CN105732021A - Ceramic material, preparation method thereof, resonator, filter, and radio remote equipment - Google Patents

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

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CN105732021A
CN105732021A CN201511027978.8A CN201511027978A CN105732021A CN 105732021 A CN105732021 A CN 105732021A CN 201511027978 A CN201511027978 A CN 201511027978A CN 105732021 A CN105732021 A CN 105732021A
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bati
preparation
resonator
organic binder
binder bond
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CN105732021B (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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Abstract

The invention provides a BaTi4O9 base microwave medium ceramic material, a preparation method thereof, a resonator, a filter, and radio remote equipment. The preparation method of the medium ceramic material comprises the following steps: preparing a mixed material, which at least comprises BaTi4O9 base ceramic powder and an organic adhesive; subjecting the mixed material to an injection moulding treatment to obtain a blank; subjecting the blank to non-polar solvent extraction degreasing and thermal degreasing in sequence; and after thermal degreasing, sintering the blank to obtain the BaTi4O9 base microwave medium ceramic. According to the preparation method, an injection moulding technology is used to obtain the medium ceramic material, which has the advantages of uniform density and size distribution, and high size precision after sintering, moreover, the material cost is low, and the preparation technology is simple. Compared with the resonator prepared through a dry pressing technology, the provided resonator has a higher quality factor (Q*f) value and more stable property.

Description

Ceramic material and preparation method thereof, resonator, wave filter and radio frequency remote equipment
Technical field
The present invention relates to the technical field of dielectric resonator, be specifically related to a kind of microwave dielectric ceramic materials and preparation method thereof, resonator, cavity body filter and radio frequency remote equipment.
Background technology
Dielectric resonator is a most basic microwave component, dielectric resonator is utilized to may be constructed the microwave circuits such as wave filter, agitator and antenna, it is widely used in the modern communicationses such as mobile communication, satellite communication, military radar, global positioning system, Bluetooth technology, WLAN, is the key foundation device of modern communication technology.It is applied to the dielectric resonator of microwave circuit, except indispensable mechanical strength, also needs to meet following dielectric properties and require: (1) has of a relatively high DIELECTRIC CONSTANT ε at microwave frequenciesr, generally require εr> 20, in order to microwave device miniaturization, integrated;(2) having extremely low dielectric loss under microwave resonance frequency, namely significantly high quality factor (Q × f), to ensure excellent selecting frequency characteristic and to reduce device insertion loss in high frequency;(3) close to the temperature coefficient of resonance frequency (τ of zerof), to ensure device high stability of resonant frequency in variations in temperature environment.
Mhaisalkar et al.[1]Report BaTi4O9The dielectric properties of material: εr=37, Q × f=22700GHz, τf=+15ppm/ DEG C.Mhaisalkar et al.[1]Also studied alloy such as Mn, Sn, Zr, Ca, Sr, Pb to BaTi4O9The impact of dielectric properties.Result of study shows that doping Mn, Sn, Pb can seriously reduce Q × f value, and adulterate Zr, Ca, Sr then can increase Q × f value.Due to BaTi4O9Pottery has high positive temperature coefficient of resonance frequency τf(+15ppm/ DEG C) is so limiting its practical application.
Performance requirement according to dielectric resonator, to BaTi4O9Add different compounds.Prepare BaTi at present4O9Base medium ceramic material resonator is mainly dry pressing.The document quoted is as follows:
[1]S.G.Mhaisalker,D.W.Readey,S.A.Akbar,MicrowavedielectricpropertiesofdopedBaTi4O9,J.Am.Ceram.Soc.,741894-1898(1991).
Currently with BaTi prepared by dry pressing4O9Base medium ceramic material resonator DIELECTRIC CONSTANT εrRelatively low, it is unfavorable for microwave device miniaturization, integrated;Quality factor are relatively low, thus dielectric loss is higher, and temperature coefficient of resonance frequency (τf) higher, it is impossible to ensure device high stability of resonant frequency in variations in temperature environment.Therefore, BaTi prepared by dry pressing is utilized4O9Base medium ceramic material resonator dielectric properties are poor.
