000GHz, τf=+2ppm/ DEG C.Also someone has studied Dopant such as Mn, Sn, Zr, Ca, Sr, Pb are to Ba2Ti9O20The influence of dielectric properties.Result of study shows to adulterate Mn, Sn, Pb meeting Q × f value is seriously reduced, and Q × f value can then be increased by adulterating Zr, Ca, Sr.
According to the performance requirement of dielectric resonator, to Ba2Ti9O20Add different compounds.Preparation Ba at present2Ti9O20Base Medium ceramic material resonator is mainly dry pressing.The document of reference is as follows:
[1]H.M.O’Bryan,J.Thomson Jr,J.K.Plourde,A new BaO-TiO2 compound with temperature-stable high permitivity and lowmicrowave loss,J.Am.Ceram.Soc.,57 450-453(1974).
[2]J.K.Plourde,D.F.Lim,H.M.O’Bryan,J.Thomson Jr.,Ba2Ti9O20 as a microwave dielectric resonator,J.Amer.Ceram.Soc.,58 418-420(1975).
The Ba prepared currently with dry pressing2Ti9O20Base medium ceramic material resonator permittivity εrIt is lower, it is unfavorable for Microwave device minimizes, is integrated;Quality factor are lower, so that dielectric loss is higher, temperature coefficient of resonance frequency (τf) higher, The high stability of device resonance frequency in temperature change environment is not can guarantee.Therefore, dry pressing preparation is utilized Ba2Ti9O20Base medium ceramic material resonator dielectric properties are poor.
Although injection molding research and applying and constantly developing, again to ceramics (main application from polymer to metal In structural ceramics, aluminium oxide, zirconium oxide etc.).But for the injection moulding of media ceramic resonator study and produce almost without. Moulding process in the prior art is mainly dry-pressing formed.Dry-pressing formed principle is: making to media ceramic powder adding additives Grain is sintered after being pressed by mold.This technique preparation media resonator has the following disadvantages: that (1) is pressed into During type, existing inside and outside rub causes the pressure loss to make each position stress of green compact not between particle and between particle and die wall , therefore green compact, sintered sample Density Distribution are uneven.Non-uniform degree is related with the pressing mode of selection, common to press Mode processed has unidirectional compacting and two-way compacting, and as seen in figure la and lb, the uniformity of density will affect Jie to Density Distribution situation The dielectric properties of matter resonator, and then also will affect the working performance of filter;(2) pressing mode, dielectric resonator are limited to Major part is column (or analogous shape), and not all geomery can be prepared with dry pressing, such as complex-shaped Resonator demoulding is difficult to realize, and the big resonator of draw ratio can not be also made by suppressing, because being easy due to Density inhomogeneity There is low density area, and then resonator in sintering process is caused to deform, makes low precision, in order to obtain desired shape or size It also needs to be machined out acquisition.
In conclusion the microwave-medium ceramics of the dry pressing preparation generallyd use in the prior art, there are prepared microwaves The Density inhomogeneity of medium ceramic material resonator causes microwave dielectric ceramic materials resonator dielectric properties poor;Meanwhile it is dry Platen press can not prepare complex-shaped resonator.
Summary of the invention
The embodiment of the present invention provides a kind of Ba2Ti9O20Base microwave medium ceramic material resonator and preparation method thereof, with solution Certainly cause to use the microwave-medium ceramics using the density unevenness of microwave-medium ceramics made from dry pressing in the prior art It is made into the poor technical problem of the dielectric properties of resonator.
To solve the above problems, one aspect of the present invention provides a kind of Ba2Ti9O20Base microwave medium ceramic material resonator Preparation method described in preparation method include:
Mixture is prepared, includes at least Ba in the mixture2Ti9O20Based ceramic powder body and organic binder;Wherein, institute State Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, wherein x, y include at least MoO3、WO3、B2O3、 ZnO、Nb2O5、ZrO2、CaCO3、SrCO3One of or a variety of, 0 < mol≤a, b≤0.20mol.
