CN105622093A - Ceramic material and preparation method thereof, and harmonic oscillator, filter and radio frequency zooming-out equipment - Google Patents
Ceramic material and preparation method thereof, and harmonic oscillator, filter and radio frequency zooming-out equipment Download PDFInfo
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Abstract
The invention provides a Ba2Ti9O2O-basedmicrowave dielectric ceramic material and a preparation method thereof, and a harmonic oscillator, a filter and radio frequency zooming-out equipment thereof, wherein the preparation method for the dielectric ceramic material comprises the following steps: preparing a mixed material which at least includes Ba2Ti9O2O-based ceramic powder and organic adhesive, injection molding the mixed material to obtain a green body, subjecting the green body to nonpolar solvent extraction degreasing and thermal degreasing successively, and sintering the thermally degreased green body to obtain Ba2Ti9O2O-based microwave dielectric ceramic. According to the preparation method provided by the invention, a dielectric ceramic material featured with uniform density and size distribution and high dimensional precision after sintering can be obtained by injection molding the Ba2Ti9O2O-baseddielectric ceramic, the material cost is low, and the preparation technique is simple. Compared with a harmonic oscillator prepared through dry pressing, the harmonic oscillator provided by the invention has a high quality factor Q*F value and performance stability.
Description
Technical field
The present invention relates to the technical field of dielectric resonator, specifically relate to a kind of microwave dielectric ceramic materials and its preparation method, resonator, cavity body filter and radio frequency remote equipment.
Background technology
Dielectric resonator is a microwave component the most basic, utilize dielectric resonator can form the microwave circuits such as wave filter, vibrator and antenna, it is widely used in the modern communicationses such as mobile communication, satellite communications, military radar, global positioning system (GPS), Bluetooth technology, WLAN (wireless local area network), it is the key foundation device of modern communication technology. The dielectric resonator being applied to microwave circuit, except the physical strength of indispensability, also needs satisfied following dielectric properties to require: (1) has relatively high DIELECTRIC CONSTANT �� at microwave frequenciesr, general requirement ��r> 20, so that microwave device miniaturization, integrated; (2) there is extremely low dielectric loss under microwave resonance frequency, namely very high quality factor (Q �� f), to ensure excellent selecting frequency characteristic and to reduce device insertion loss in high frequency; (3) close to zero temperature coefficient of resonance frequency (��f), to ensure the high stability of device resonant frequency in temperature variation environment.
Ba2Ti9O20The dielectric properties of material: ��r=39, Q �� f=32000GHz, ��f=+2ppm/ DEG C. Also someone have studied hotchpotch if Mn, Sn, Zr, Ca, Sr, Pb are to Ba2Ti9O20The impact of dielectric properties. Result of study shows that doped with Mn, Sn, Pb can seriously reduce Q �� f value, and adulterate Zr, Ca, Sr then can increase Q �� f value.
Performance requriements according to dielectric resonator, to Ba2Ti9O20Add different compounds. Prepare Ba at present2Ti9O20Base medium ceramic material resonator mainly dry-pressing formed method. The document quoted is as follows:
[1]H.M.O��Bryan,J.ThomsonJr,J.K.Plourde,AnewBaO-TiO2compoundwithtemperature-stablehighpermitivityandlowmicrowaveloss,J.Am.Ceram.Soc.,57450-453(1974).
[2]J.K.Plourde,D.F.Lim,H.M.O��Bryan,J.ThomsonJr.,Ba2Ti9O20asamicrowavedielectricresonator,J.Amer.Ceram.Soc.,58418-420(1975).
Utilize Ba prepared by dry pressing at present2Ti9O20Base medium ceramic material resonator DIELECTRIC CONSTANT ��rLower, it is unfavorable for microwave device miniaturization, integrated; Quality factor are lower, thus dielectric loss is higher, temperature coefficient of resonance frequency (��f) higher, the high stability of device resonant frequency in temperature variation environment cannot be ensured. Therefore, utilize Ba prepared by dry pressing2Ti9O20Base medium ceramic material resonator dielectric properties are poor.