Although injection molding research and be applied in continuous development, again to pottery (being mainly used in structural ceramics, aluminium oxide, zirconium oxide etc.) from polymer to metal.But for media ceramic resonator injection moulding study and produce almost without.Moulding process of the prior art is mainly dry-pressing formed.Dry-pressing formed principle is: to media ceramic powder adding additives pelletize, be pressed by mould after be sintered.This technique is prepared dielectric resonator and is had a disadvantage in that in (1) compressing process, the inside and outside friction existed between granule and between granule and die wall causes the pressure loss 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 of selection, conventional pressing mode has unidirectional compacting and two-way compacting, as seen in figure la and lb, the uniformity of density can affect the dielectric properties of dielectric resonator to its Density Distribution situation, and then also can affect the service behaviour of wave filter;(2) it is limited to pressing mode, dielectric resonator major part is column (or analogous shape), not all geomery can be prepared by dry pressing, the such as complex-shaped resonator demoulding is difficult to, the resonator that draw ratio is big also cannot pass through to suppress to prepare, because easily there is low density area because of Density inhomogeneity, and then causes resonator deformation in sintering process, make low precision, also need to be machined out obtaining to obtain the shape wanted or size.
In sum, microwave-medium ceramics prepared by the dry pressing generally adopted in prior art, there is the Density inhomogeneity of prepared microwave dielectric ceramic materials resonator, cause that microwave dielectric ceramic materials resonator dielectric properties are poor;Meanwhile, dry pressing cannot prepare complex-shaped resonator.
Summary of the invention
The embodiment of the present invention provides a kind of BaTi4O9Base microwave medium ceramic material resonator and preparation method thereof, to solve the density unevenness of microwave-medium ceramics adopting dry pressing to prepare in prior art, causes using this microwave-medium ceramics to make the technical problem that the dielectric properties of resonator are poor
For solving the problems referred to above, one aspect of the present invention provides a kind of BaTi4O9Preparation method described in the preparation method of base microwave medium ceramic material resonator includes:
Prepare compound, described compound at least includes BaTi4O9Based ceramic powder body and organic binder bond;
By described compound injection moulding, obtain base substrate;
Described idiosome is successively carried out nonpolar solvent extraction defat and thermal debinding;
Base substrate after thermal debinding is sintered, to obtain described BaTi4O9Base microwave dielectric ceramics.
According to one preferred embodiment of the present invention, the BaTi in described compound4O9The 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 BaTi4O9The formula chemical formula of based ceramic powder body is BaTi4O9+ ax+by, wherein x, y at least include MoO3、MnO2、WO3、SnO2、B2O3、ZnO、Nb2O5、ZrO2、CaCO3、SrCO3、PbCO3In one or more, 0.005mol≤a, b≤0.20mol.
According to one preferred embodiment of the present invention, described organic binder bond includes binding agent, surfactant, low melting point Organic substance and plasticizer.
According to one preferred embodiment of the present invention, described injection molding for compound step is included:
Described compound is heated into toughness melt in injection (mo(u)lding) 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 nonpolar solvent extraction skimming processes of described idiosome specifically includes:
Base substrate injection moulding obtained is put in non-polar solven, to dissolve elimination part organic binder bond;
Base substrate after nonpolar solvent extraction defat is dried.
According to one preferred embodiment of the present invention, thermal debinding will be proceeded via nonpolar solvent extraction defat dry idiosome, to remove remaining organic binder bond in idiosome, the process of described thermal debinding is: with the heating 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 solven in described idiosome nonpolar solvent extraction skimming processes is 30~50 DEG C, and degreasing time is 12~36 hours;The temperature being dried after defat is 50~70 DEG C, and drying time 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%;Surfactant 1~5%;Low melting point Organic substance 2~11% and plasticizer 1~11%.
According to one preferred embodiment of the present invention, described binding agent at least includes one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer;Described surfactant at least includes one or more in stearic acid, sad, microcrystalline wax;Described plasticizer at least includes one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.
For solving above-mentioned technical problem, second aspect present invention provides a kind of BaTi4O9Base microwave medium ceramic material, described microwave dielectric ceramic materials includes the BaTi that weight percentage is 76~85%4O9Based ceramic powder body and weight percentage are the organic binder bond of 15~24%.
According to one preferred embodiment of the present invention, described BaTi4O9The formula chemical formula of based ceramic powder body is BaTi4O9+ ax+by, wherein x, y at least include MoO3、MnO2、WO3、SnO2、B2O3、ZnO、Nb2O5、ZrO2、CaCO3、SrCO3、PbCO3In one or more, 0.005mol≤a, b≤0.20mol.