By the mixing material injection forming, green body is obtained;
The idiosome is successively subjected to nonpolar solvent extraction degreasing and thermal debinding;
Green body after thermal debinding is sintered, to obtain the Ba2Ti9O20Base microwave dielectric ceramics.
According to one preferred embodiment of the present invention, the Ba in the mixture2Ti9O20The weight percentage of based ceramic powder body It is 76~85%, the weight percentage of the organic binder is 15~24%.
According to one preferred embodiment of the present invention, the organic binder includes that binder, surfactant, low melting point are organic Object and plasticizer.
According to one preferred embodiment of the present invention, described the step of being injection moulded mixture, includes:
The mixture is heated into toughness melt in injection (mo(u)lding) machine;
The toughness melt is injected in mold, is demoulded after cooling in mold and obtains green body;
Wherein, injection temperature is 170 DEG C~200 DEG C.
According to one preferred embodiment of the present invention, the nonpolar solvent extraction skimming processes of the green body specifically include:
The green body that injection moulding obtains is put into nonpolar solvent, part organic binder is removed with dissolution;
Green body after nonpolar solvent extraction degreasing is dried.
According to one preferred embodiment of the present invention, heat will be continued via the green body of nonpolar solvent extraction degreasing and drying Degreasing, to remove remaining organic binder in green body, the process of the thermal debinding are as follows: by green body with the liter of 0.5~5 DEG C/min Warm rate is warming up to 550 DEG C, then keeps the temperature 2~3 hours.
According to one preferred embodiment of the present invention, the temperature of the sintering is 1200~1400 DEG C, and it is small that 2~6 are kept the temperature after heating When.
According to one preferred embodiment of the present invention, nonpolar solvent in the idiosome nonpolar solvent extraction skimming processes Temperature is 30~50 DEG C, and degreasing time is 12~36 hours;The temperature being dried after degreasing is 50~70 DEG C, and drying time is 4~12h.
According to one preferred embodiment of the present invention, in the organic binder each component weight percentage are as follows: binder 80~90%;Surfactant 1~5%;Low melting point organic matter 2~11% and plasticizer 1~11%.
According to one preferred embodiment of the present invention, the binder include at least paraffin, ethane-acetic acid ethyenyl resin copolymer, One of polypropylene, random polypropylene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer are a variety of; The surfactant includes at least one of stearic acid, octanoic acid, microcrystalline wax or a variety of;The plasticizer includes at least neighbour One of dibatyl phithalate, diethyl phthalate, o-phthalic acid dibutyl ester are a variety of.
Second aspect of the present invention provides a kind of resonator, resonator system as described in any one of above-described embodiment Preparation Method is made.
Third aspect present invention provides a kind of cavity body filter, and the cavity body filter includes cavity, cover board and second Resonator in aspect, the cover board cover the cavity to form resonant cavity, and the resonator installation is in the cavity.
Fourth aspect present invention provides a kind of radio frequency remote equipment, and the radio frequency remote equipment includes: RF transceiver Cavity body filter described in module, power amplifier module and the third aspect, the RF transceiver module and the power amplifier module Connection, the power amplifier module are connect with the cavity body filter.
Compared with the existing technology, Ba provided by the invention2Ti9O20The preparation of base microwave medium ceramic material and its resonator Method, by by Ba2Ti9O20The microwave-medium pottery of the injection moulding of base media ceramic, available density and even size distribution Ceramic material, using resonator made of the microwave dielectric ceramic materials, not only dimensional accuracy is high, permittivity ε also with higher R, higher quality factor q × f value and the advantages that lower temperature coefficient of resonance frequency (τ f), and then make the cavity being prepared Filter has preferable dielectric properties and stability.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other Attached drawing.