Although injection molding investigation and application is in continuous development, again to pottery (being mainly used in structural ceramics, aluminum oxide, zirconium white etc.) from polymkeric substance to metal. But injection molding research and production for media ceramic resonator almost do not have. Moulding process of the prior art is mainly dry-pressing formed. Dry-pressing formed principle is: to media ceramic powder adding additives granulation, be pressed by mould after sinter. This technique is prepared dielectric resonator and be there is following shortcoming: in (1) compression moulding process, the inside and outside friction existed between particle and between particle and mould wall causes the pressure-losses to make pressed compact each position unbalance stress, and therefore green compact, sintered sample density distribution are uneven. Uneven degree is relevant with the pressing mode selected, conventional pressing mode has unidirectional compacting and two-way compacting, as seen in figure la and lb, the homogeneity of density can affect the dielectric properties of dielectric resonator to its density distribution situation, and then also can affect the serviceability of wave filter; (2) it is limited to pressing mode, dielectric resonator major part is column (or analogous shape), not all shape size can be prepared by dry pressing, the such as complex-shaped resonator demoulding is difficult to realize, the resonator that length-to-diameter ratio is big also cannot be obtained by compacting, because easily there is low density area because of Density inhomogeneity, and then causes resonator distortion in sintering process, make low precision, also need to carry out machining acquisition to obtain the shape wanted or size.
In sum, there is the Density inhomogeneity of prepared microwave dielectric ceramic materials resonator, cause microwave dielectric ceramic materials resonator dielectric properties poor in microwave-medium ceramics prepared by the dry pressing usually adopted in prior art; Meanwhile, dry pressing cannot 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 its preparation method, to solve the density unevenness of the microwave-medium ceramics adopting dry-pressing formed method obtained in prior art, cause using this microwave-medium ceramics to make the poor technical problem of the dielectric properties of resonator.
For solving the problem, one aspect of the present invention provides a kind of Ba2Ti9O20Preparation method described in the preparation method of base microwave medium ceramic material resonator comprises:
Prepare compound, described compound at least comprises Ba2Ti9O20Based ceramic powder body and organic binder bond;
By described compound injection molding, obtain base substrate;
Described idiosome is successively carried out non-polar solvent extraction degreasing and thermal debinding;
Base substrate after thermal debinding is sintered, to obtain described Ba2Ti9O20Base microwave dielectric ceramics.
According to one preferred embodiment of the present invention, the Ba in described compound2Ti9O20The weight percentage of based ceramic powder body is 76��85%, and the weight percentage of described organic binder bond is 15��24%.
According to one preferred embodiment of the present invention, described Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, wherein x, y at least comprise MoO3��MnO2��WO3��SnO2��B2O3��ZnO��Nb2O5��ZrO2��CaCO3��SrCO3��PbCO3In one or more, 0mol��a, b��0.20mol.
According to one preferred embodiment of the present invention, described organic binder bond comprises binding agent, tensio-active agent, low melting point organism and softening agent.
According to one preferred embodiment of the present invention, described injection molding for compound step is comprised:
Described compound is heated into toughness melt in injection moulding machine;
Being injected by described toughness melt in mould, in mould, after cooling, the demoulding obtains base substrate;
Wherein, injection temperature is 170 DEG C��200 DEG C.
According to one preferred embodiment of the present invention, the non-polar solvent extraction skimming processes of described idiosome specifically comprises:
Base substrate injection molding obtained puts into non-polar solvent, de-except part organic binder bond to dissolve;
Non-polar solvent extracts the base substrate after degreasing be dried.
According to one preferred embodiment of the present invention, thermal debinding will be proceeded via the idiosome that non-polar solvent extracts degreasing also dry, with de-except remaining organic binder bond in idiosome, the process of described thermal debinding is: with the temperature rise rate of 0.5��5 DEG C/min, idiosome is warming up to 550 DEG C, is then incubated 2��3 hours.
According to one preferred embodiment of the present invention, the temperature of described sintering is 1200��1400 DEG C, is incubated 2��6 hours after heating.
According to one preferred embodiment of the present invention, the temperature of the non-polar solvent in described idiosome non-polar solvent extraction skimming processes is 30��50 DEG C, and degreasing time is 12��36 hours; The temperature being dried after degreasing is 50��70 DEG C, and time of drying is 4��12h.