According to one preferred embodiment of the present invention, described organic binder bond includes binding agent, surfactant, low melting point Organic substance and plasticizer.
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%;Surfactant 1~5%;Low melting point Organic substance 2~11% and plasticizer 1~11%.
According to one preferred embodiment of the present invention, described binding agent at least includes one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer;Described surfactant at least includes one or more in stearic acid, sad, microcrystalline wax;Described plasticizer at least includes 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 preparation method described in any one in above-described embodiment prepares.
Fourth aspect present invention provides a kind of cavity body filter, and described cavity body filter includes the resonator in cavity, cover plate and the third aspect, and described cover plate covers described cavity 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 includes: 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 BaTi4O9The formula of base microwave medium ceramic material, this formula includes the component of following weight percentage: BaTi4O9Based ceramic powder body 76~85%;Organic binder bond 15~24%.
Relative to prior art, BaTi provided by the invention4O9The preparation method of base microwave medium ceramic material and resonator thereof, by by BaTi4O9Base media ceramic injection moulding, the microwave dielectric ceramic materials of density and even size distribution can be obtained, use the resonator not only dimensional accuracy that this microwave dielectric ceramic materials is made high, also there is the advantages such as higher dielectric constant, higher quality factor q × f value and relatively low temperature coefficient of resonance frequency (τ f), and then make the cavity body filter prepared have preferably dielectric properties and stability.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme in the embodiment of the present invention, below the accompanying drawing used required during embodiment is 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 premise 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 BaTi of the present invention4O9The schematic flow sheet of preparation method one preferred embodiment of base microwave medium ceramic material resonator;
Fig. 3 a is the BaTi of dry-pressing formed preparation4O9Electron microscope scanning figure after the corrosion of base dielectric resonator port;
Fig. 3 b is BaTi prepared by injection moulding4O9Electron 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.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.It is emphasized that following example are merely to illustrate the present invention, but the scope of the present invention is not defined.Same, following example are only the section Example of the present invention and not all embodiments, all other embodiments that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
Referring to Fig. 2, Fig. 2 is BaTi of the present invention4O9The schematic flow sheet of preparation method one preferred embodiment of base microwave medium ceramic material;This preparation method includes but not limited to following steps:
Step S100, prepares compound.Compound at least includes BaTi4O9Based ceramic powder body and organic binder bond.
In the present embodiment, by BaTi4O9Based ceramic powder body and organic binder bond mix on mixing roll, until mix homogeneously, it is preferable that incorporation time is 4~8h, obtains injection molding mixture, in batch mixing, the content of heterogeneity is relevant with the granularity of powder, pattern, density, so its design of mixture of different powder is different;It is directed to the BaTi in the present invention4O9Base media ceramic, in injection molding mixture, BaTi4O9The 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 BaTi4O9BaTi prepared by the configuration mode of based ceramic powder body4O9Base microwave dielectric ceramics, has excellent dielectric properties and quality stability.
Wherein, BaTi4O9The formula chemical formula of based ceramic powder body is BaTi4O9+ ax+by, x, y at least include MoO3、MnO2、WO3、SnO2、B2O3、ZnO、Nb2O5、ZrO2、CaCO3、SrCO3、PbCO3In one or more, and the span of a, the b in chemical formula be preferably: 0.005mol≤a, b≤0.20mol.Utilize the BaTi of the stoichiometric factor of chemical formula in the present invention4O9Based ceramic powder body, it is possible to make the microwave dielectric ceramic materials that injection moulding obtains have higher dielectric constant, higher quality factor q × f value and relatively low temperature coefficient of resonance frequency (τ f).
This wherein, BaTi4O9The formula of base determines and prepares mainly through solid phase method that dispensing in proportion is generally BaCO3And TiO2Carry out proportioning according to the ratio of 1:4 to be obtained by reacting, afterwards then through ball milling, calcining (calcining heat 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, Ball-milling Time is 4~12h, mechanical milling process adds PVA (polyvinyl alcohol) binding agent of 2%~5%, through carrying out pelletize on spray tower, then prilling powder is put into (pressure is 100MPa~200MPa) after mould is pressed and carries out the calcining test performance of material own, eventually pass through and after grinder grinds, obtain required BaTi4O9Base microwave dielectric material.