Fig. 1 a is the density profile that unidirectional compacting in dry pressing prepares sample;
Fig. 1 b is the density profile that two-way compacting in dry pressing prepares sample;
Fig. 2 is Ba of the present invention2Ti9O20The stream of one preferred embodiment of preparation method of base microwave medium ceramic material resonator Journey schematic diagram;
Fig. 3 a is the Ba of dry-pressing formed preparation2Ti9O20Electron microscope scanning figure after the corrosion of base dielectric resonator port;
Fig. 3 b is the Ba of injection moulding preparation2Ti9O20Electron microscope scanning after the corrosion of base dielectric resonator extremity piece mouth Figure;And
Fig. 4 is the structure composition block diagram of one preferred embodiment of radio frequency remote equipment of the present invention.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is described in further detail.It is emphasized that following implement Example is merely to illustrate the present invention, but is not defined to the scope of the present invention.Likewise, following embodiment is only portion of the invention Point embodiment and not all embodiments, institute obtained by those of ordinary skill in the art without making creative efforts There are other embodiments, shall fall within the protection scope of the present invention.
Referring to Fig. 2, Fig. 2 is Ba of the present invention2Ti9O20One preferred embodiment of preparation method of base microwave medium ceramic material Flow diagram;The preparation method includes but is not limited to following steps:
Step S100, prepares mixture.Ba is included at least in mixture2Ti9O20Based ceramic powder body and organic binder.
In the present embodiment, by Ba2Ti9O20Based ceramic powder body and organic binder are mixed on kneading machine, until It is uniformly mixed, preferably incorporation time is 4~8h, obtains injection molding mixture, the content of heterogeneity is with powder in mixing Granularity, pattern, density are related, so its design of mixture of different powder is different;The Ba being directed in the present invention2Ti9O20Base Media ceramic, in injection molding mixture, Ba2Ti9O20The weight percentage of based ceramic powder body is preferably 76~85%, is had The weight percentage of machine binder is preferably 15~24%.Using weight percentage Ba2Ti9O20Based ceramic powder body is matched Ba prepared by the mode of setting2Ti9O20Base microwave dielectric ceramics have excellent dielectric properties and quality stability.
Wherein, Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, x, y include at least MoO3、 MnO2、WO3、SnO2、B2O3、ZnO、Nb2O5、ZrO2、CaCO3、SrCO3、PbCO3One of or a variety of, and a, b in chemical formula Value range it is preferred are as follows: 0mol≤a, b≤0.20mol.Utilize the Ba of the stoichiometric factor of chemical formula in the present invention2Ti9O20Base Ceramic powder, the microwave dielectric ceramic materials dielectric constant with higher that injection moulding can be made to obtain, higher quality Factor Q × f value and lower temperature coefficient of resonance frequency (τ f).
Among these, Ba2Ti9O20The formula determination of base is mainly prepared by solid phase method, in proportion ingredient, generally BaCO3And TiO2According to the ratio of 1:4 carry out proportion reaction obtain, later again through ball milling, calcining (calcination temperature be 1000 DEG C~ 1200 DEG C) and mill;Wherein, ball-milling medium when ball mill carries out ball milling is put into (the react after) powder calcined is Zirconia ball, Ball-milling Time are 4~12h, 2%~5% PVA (polyvinyl alcohol) binder are added in mechanical milling process, through spraying It is granulated on mist tower, then prilling powder is put into after mold is pressed (pressure is 100MPa~200MPa) and is carried out Test material performance itself is calcined, eventually passes through and obtains required Ba after grinder is ground2Ti9O20Base microwave dielectric material Material.
The organic binder may include binder, surfactant, low melting point organic matter and plasticizer etc..Wherein, The weight percentage of each component is preferred in organic binder are as follows: binder 50~90%;Surfactant 1~5%;Low melting point Organic matter 2~11% and plasticizer 1~11%.