According to one preferred embodiment of the present invention, in described organic binder bond, the weight percentage of each component is: binding agent 50��90%; Tensio-active agent 1��5%; Low melting point organism 2��11% and softening agent 1��11%.
According to one preferred embodiment of the present invention, described binding agent at least comprises one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, Atactic Polypropelene, polystyrene, polymethacrylate, ethylene ethyl acrylate copolymer; Described tensio-active agent at least comprises one or more in stearic acid, sad, microcrystalline wax; Described softening agent at least comprises one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.
For solving the problems of the technologies described above, second aspect present invention provides a kind of Ba2Ti9O20Base microwave medium ceramic material, described microwave dielectric ceramic materials comprises the Ba that weight percentage is 76��85%2Ti9O20Based ceramic powder body and weight percentage are the organic binder bond of 15��24%.
According to one preferred embodiment of the present invention, described Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, wherein x, y at least comprise MoO3��MnO2��WO3��SnO2��B2O3��ZnO��Nb2O5��ZrO2��CaCO3��SrCO3��PbCO3In one or more, 0mol��a, b��0.20mol.
According to one preferred embodiment of the present invention, described organic binder bond comprises binding agent, tensio-active agent, low melting point organism and softening agent.
According to one preferred embodiment of the present invention, in described organic binder bond, the weight percentage of each component is: binding agent 50��90%; Tensio-active agent 1��5%; Low melting point organism 2��11% and softening agent 1��11%.
According to one preferred embodiment of the present invention, described binding agent at least comprises one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, Atactic Polypropelene, polystyrene, polymethacrylate, ethylene ethyl acrylate copolymer; Described tensio-active agent at least comprises one or more in stearic acid, sad, microcrystalline wax; Described softening agent at least comprises one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.
Third aspect present invention provides a kind of resonator, and described resonator is obtained by the preparation method described in the arbitrary item in above-described embodiment.
Fourth aspect present invention provides a kind of cavity body filter, and described cavity body filter comprises the resonator in cavity, cover plate and the third aspect, and the described cover plate envelope described cavity of lid is to form resonator cavity, and described resonator is arranged in described cavity.
Fifth aspect present invention provides a kind of radio frequency remote equipment, described radio frequency remote equipment comprises: the cavity body filter described in RF transceiver module, power amplifier module and fourth aspect, described RF transceiver module is connected with described power amplifier module, and described power amplifier module is connected with described cavity body filter.
Sixth aspect present invention provides a kind of Ba2Ti9O20The formula of base microwave medium ceramic material, this formula comprises the component of following weight percentage: Ba2Ti9O20Based ceramic powder body 76��85%; Organic binder bond 15��24%.
Relative to prior art, Ba provided by the invention2Ti9O20The preparation method of base microwave medium ceramic material and resonator thereof, by by Ba2Ti9O20Base media ceramic injection molding, the microwave dielectric ceramic materials of density and even size distribution can be obtained, use the resonator not only dimensional precision height that this microwave dielectric ceramic materials is made, also there is the advantages such as higher dielectric constant, higher quality factor q �� f value and lower temperature coefficient of resonance frequency (�� f), and then make the cavity body filter prepared have preferably dielectric properties and stability.
Accompanying drawing explanation
In order to the technical scheme being illustrated more clearly in the embodiment of the present invention, below the accompanying drawing used required in embodiment being described is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 a is the density profile that sample is prepared in the unidirectional compacting in dry pressing;
Fig. 1 b is the density profile that sample is prepared in the two-way compacting in dry pressing;
Fig. 2 is Ba of the present invention2Ti9O20The schematic flow sheet of preparation method one preferred embodiment of base microwave medium ceramic material resonator;
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 Ba prepared by injection molding2Ti9O20Electron microscope scanning figure after the corrosion of base dielectric resonator extremity piece mouth; And
Fig. 4 is the structure composition frame chart of radio frequency remote equipment one preferred embodiment of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail. Refer in particular to
Going out, following examples are only for illustration of the present invention, but the scope of the present invention do not limited. Same, following examples are only the part embodiment of the present invention and not all embodiments, and those of ordinary skill in the art are not making other embodiments all obtained under creative work prerequisite, all belong to the scope of protection of the invention.