This organic binder bond can include binding agent, surfactant, low melting point Organic substance and plasticizer etc..Wherein, in organic binder bond, the weight percentage of each component is preferably: binding agent 50~90%;Surfactant 1~5%;Low melting point Organic substance 2~11% and plasticizer 1~11%.
It is further preferred that binding agent at least includes one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer;Surfactant at least includes one or more in stearic acid, sad, microcrystalline wax;Plasticizer at least includes one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.Carry out Rational choice from the kind of multiple binding agent provided above, meet material function at the same time it can also be save certain cost.
Step S200, by compound injection moulding, obtains base substrate.
Step S200 farther includes: compound is heated into toughness melt in injection (mo(u)lding) 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 cool time, it is possible to make the density of microwave dielectric ceramic materials that obtains and distribution of sizes more uniform, and then performance is more stable.
Step S300, successively carries out nonpolar solvent extraction defat and thermal debinding by idiosome.
Nonpolar solvent extraction skimming processes is as follows: base substrate injection moulding obtained is put in the non-polar solvens such as gasoline, Carbon bisulfide, dimethylbenzene, ether, stupid, chloroform, carbon tetrachloride, Petroleum, to dissolve elimination part organic binder bond, the temperature of non-polar solven is preferably controlled between 30~50 DEG C, and degreasing time was at 12~36 hours.Base substrate after nonpolar solvent extraction defat is fully dry in an oven, and baking temperature is preferably 50~70 DEG C, and the time is 4~12h.
Nonpolar solvent extraction skimming processes in this step is very important, because if being made directly, heat is de-owing in idiosome, organic binder bond composition is too high, and causes sample fragmentation in skimming processes.
Thermal debinding process is as follows: dried base substrate is put into electric furnace and carries out thermal debinding, to remove remaining organic binder bond.This process is preferably and with the heating rate of 0.5~5 DEG C/min, idiosome is warming up to 550 DEG C, is then incubated 2~3 hours.Heating rate in this step and temperature retention time parameter, under the premise meeting production efficiency, it can be ensured that make the microwave dielectric ceramic materials compact structure obtained, occur without crackle, the stability of further improving performance.
Step S400, is sintered the base substrate after thermal debinding, to obtain BaTi4O9Base microwave dielectric ceramics.
In this step, sintering temperature is preferably between 1200~1400 DEG C, being incubated 2~6 hours.
Present invention injection moulding prepares BaTi4O9Base microwave medium ceramic material, by by BaTi4O9Base media ceramic injection moulding, the microwave dielectric ceramic materials of density and even size distribution can be obtained, use the resonator not only dimensional accuracy that this microwave dielectric ceramic materials makes high, also there is the advantages such as higher dielectric constant, higher quality factor q × f value and relatively low temperature coefficient of resonance frequency (τ f).
Several specific embodiments describe BaTi in the present invention in detail below4O9The performance parameter of base microwave medium ceramic material resonator manufacturing process and finished product resonator.
Embodiment one
The present embodiment main material formula adopts chemical formula: BaTi4O9+ 0.5mol%MoO3For chemical composition, it is respectively compared dry pressing and the performance of dielectric resonator prepared by injection moulding, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrBeing 37, quality factor (Q × f) value is 45000GHz, temperature coefficient of resonance frequency τfFor+5ppm/ DEG C.Injection molding technique prepares BaTi4O9Base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder body and organic binder bond: by BaTi4O9Based ceramic powder body and organic binder bond mix homogeneously obtain injection molding mixture, and in batch mixing, the content of heterogeneity is relevant with the granularity of powder, pattern, density, so its design of mixture of different powder is different;It is directed to BaTi4O9Base media ceramic, in described injection molding mixture, BaTi4O9The weight percentage of based ceramic powder body is 80%, and the weight percentage of organic binder bond is 20%;Wherein, organic binder bond is made up of binding agent, surfactant, low melting point Organic substance and plasticizer, and each composition weight percentage composition is: binding agent 80%;Surfactant 5%;Low melting point Organic substance 10%;Plasticizer 5%.
(2) injection moulding: injection molding mixture injection moulding on injection (mo(u)lding) machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank.
(3) nonpolar solvent extraction defat: base substrate injection moulding obtained is put in non-polar solven, dissolve elimination part organic binder bond, the temperature of non-polar solven is 30 DEG C, and degreasing time is 24 hours, and the base substrate after nonpolar solvent extraction defat is dried in an oven.