It is further preferred that binder includes at least paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random poly- third One of alkene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer are a variety of;Surfactant is at least Including one of stearic acid, octanoic acid, microcrystalline wax or a variety of;Plasticizer includes at least dibutyl phthalate, adjacent benzene two One of formic acid diethylester, o-phthalic acid dibutyl ester are a variety of.It is closed from the type of a variety of binders provided above Reason is chosen, and while meeting material function, can also save certain cost.
Step S200 will mix material injection forming, obtain green body.
Step S200 further comprises: mixture is heated into toughness melt in injection (mo(u)lding) machine;Then should Toughness melt injects in mold, demoulds after cooling in mold and obtains green body.Wherein, injection temperature is preferably 170 DEG C~200 DEG C, demoulding obtains molding blank in 2~4 minutes after toughness melt injection mold.Injection temperature in the step and cold But density and the size distribution of time, the microwave dielectric ceramic materials that can make are more uniform, and then performance is more stable.
Idiosome is successively carried out nonpolar solvent extraction degreasing and thermal debinding by step S300.
Nonpolar solvent extraction skimming processes are as follows: the green body that injection moulding obtains is put into gasoline, carbon disulfide, diformazan In the nonpolar solvents such as benzene, ether, stupid, chloroform, carbon tetrachloride, naphtha, part organic binder, nonpolarity are removed with dissolution The temperature of solvent is preferably controlled between 30~50 DEG C, and degreasing time was at 12~36 hours.After nonpolar solvent extraction degreasing Green body is sufficiently dry in an oven, and drying temperature is preferably 50~70 DEG C, and the time is 4~12h.
Nonpolar solvent extraction skimming processes in the step are very important, because if directly carrying out that heat is de- can be by Organic binder ingredient is excessively high in idiosome, and leads to fragmentation of the sample in skimming processes.
Thermal degreasing process is as follows: the green body after drying being put into electric furnace and carries out thermal debinding, remaining is had to remove Machine binder.Idiosome is preferably warming up to 550 DEG C with the heating rate of 0.5~5 DEG C/min by the process, and it is small then to keep the temperature 2~3 When.Heating rate and soaking time parameter in the step, under the premise of meeting production efficiency, it can be ensured that is made is micro- Wave medium ceramic material compact structure, not cracked, the stability further improved performance.
Green body after thermal debinding is sintered by step S400, to obtain Ba2Ti9O20Base microwave dielectric ceramics.
In this step, sintering temperature keeps the temperature 2~6 hours preferably between 1200~1400 DEG C.
The present invention prepares Ba with injection moulding2Ti9O20Base microwave medium ceramic material, by by Ba2Ti9O20Base medium Ceramic injection forming, the microwave dielectric ceramic materials of available density and even size distribution use the microwave-medium ceramics Not only dimensional accuracy is high for resonator made of material, dielectric constant also with higher, higher quality factor q × f value with The advantages that lower temperature coefficient of resonance frequency (τ f).
Several specific embodiments carry out Ba during the present invention will be described in detail below2Ti9O20Base microwave medium ceramic material resonator The performance parameter of manufacturing process and finished product resonator.
Embodiment one
The present embodiment main material material formula uses chemical formula: Ba2Ti9O20+ 0.5mol%ZrO2For chemical composition, it is respectively compared The performance of dry pressing and the dielectric resonator of injection moulding preparation, the dielectric properties of the present embodiment main material itself are with respect to dielectric Constant ε r is 40, and quality factor (Q × f) value is 43 500GHz, and temperature coefficient of resonance frequency tf is+3ppm/ DEG C.Injection moulding Technique preparation Ba2Ti9O20 base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: by Ba2Ti9O20Based ceramic powder body and organic binder are uniformly mixed Injection molding mixture is obtained, the content of heterogeneity is related with the granularity of powder, pattern, density in mixing, so different Its design of mixture of powder is different;It is directed to Ba2Ti9O20Base media ceramic, in the injection molding mixture, Ba2Ti9O20Base pottery The weight percentage of porcelain powder is 78%, and the weight percentage of organic binder is 22%;Wherein, the organic binder by Binder, surfactant, low melting point organic matter and plasticizer composition, each component weight percentage are as follows: binder 80%;Table Face activating agent: 5%;Low melting point organic matter: 10%;Plasticizer: 5%;
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is 180 DEG C, inject mold after in 2 minutes demoulding obtain molding blank;
(3) nonpolar solvent extraction degreasing: the green body that injection moulding obtains is put into nonpolar solvent, dissolves removing portion Divide organic binder, the temperature of nonpolar solvent is at 30 DEG C, and degreasing time is 24 hours, the base after nonpolar solvent extraction degreasing Body is sufficiently dry in an oven.