Referring to Fig. 2, Fig. 2 is Ba of the present invention2Ti9O20The schematic flow sheet of preparation method one preferred embodiment of base microwave medium ceramic material; This preparation method includes but not limited to following step:
Step S100, prepares compound. Compound at least comprises Ba2Ti9O20Based ceramic powder body and organic binder bond.
In the present embodiment, by Ba2Ti9O20Based ceramic powder body and organic binder bond mix on mixing roll, until mixing, it is preferable that mixing time is 4��8h, obtains injection molding mixture, content not congruent in batch mixing is relevant with the granularity of powder, shape looks, density, 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%, and the weight percentage of organic binder bond is preferably 15��24%. Adopt this weight percentage Ba2Ti9O20Ba prepared by the distributing style of based ceramic powder body2Ti9O20Base microwave dielectric ceramics, has excellent dielectric properties and quality stability.
Wherein, Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, x, y at least comprise MoO3��MnO2��WO3��SnO2��B2O3��ZnO��Nb2O5��ZrO2��CaCO3��SrCO3��PbCO3In one or more, and the span of a, b in chemical formula is preferably: 0mol��a, b��0.20mol. Utilize the Ba of the stoichiometric factor of chemical formula in the present invention2Ti9O20Based ceramic powder body, it is possible to the microwave dielectric ceramic materials that injection molding is obtained has higher dielectric constant, higher quality factor q �� f value and lower temperature coefficient of resonance frequency (�� f).
This wherein, Ba2Ti9O20The formula of base is determined to prepare mainly through solid phase method, prepares burden in proportion, is generally BaCO3And TiO2Carry out proportioning according to the ratio of 1:4 to be obtained by reacting, afterwards again through ball milling, calcining (calcining temperature is 1000 DEG C��1200 DEG C) and mill; Wherein, (namely after the reaction) powder calcined is put into ball-milling medium when ball mill carries out ball milling is zirconia ball, the ball milling time is 4��12h, mechanical milling process adds PVA (polyvinyl alcohol) binding agent of 2%��5%, through carrying out granulation on spray tower, then prilling powder is put into mould be pressed after (pressure is 100MPa��200MPa) carry out calcining the performance of test material own, eventually pass through after shredder grinds and obtain required Ba2Ti9O20Base microwave dielectric material.
This organic binder bond can comprise binding agent, tensio-active agent, low melting point organism and softening agent etc. Wherein, in organic binder bond, the weight percentage of each component is preferably: binding agent 50��90%; Tensio-active agent 1��5%; Low melting point organism 2��11% and softening agent 1��11%.
Further preferably, binding agent at least comprises one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, Atactic Polypropelene, polystyrene, polymethacrylate, ethylene ethyl acrylate copolymer; Tensio-active agent at least comprises one or more in stearic acid, sad, microcrystalline wax; Softening agent at least comprises one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester. Rational choice is carried out, while meeting material function, it is also possible to save certain cost from the kind of the above multiple binding agent provided.
Step S200, by compound injection molding, obtains base substrate.
Step S200 comprises further: compound is heated into toughness melt in injection moulding machine; Then injecting in mould by this toughness melt, in mould, after cooling, the demoulding obtains base substrate. Wherein, injection temperature is preferably 170 DEG C��200 DEG C, and after toughness melt injection mould, in 2��4 minutes, the demoulding obtains molding blank. Injection temperature in this step and cooling time, it is possible to make the density of microwave dielectric ceramic materials that obtains and distribution of sizes more even, and then performance is more stable.
Step S300, successively carries out non-polar solvent extraction degreasing and thermal debinding by idiosome.