(4) thermal debinding: dried base substrate is put into electric furnace and carries out thermal debinding, to remove remaining organic binder bond, in this embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is incubated 2 hours.
(5) sintering: the base substrate after thermal debinding is sintered, and sintering temperature is 1350 DEG C, is incubated 4 hours, obtains dielectric resonator.
Prepare 60 dielectric resonators with dry-pressing and injection molding technique respectively, sample as it is shown on figure 3,
As can be seen from Figure 3, compared with injection moulding is prepared with dry pressing, crystallite dimension is more uniform, and particle size is less, and this is for BaTi4O9Performance that base dielectric resonator product is final and stability influence correlation.The performance of sample being tested, performance is table 1 such as simultaneously:
Table 1: injection moulding and the dry-pressing formed performance parameter comparison preparing dielectric resonator
The dielectric resonator that as can be seen from Table 1 prepared by injection moulding 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: BaTi4O9+ 5mol%MoO3For chemical composition, it is respectively compared dry pressing and the performance of dielectric resonator prepared by injection moulding, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrBeing 36.4, quality factor (Q × f) value is 53050GHz, temperature coefficient of resonance frequency τfFor+2ppm/ DEG C.Injection molding technique prepares BaTi4O9Base 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, BaTi4O9The weight percentage of based ceramic powder body is 76%, and the weight percentage of organic binder bond is 24%;In organic binder bond, each composition weight percentage composition is binding agent 80%;Surfactant 5%;Low melting point Organic substance 10%;Plasticizer 5%.
(2) injection moulding: injection molding mixture injection moulding on injection (mo(u)lding) machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank.
(3) nonpolar solvent extraction defat: base substrate injection moulding obtained is put in non-polar solven, dissolve elimination part organic binder bond, the temperature of non-polar solven is 30 DEG C, and degreasing time is 24 hours, and the base substrate after nonpolar solvent extraction defat is dried in an oven.
(4) thermal debinding: dried base substrate is put into electric furnace and carries out thermal debinding, to remove remaining organic binder bond, in this embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is incubated 2 hours.
(5) sintering: the base substrate after thermal debinding is sintered, and sintering temperature is 1340 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 is tested, performance is table 2 such as:
Table 2: injection moulding and the dry-pressing formed performance parameter comparison preparing dielectric resonator
Embodiment three
The present embodiment main material formula adopts chemical formula: BaTi4O9+ 10mol%MoO3For chemical composition, it is respectively compared dry pressing and the performance of dielectric resonator prepared by injection moulding, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrBeing 35, quality factor (Q × f) value is 69200GHz, temperature coefficient of resonance frequency τfFor-3ppm/ DEG C.Injection molding technique prepares BaTi4O9Base 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, BaTi4O9The 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%;Surfactant 5%;Low melting point Organic substance 10%;Plasticizer 5%.
(2) injection moulding: injection molding mixture injection moulding on injection (mo(u)lding) machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank.
(3) nonpolar solvent extraction defat: base substrate injection moulding obtained is put in non-polar solven, dissolve elimination part organic binder bond, the temperature of non-polar solven is 30 DEG C, and degreasing time is 24 hours, and the base substrate after nonpolar solvent extraction defat is dried in an oven.
(4) thermal debinding: dried base substrate is put into electric furnace and carries out thermal debinding, to remove remaining organic binder bond, in this embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is incubated 2 hours.
(5) sintering: the base substrate after thermal debinding is sintered, and sintering temperature is 1340 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 is tested, performance is table 3 such as:
Table 3: injection moulding and the dry-pressing formed performance parameter comparison preparing dielectric resonator
The dielectric resonator that as can be seen from Table 3 prepared by injection moulding is more excellent than performance prepared by conventional dry platen press, and stable performance.
Embodiment four
The present embodiment main material formula adopts chemical formula: BaTi4O9+ 10mol%MoO3+ 0.5mol%B2O3For chemical composition, it is respectively compared dry pressing and the performance of dielectric resonator prepared by injection moulding, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrBeing 34, quality factor (Q × f) value is 61000GHz, temperature coefficient of resonance frequency τfFor-1.5ppm/ DEG C.Dry pressing mainly through pelletize, compressing after, be sintered obtaining dielectric resonator, technique is simple.Injection molding technique prepares BaTi4O9Base 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, BaTi4O9The 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%;Surfactant 5%;Low melting point Organic substance 10%;Plasticizer 5%.