(4) thermal debinding: the green body after drying being put into electric furnace and carries out thermal debinding, to remove remaining organic adhesive Agent in the embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, keeps the temperature 2 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1400 DEG C, keeps the temperature 2 hours, it is humorous to obtain medium Shake device.
60 dielectric resonators are prepared with dry-pressing and injection molding technique respectively, sample is as shown in figure 3, can be with from Fig. 3 Find out injection moulding with dry pressing preparation compared with, crystallite dimension is more uniform, and particle size is smaller, this for Ba2Ti9O20The final performance and stability of base dielectric resonator product influence correlation.Simultaneously to the performance of sample into Go test, performance such as table 1:
Table 1: the performance parameter of injection moulding and dry-pressing formed preparation media resonator compares
The dielectric resonator for being injection moulded preparation as can be seen from Table 1 is more excellent than performance prepared by traditional dry pressing, and property It can stablize.
Embodiment two
The present embodiment main material material formula uses chemical formula: Ba2Ti9O20+ 1mol%ZrO2For chemical composition, it is respectively compared dry The performance of platen press and the dielectric resonator of injection moulding preparation, the dielectric properties of the present embodiment main material itself are normal with respect to dielectric Number εrIt is 39, quality factor (Q × f) value is 50070GHz, temperature coefficient of resonance frequency τfIt is -5ppm/ DEG C.Dry pressing is mainly led to After crossing granulation, compression moulding, it is sintered to obtain dielectric resonator, simple process.Injection molding technique prepares Ba2Ti9O20Base Dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: in the injection molding mixture of the embodiment, Ba2Ti9O20Base ceramics The weight percentage of powder is 75%, and the weight percentage of organic binder is 25%;Each component weight in organic binder Amount percentage composition is binder 80%;Surfactant 5%;Low melting point organic matter 10%;Plasticizer 5%.
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is 180 DEG C, inject mold after in 2 minutes demoulding obtain molding blank.
(3) nonpolar solvent extraction degreasing: the green body that injection moulding obtains is put into nonpolar solvent, dissolves removing portion Divide organic binder, the temperature of nonpolar solvent is 30 DEG C, and degreasing time is 24 hours, the base after nonpolar solvent extraction degreasing Body is dried in an oven.
(4) thermal debinding: the green body after drying being put into electric furnace and carries out thermal debinding, to remove remaining organic adhesive Agent in the embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, keeps the temperature 2 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1400 DEG C, keeps the temperature 2 hours, it is humorous to obtain medium Shake device.
60 dielectric resonators are prepared with dry-pressing and injection molding technique respectively, and the performance of sample is tested, Performance such as table 2:
Table 2: the performance parameter of injection moulding and dry-pressing formed preparation media resonator compares
Embodiment three
The present embodiment main material material formula uses chemical formula: Ba2Ti9O20+ 2mol%ZrO2For chemical composition, it is respectively compared dry The performance of platen press and the dielectric resonator of injection moulding preparation, the dielectric properties of the present embodiment main material itself are normal with respect to dielectric Number εrIt is 40, quality factor (Q × f) value is 56000GHz, temperature coefficient of resonance frequency τfIt is+2ppm/ DEG C.Dry pressing is mainly led to After crossing granulation, compression moulding, it is sintered to obtain dielectric resonator, simple process.Injection molding technique prepares Ba2Ti9O20Base Dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: in the injection molding mixture of the embodiment, Ba2Ti9O20Base ceramics The weight percentage of powder is 75%, and the weight percentage of organic binder is 25%;Each component weight in organic binder Amount percentage composition is binder 80%;Surfactant 5%;Low melting point organic matter 10%;Plasticizer 5%.