Non-polar solvent extraction skimming processes is as follows: base substrate injection molding obtained puts into the non-polar solvents such as gasoline, dithiocarbonic anhydride, dimethylbenzene, ether, stupid, chloroform, tetracol phenixin, petroleum naphtha, de-except part organic binder bond to dissolve, the temperature of non-polar solvent preferably controls between 30��50 DEG C, and degreasing time was at 12��36 hours. Base substrate after non-polar solvent extraction degreasing is fully dry in an oven, and drying temperature is preferably 50��70 DEG C, and the time is 4��12h.
Non-polar solvent extraction skimming processes in this step is very important, because if directly carrying out that heat is de-can be too high due to organic binder bond composition in idiosome, and causes cracked in skimming processes of sample.
Thermal debinding process is as follows: dried base substrate is put into electrical heater and carries out thermal debinding, with de-except remaining organic binder bond. Idiosome is preferably warming up to 550 DEG C with the temperature rise rate of 0.5��5 DEG C/min by this process, is then incubated 2��3 hours. Temperature rise rate in this step and soaking time parameter, under the prerequisite meeting production efficiency, it is possible to guarantee the microwave dielectric ceramic materials compact structure making to obtain, crackle do not occur, promote the stability of performance further.
Step S400, sinters the base substrate after thermal debinding, to obtain Ba2Ti9O20Base microwave dielectric ceramics.
In this step, sintering temperature, preferably between 1200��1400 DEG C, is incubated 2��6 hours.
The present invention's injection molding method prepares Ba2Ti9O20Base microwave medium ceramic material, by by Ba2Ti9O20Base media ceramic injection molding, the microwave dielectric ceramic materials of density and even size distribution can be obtained, use the resonator not only dimensional precision height that this microwave dielectric ceramic materials is made, also there is the advantages such as higher dielectric constant, higher quality factor q �� f value and lower temperature coefficient of resonance frequency (�� f).
Several specific embodiments illustrate Ba in the present invention in detail below2Ti9O20The performance perameter of base microwave medium ceramic material resonator making processes and finished product resonator.
Embodiment one
The present embodiment main material formula adopts chemical formula: Ba2Ti9O20+ 0.5mol%ZrO2For chemistry composition, compare dry pressing respectively and the performance of dielectric resonator prepared by injection molding method, the dielectric properties relative permittivity �� r of the present embodiment main material itself is 40, and quality factor (Q �� f) value is 43500GHz, and temperature coefficient of resonance frequency tf is+3ppm/ DEG C. Injection molding technique is prepared Ba2Ti9O20 base dielectric resonator and is realized by following processing step:
(1) hybrid ceramic powder body and organic binder bond: by Ba2Ti9O20Based ceramic powder body and organic binder bond mix and obtain injection molding mixture, and content not congruent in batch mixing is relevant with the granularity of powder, shape looks, density, so its design of mixture of different powder is different; It is directed to Ba2Ti9O20Base media ceramic, in this injection molding mixture, Ba2Ti9O20The weight percentage of based ceramic powder body is 78%, and the weight percentage of organic binder bond is 22%; Wherein, this organic binder bond is made up of binding agent, tensio-active agent, low melting point organism and softening agent, and each composition weight percentage composition is: binding agent 80%; Tensio-active agent: 5%; Low melting point organism: 10%; Softening agent: 5%;
(2) injection molding: injection molding mixture injection molding on injection moulding machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank;
(3) non-polar solvent extraction degreasing: base substrate injection molding obtained puts into non-polar solvent, dissolve de-except part organic binder bond, the temperature of non-polar solvent is at 30 DEG C, and degreasing time is 24 hours, and the base substrate after non-polar solvent extraction degreasing is fully dry in an oven.
(4) thermal debinding: dried base substrate is put into electrical heater and carries out thermal debinding, with de-except remaining organic binder bond, in this embodiment, be warming up to 550 DEG C with the temperature rise rate of 0.5 DEG C/min, be incubated 2 hours.
(5) sinter: the base substrate after thermal debinding sinters, and sintering temperature is 1400 DEG C, is incubated 2 hours, obtains dielectric resonator.