(2) injection moulding: injection molding mixture injection moulding on injection (mo(u)lding) machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank.
(3) nonpolar solvent extraction defat: base substrate injection moulding obtained is put in non-polar solven, dissolve elimination part organic binder bond, the temperature of non-polar solven is 30 DEG C, and degreasing time is 24 hours, and the base substrate after nonpolar solvent extraction defat is dried in an oven.
(4) thermal debinding: dried base substrate is put into electric furnace and carries out thermal debinding, to remove remaining organic binder bond, in this embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is incubated 2 hours.
(5) sintering: the base substrate after thermal debinding is sintered, and sintering temperature is 1150 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 is tested, performance is table 4 such as:
Table 4: injection moulding and the dry-pressing formed performance parameter comparison preparing dielectric resonator
Embodiment five
The present embodiment main material formula adopts chemical formula: 0.62molBaTi4O9+0.35molZnO+0.03molNb2O5For chemical composition, it is respectively compared dry pressing and the performance of dielectric resonator prepared by injection moulding, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrBeing 36.4, quality factor (Q × f) value is 45500GHz, temperature coefficient of resonance frequency τfFor+0ppm/ DEG C.Injection molding technique prepares BaTi4O9Base 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, BaTi4O9The weight percentage of based ceramic powder body is 85%, and the weight percentage of organic binder bond is 15%;In organic binder bond, each composition weight percentage composition is: binding agent 80%;Surfactant 3%;Low melting point Organic substance 11%;Plasticizer 6%.
(2) injection moulding: injection molding mixture injection moulding on injection (mo(u)lding) machine obtains base substrate, injection temperature is 180 DEG C, and after injecting mould, in 2 minutes, the demoulding obtains molding blank.
(3) nonpolar solvent extraction defat: base substrate injection moulding obtained is put in non-polar solven, dissolve elimination part organic binder bond, the temperature of non-polar solven is 30 DEG C, and degreasing time is 24 hours, and the base substrate after nonpolar solvent extraction defat is dried in an oven.
(4) thermal debinding: dried base substrate is put into electric furnace and carries out thermal debinding, to remove remaining organic binder bond, in this embodiment, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is incubated 2 hours.
(5) sintering: the base substrate after thermal debinding is sintered, and sintering temperature is 1275 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 is tested, performance is table 5 such as:
Table 5: injection moulding and the dry-pressing formed performance parameter comparison preparing dielectric resonator
BaTi provided by the invention4O9The preparation method of base microwave medium ceramic material resonator, by by BaTi4O9Base media ceramic injection moulding, it is possible to obtaining having the resonator that dimensional accuracy after density and even size distribution, sintering is high, and the cost of material is low, preparation technology is simple.Compared with resonator prepared by dry-pressing, also there is high quality factor q × f value and stability.
It addition, the embodiment of the present invention also provides for a kind of resonator and a kind of cavity body filter, this resonator preparation method described in above-described embodiment prepares.Correction data in from the above is it can be seen that prepare BaTi with dry pressing and injection moulding method respectively4O9The dielectric resonator of sill, the Q-value of dielectric resonator prepared by dry pressing is 3300~3800, and frequency is 1.8G, and dielectric resonator Q-value prepared by injection moulding can reach 3800~4000, and frequency is 1.8G.It can be seen that the present invention utilizes BaTi prepared by injection moulding4O9The dielectric resonator Q-value of sill is higher, and performance is more stable.
Cavity body filter includes the resonator in above-described embodiment, be there is the advantages such as higher quality factor q × f value and relatively low temperature coefficient of resonance frequency (τ f) by this resonator, so as to the cavity body filter prepared has preferably dielectric properties and stability.And about the structure of other parts of cavity body filter and the technical characteristic of parameter within the scope of the understanding of those skilled in the art, repeat no more herein.
Referring to the structure composition frame chart that Fig. 4, Fig. 4 are radio frequency remote equipment one preferred embodiments of the present invention, this radio frequency remote equipment includes but not limited to following construction 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, cavity body filter 530 completes filtering to launching signal, 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 passes through to enter power amplifier module 520 after cavity body filter 530 filters, and is exporting to the reception passage of RF transceiver module 510 correspondence after amplifying through power amplifier module 520.