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is 180 DEG C, inject mold after in 2 minutes demoulding obtain molding blank.
(3) nonpolar solvent extraction degreasing: the green body that injection moulding obtains is put into nonpolar solvent, dissolves removing portion Divide organic binder, the temperature of nonpolar solvent is 30 DEG C, and degreasing time is 24 hours, the base after nonpolar solvent extraction degreasing Body is dried in an oven.
(4) thermal debinding: the green body after drying being put into electric furnace and carries out thermal debinding, to remove remaining organic adhesive Agent in the embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, keeps the temperature 2 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1400 DEG C, keeps the temperature 4 hours, it is humorous to obtain medium Shake device.
60 dielectric resonators are prepared with dry-pressing and injection molding technique respectively, and the performance of sample is tested, Performance such as table 3:
Table 3: the performance parameter of injection moulding and dry-pressing formed preparation media resonator compares
Ba provided by the invention2Ti9O20The preparation method of base microwave medium ceramic material resonator, by by Ba2Ti9O20 The injection moulding of base media ceramic, the available resonator high with dimensional accuracy after density and even size distribution, sintering, and The cost of material is low, and preparation process is simple.Compared with the resonator of dry-pressing preparation, also there is high quality factor q × f value and performance Stability.
In addition, the embodiment of the present invention also provides a kind of resonator and a kind of cavity body filter, the resonator is by above-mentioned implementation Preparation method described in example is made.From the correlation data in above-described embodiment it is found that using dry pressing and injection moulding method respectively Prepare Ba2Ti9O20The Q value of the dielectric resonator of sill, the dielectric resonator of dry pressing preparation is 3500~4200, and frequency is 1.6G, and the dielectric resonator Q value for being injection moulded preparation can achieve 3900~4300, frequency 1.6G.It can be seen that this hair The Ba using injection moulding preparation in bright2Ti9O20The dielectric resonator Q value of sill is higher, and performance is more stable.
Cavity body filter includes the resonator in above-described embodiment, by resonator quality factor q with higher × f value The advantages that with lower temperature coefficient of resonance frequency (τ f), is allowed to the cavity body filter being prepared with preferable dielectric properties And stability.And the technical characteristic of the structure of the other parts about cavity body filter and parameter is in the reason of those skilled in the art It solves in range, details are not described herein again.
Referring to Fig. 4, Fig. 4 is the structure composition block diagram of one preferred embodiment of radio frequency remote equipment of the present invention, which is drawn Remote equipment includes but is not limited to following structural unit: RF transceiver module 510, power amplifier module 520 and cavity body filter 530.Wherein, RF transceiver module 510 is connect with power amplifier module 520, power amplifier module 520 further with cavity body filter 530 connections.
Radio frequency remote equipment works in descending time slot, the transmitting in two channels from RF transceiver module 510 Signal enters cavity body filter 530 by power amplifier module 520, and 530 pairs of transmitting signals of cavity body filter complete filtering, then power Antenna opening is emitted to after synthesis;Radio frequency remote equipment works in ascending time slot, and the signal received from antenna opening passes through cavity Filter 530 enters power amplifier module 520 after filtering, and exports after the amplification of power amplifier module 520 to RF transceiver module 510 Corresponding receiving channel.
Further, which can also include power module 540, and the power module 540 is for penetrating this The modules of frequency remote device are powered.