Preparing 60 dielectric resonators with dry-pressing and injection molding technique respectively, as shown in Figure 3, compared with as can be seen from Figure 3 injection molding is prepared with dry-pressing formed method, grain-size is more even, and particle size is less, and this is for Ba for sample2Ti9O20The performance that base dielectric resonator product is final and stability influence are proportionate relation. The performance of sample having been tested, performance is such as table 1 simultaneously:
Table 1: injection molding and the dry-pressing formed performance perameter comparison preparing dielectric resonator
The dielectric resonator that as can be seen from Table 1 prepared by injection molding is more excellent than performance prepared by conventional dry platen press, and stable performance.
Embodiment two
The present embodiment main material formula adopts chemical formula: Ba2Ti9O20+ 1mol%ZrO2For chemistry composition, compare dry pressing respectively and the performance of dielectric resonator prepared by injection molding method, the dielectric properties relative permittivity �� of the present embodiment main material itselfrBeing 39, quality factor (Q �� f) value is 50070GHz, temperature coefficient of resonance frequency ��fFor-5ppm/ DEG C. Dry pressing is mainly through, after granulation, compression moulding, carrying out sintering and obtain dielectric resonator, and technique is simple. Injection molding technique prepares Ba2Ti9O20Base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder body and organic binder bond: in the injection molding mixture of this embodiment, Ba2Ti9O20The weight percentage of based ceramic powder body is 75%, and the weight percentage of organic binder bond is 25%; In organic binder bond, each composition weight percentage composition is binding agent 80%; Tensio-active agent 5%; Low melting point organism 10%; Softening agent 5%.
(2) injection molding: injection molding mixture injection molding on injection moulding machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank.
(3) non-polar solvent extraction degreasing: base substrate injection molding obtained puts into non-polar solvent, dissolve de-except part organic binder bond, the temperature of non-polar solvent is 30 DEG C, and degreasing time is 24 hours, and the base substrate after non-polar solvent extraction degreasing is dried in an oven.
(4) thermal debinding: dried base substrate is put into electrical heater and carries out thermal debinding, with de-except remaining organic binder bond, in this embodiment, be warming up to 550 DEG C with the temperature rise rate of 0.5 DEG C/min, be incubated 2 hours.
(5) sinter: the base substrate after thermal debinding sinters, and sintering temperature is 1400 DEG C, is incubated 2 hours, obtains dielectric resonator.
Preparing 60 dielectric resonators with dry-pressing and injection molding technique respectively, and the performance of sample tested, performance is such as table 2:
Table 2: injection molding and the dry-pressing formed performance perameter comparison preparing dielectric resonator
Embodiment three
The present embodiment main material formula adopts chemical formula: Ba2Ti9O20+ 2mol%ZrO2For chemistry composition, compare dry pressing respectively and the performance of dielectric resonator prepared by injection molding method, the dielectric properties relative permittivity �� of the present embodiment main material itselfrBeing 40, quality factor (Q �� f) value is 56000GHz, temperature coefficient of resonance frequency ��fFor+2ppm/ DEG C. Dry pressing is mainly through, after granulation, compression moulding, carrying out sintering and obtain dielectric resonator, and technique is simple. Injection molding technique prepares Ba2Ti9O20Base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder body and organic binder bond: in the injection molding mixture of this embodiment, Ba2Ti9O20The weight percentage of based ceramic powder body is 75%, and the weight percentage of organic binder bond is 25%; In organic binder bond, each composition weight percentage composition is binding agent 80%; Tensio-active agent 5%; Low melting point organism 10%; Softening agent 5%.
(2) injection molding: injection molding mixture injection molding on injection moulding machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank.
(3) non-polar solvent extraction degreasing: base substrate injection molding obtained puts into non-polar solvent, dissolve de-except part organic binder bond, the temperature of non-polar solvent is 30 DEG C, and degreasing time is 24 hours, and the base substrate after non-polar solvent extraction degreasing is dried in an oven.
(4) thermal debinding: dried base substrate is put into electrical heater and carries out thermal debinding, with de-except remaining organic binder bond, in this embodiment, be warming up to 550 DEG C with the temperature rise rate of 0.5 DEG C/min, be incubated 2 hours.
(5) sinter: the base substrate after thermal debinding sinters, and sintering temperature is 1400 DEG C, is incubated 4 hours, obtains dielectric resonator.