Further, this radio frequency remote equipment can also include power module 540, and this power module 540 is for powering to the modules of this radio frequency remote equipment.
The foregoing is only the section Example of the present invention; not thereby limit the scope of the invention; every equivalent device utilizing description of the present invention and accompanying drawing content to make or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, all in like manner include in the scope of patent protection of the present invention.

Claims (20)

1. a BaTi4O9The preparation method of base microwave medium ceramic material, it is characterised in that described preparation method includes:
Prepare compound, described compound at least includes BaTi4O9Based ceramic powder body and organic binder bond;
By described compound injection moulding, obtain base substrate;
Described idiosome is successively carried out nonpolar solvent extraction defat and thermal debinding;
Base substrate after thermal debinding is sintered, to obtain described BaTi4O9Base microwave dielectric ceramics.
2. preparation method according to claim 1, it is characterised in that the BaTi in described compound4O9The 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 BaTi4O9The formula chemical formula of based ceramic powder body is BaTi4O9+ ax+by, wherein x, y at least include MoO3、MnO2、WO3、SnO2、B2O3、ZnO、Nb2O5、ZrO2、CaCO3、SrCO3、PbCO3In one or more, 0.005mol≤a, b≤0.20mol.
4. preparation method according to claim 1, it is characterised in that described organic binder bond includes binding agent, surfactant, low melting point Organic substance and plasticizer.
5. preparation method according to claim 1, it is characterised in that described injection molding for compound step is included:
Described compound is heated into toughness melt in injection (mo(u)lding) 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 nonpolar solvent extraction skimming processes of described idiosome specifically includes:
Base substrate injection moulding obtained is put in non-polar solven, to dissolve elimination part organic binder bond;
Base substrate after nonpolar solvent extraction defat is dried.
7. preparation method according to claim 6, it is characterized in that, thermal debinding will be proceeded via nonpolar solvent extraction defat dry idiosome, to remove remaining organic binder bond in idiosome, the process of described thermal debinding is: with the heating 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 solven in described idiosome nonpolar solvent extraction skimming processes is 30~50 DEG C, and degreasing time is 12~36 hours;The temperature being dried after defat is 50~70 DEG C, and drying time 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%;Surfactant 1~5%;Low melting point Organic substance 2~11% and plasticizer 1~11%.
11. preparation method according to claim 10, it is characterized in that, described binding agent at least includes one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer;Described surfactant at least includes one or more in stearic acid, sad, microcrystalline wax;Described plasticizer at least includes one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.
12. a BaTi4O9Base microwave medium ceramic material, it is characterised in that described microwave dielectric ceramic materials includes the BaTi that weight percentage is 76~85%4O9Based 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 BaTi4O9The formula chemical formula of based ceramic powder body is BaTi4O9+ ax+by, wherein x, y at least include MoO3、MnO2、WO3、SnO2、B2O3、ZnO、Nb2O5、ZrO2、CaCO3、SrCO3、PbCO3In one or more, 0.005mol≤a, b≤0.20mol.
14. microwave dielectric ceramic materials according to claim 12, it is characterised in that described organic binder bond includes binding agent, surfactant, low melting point Organic substance and plasticizer.
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%;Surfactant 1~5%;Low melting point Organic substance 2~11% and plasticizer 1~11%.
16. microwave dielectric ceramic materials according to claim 14, it is characterized in that, described binding agent at least includes one or more in paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates, ethylene ethyl acrylate copolymer;Described surfactant at least includes one or more in stearic acid, sad, microcrystalline wax;Described plasticizer at least includes one or more in dibutyl phthalate, diethyl phthalate, o-phthalic acid dibutyl ester.
17. a resonator, it is characterised in that described resonator preparation method described in any one of claim 1-11 prepares.
18. a cavity body filter, it is characterised in that described cavity body filter includes the resonator described in cavity, cover plate and claim 17, described cover plate covers described cavity to form resonator cavity, and described resonator is arranged in described cavity.
19. a radio frequency remote equipment, it is characterized in that, described radio frequency remote equipment includes: the cavity body filter described in RF transceiver module, power amplifier module and 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. a BaTi4O9The formula of base microwave medium ceramic material, it is characterised in that include the component of following weight percentage:
BaTi4O9Based ceramic powder body 76~85%;
Organic binder bond 15~24%.
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