The foregoing is merely section Examples of the invention, are not intended to limit protection scope of the present invention, all utilizations Equivalent device made by description of the invention and accompanying drawing content or equivalent process transformation are applied directly or indirectly in other correlations Technical field, be included within the scope of the present invention.

Claims (14)

1. a kind of Ba2Ti9O20The preparation method of base microwave medium ceramic material, which is characterized in that the preparation method includes:
Mixture is prepared, includes at least Ba in the mixture2Ti9O20Based ceramic powder body and organic binder;Wherein, described Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, wherein x, y include at least MoO3、WO3、B2O3、 ZnO、Nb2O5、ZrO2、CaCO3、SrCO3One of or a variety of, 0 < a, b≤0.20mol;
By the mixing material injection forming, green body is obtained;
The green body is successively subjected to nonpolar solvent extraction degreasing and thermal debinding;
Green body after thermal debinding is sintered, to obtain the Ba2Ti9O20Base microwave dielectric ceramics.
2. preparation method according to claim 1, which is characterized in that the Ba in the mixture2Ti9O20Based ceramic powder body Weight percentage be 76~85%, the weight percentage of the organic binder is 15~24%.
3. preparation method according to claim 1, which is characterized in that the organic binder includes binder, surface work Property agent, low melting point organic matter and plasticizer.
4. preparation method according to claim 1, which is characterized in that described the step of being injection moulded mixture includes:
The mixture is heated into toughness melt in injection (mo(u)lding) machine;
The toughness melt is injected in mold, is demoulded after cooling in mold and obtains green body;
Wherein, injection temperature is 170 DEG C~200 DEG C.
5. preparation method according to claim 1, which is characterized in that the nonpolar solvent extraction skimming processes of the green body It specifically includes:
The green body that injection moulding obtains is put into nonpolar solvent, part organic binder is removed with dissolution;
Green body after nonpolar solvent extraction degreasing is dried.
6. preparation method according to claim 5, which is characterized in that will be via nonpolar solvent extraction degreasing and drying Green body continues thermal debinding, to remove remaining organic binder in green body, the process of the thermal debinding are as follows: by green body with The heating rate of 0.5~5 DEG C/min is warming up to 550 DEG C, then keeps the temperature 2~3 hours.
7. preparation method according to claim 1, which is characterized in that the temperature of the sintering is 1200~1400 DEG C, is added 2~6 hours are kept the temperature after heat.
8. preparation method according to claim 5, which is characterized in that in the green body nonpolar solvent extraction skimming processes Nonpolar solvent temperature be 30~50 DEG C, degreasing time be 12~36 hours;The temperature being dried after degreasing be 50~ 70 DEG C, drying time is 4~12h.
9. preparation method according to claim 3, which is characterized in that the weight percent of each component in the organic binder Content are as follows: binder 80~90%;Surfactant 1~5%;Low melting point organic matter 2~11% and plasticizer 1~11%.
10. preparation method according to claim 9, which is characterized in that the binder includes at least paraffin, ethylene-second One of sour ethylene resin copolymer, polypropylene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer or It is a variety of;The surfactant includes at least one of stearic acid, octanoic acid, microcrystalline wax or a variety of;The plasticizer is at least Including one of dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester or a variety of.
11. preparation method according to claim 10, which is characterized in that the polypropylene includes random polypropylene.
12. a kind of resonator, which is characterized in that the resonator includes by the described in any item preparation methods of claim 1-11 Material obtained.
13. a kind of cavity body filter, which is characterized in that the cavity body filter includes cavity, cover board and claim 12 institute The resonator stated, the cover board cover the cavity to form resonant cavity, and the resonator installation is in the cavity.
14. a kind of radio frequency remote equipment, which is characterized in that the radio frequency remote equipment includes: RF transceiver module, power amplifier Cavity body filter described in module and claim 13, the RF transceiver module are connect with the power amplifier module, institute Power amplifier module is stated to connect with the cavity body filter.
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