Preparing 60 dielectric resonators with dry-pressing and injection molding technique respectively, and the performance of sample tested, performance is such as table 3:
Table 3: injection molding and the dry-pressing formed performance perameter comparison preparing dielectric resonator
Ba provided by the invention2Ti9O20The preparation method of base microwave medium ceramic material resonator, by by Ba2Ti9O20Base media ceramic injection molding, it is possible to obtaining having the resonator that dimensional precision after density and even size distribution, sintering is high, and material cost is low, preparation technology is simple. Compared with resonator prepared by dry-pressing, also there is high quality factor q �� f value and stability.
In addition, the embodiment of the present invention also provides a kind of resonator and a kind of cavity body filter, and this resonator is obtained by the preparation method described in above-described embodiment. From the correlation data above-described embodiment it will be seen that prepare Ba with dry pressing and injection moulding method respectively2Ti9O20The dielectric resonator of sill, the Q value of dielectric resonator prepared by dry pressing is 3500��4200, and frequency is 1.6G, and dielectric resonator Q value prepared by injection molding can reach 3900��4300, and frequency is 1.6G. It may be seen that the present invention utilizes Ba prepared by injection molding2Ti9O20The dielectric resonator Q value of sill is higher, and performance is more stable.
Cavity body filter comprises the resonator in above-described embodiment, having the advantage such as higher quality factor q �� f value and lower temperature coefficient of resonance frequency (�� f) by this resonator, the cavity body filter making it to prepare has preferably dielectric properties and stability. And about the technology feature of structure and parameters of other parts of cavity body filter within the scope of the understanding of those skilled in the art, repeat no more herein.
Referring to Fig. 4, Fig. 4 is the structure composition frame chart of radio frequency remote equipment one preferred embodiment of the present invention, and this radio frequency remote equipment includes but 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 connected with power amplifier module 520, and power amplifier module 520 is connected with cavity body filter 530 further.
When radio frequency remote equipment is operated in descending time slot, transmitting signal from two passages of RF transceiver module 510 enters cavity body filter 530 by power amplifier module 520, transmitting signal is completed filtering by cavity body filter 530, is then transmitted into antenna opening after power combing; When radio frequency remote equipment is operated in ascending time slot, the signal received from antenna opening, by entering power amplifier module 520 after cavity body filter 530 filtering, is exporting to the reception channel of RF transceiver module 510 correspondence through power amplifier module 520 after amplifying.
Further, this radio frequency remote equipment can also comprise power supply module 540, and this power supply module 540 is for each module for power supply to this radio frequency remote equipment.
The foregoing is only the part embodiment of the present invention; not thereby limit the scope of the invention; every utilize specification sheets of the present invention and accompanying drawing content to do equivalent device or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, all it is included in the scope of patent protection of the present invention with reason.
Claims (20)
1. a Ba2Ti9O20The preparation method of base microwave medium ceramic material, it is characterised in that, described preparation method comprises:
Prepare compound, described compound at least comprises Ba2Ti9O20Based ceramic powder body and organic binder bond;
By described compound injection molding, obtain base substrate;
Described idiosome is successively carried out non-polar solvent extraction degreasing and thermal debinding;
Base substrate after thermal debinding is sintered, to obtain described Ba2Ti9O20Base microwave dielectric ceramics.
2. preparation method according to claim 1, it is characterised in that, the Ba in described compound2Ti9O20The weight percentage of based ceramic powder body is 76��85%, and the weight percentage of described organic binder bond is 15��24%.
3. preparation method according to claim 2, it is characterised in that, described Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, wherein x, y at least comprise MoO3��MnO2��WO3��SnO2��B2O3��ZnO��Nb2O5��ZrO2��CaCO3��SrCO3��PbCO3In one or more, 0��a, b��0.20mol.
4. preparation method according to claim 1, it is characterised in that, described organic binder bond comprises binding agent, tensio-active agent, low melting point organism and softening agent.
5. preparation method according to claim 1, it is characterised in that, described injection molding for compound step is comprised:
Described compound is heated into toughness melt in injection moulding machine;
Being injected by described toughness melt in mould, in mould, after cooling, the demoulding obtains base substrate;
Wherein, injection temperature is 170 DEG C��200 DEG C.
6. preparation method according to claim 1, it is characterised in that, the non-polar solvent extraction skimming processes of described idiosome specifically comprises:
Base substrate injection molding obtained puts into non-polar solvent, de-except part organic binder bond to dissolve;
Non-polar solvent extracts the base substrate after degreasing be dried.
7. preparation method according to claim 6, it is characterized in that, thermal debinding will be proceeded via the idiosome that non-polar solvent extracts degreasing also dry, with de-except remaining organic binder bond in idiosome, the process of described thermal debinding is: with the temperature rise rate of 0.5��5 DEG C/min, idiosome is warming up to 550 DEG C, is then incubated 2��3 hours.
8. preparation method according to claim 1, it is characterised in that, the temperature of described sintering is 1200��1400 DEG C, is incubated 2��6 hours after heating.
9. preparation method according to claim 6, it is characterised in that, the temperature of the non-polar solvent in described idiosome non-polar solvent extraction skimming processes is 30��50 DEG C, and degreasing time is 12��36 hours; The temperature being dried after degreasing is 50��70 DEG C, and time of drying is 4��12h.
10. preparation method according to claim 4, it is characterised in that, in described organic binder bond, the weight percentage of each component is: binding agent 50��90%; Tensio-active agent 1��5%; Low melting point organism 2��11% and softening agent 1��11%.
11. preparation methods according to claim 10, it is characterized in that, described binding agent at least comprises one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, Atactic Polypropelene, polystyrene, polymethacrylate, ethylene ethyl acrylate copolymer; Described tensio-active agent at least comprises one or more in stearic acid, sad, microcrystalline wax; Described softening agent at least comprises one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.
12. 1 kinds of Ba2Ti9O20Base microwave medium ceramic material, it is characterised in that, described microwave dielectric ceramic materials comprises the Ba that weight percentage is 76��85%2Ti9O20Based ceramic powder body and weight percentage are the organic binder bond of 15��24%.
13. microwave dielectric ceramic materials according to claim 12, it is characterised in that, described Ba2Ti9O20The formula chemical formula of based ceramic powder body is Ba2Ti9O20+ ax+by, wherein x, y at least comprise MoO3��MnO2��WO3��SnO2��B2O3��ZnO��Nb2O5��ZrO2��CaCO3��SrCO3��PbCO3In one or more, 0mol��a, b��0.20mol.
14. microwave dielectric ceramic materials according to claim 12, it is characterised in that, described organic binder bond comprises binding agent, tensio-active agent, low melting point organism and softening agent.
15. microwave dielectric ceramic materials according to claim 14, it is characterised in that, in described organic binder bond, the weight percentage of each component is: binding agent 50��90%; Tensio-active agent 1��5%; Low melting point organism 2��11% and softening agent 1��11%.
16. microwave dielectric ceramic materials according to claim 14, it is characterized in that, described binding agent at least comprises one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, Atactic Polypropelene, polystyrene, polymethacrylate, ethylene ethyl acrylate copolymer; Described tensio-active agent at least comprises one or more in stearic acid, sad, microcrystalline wax; Described softening agent at least comprises one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.
17. 1 kinds of resonators, it is characterised in that, described resonator is obtained by the preparation method described in the arbitrary item of claim 1-11.
18. 1 kinds of cavity body filters, it is characterised in that, described cavity body filter comprises cavity, cover plate and resonator according to claim 17, and the described cover plate envelope described cavity of lid is to form resonator cavity, and described resonator is arranged in described cavity.
19. 1 kinds of radio frequency remote equipments, it is characterized in that, described radio frequency remote equipment comprises: RF transceiver module, power amplifier module and cavity body filter according to claim 18, described RF transceiver module is connected with described power amplifier module, and described power amplifier module is connected with described cavity body filter.
20. 1 kinds of Ba2Ti9O20The formula of base microwave medium ceramic material, it is characterised in that, comprise the component of following weight percentage:
Ba2Ti9O20Based ceramic powder body 76��85%;
Organic binder bond 15��24%.
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