CN107614461A - Ceramic material and preparation method thereof, resonator, wave filter and radio frequency remote equipment - Google Patents

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

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Publication number
CN107614461A
CN107614461A CN201580079830.0A CN201580079830A CN107614461A CN 107614461 A CN107614461 A CN 107614461A CN 201580079830 A CN201580079830 A CN 201580079830A CN 107614461 A CN107614461 A CN 107614461A
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organic binder
green body
degreasing
preparation
dielectric resonator
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庄后荣
陆正武
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Shenzhen Tatfook Technology Co Ltd
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Shenzhen Tatfook Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers

Abstract

The invention provides a kind of ceramic material and preparation method thereof, resonator, wave filter and radio frequency remote equipment.The composition of raw materials includes weight percentage for 76% 85% barium zinc niobium based ceramic powder body and 15% 24% organic binder bonds；The preparation method comprises the following steps：The barium zinc niobium based ceramic powder body and organic binder bond of above-mentioned formula are mixed to obtain mixed material；Mixed material is heated to form melt；Melt is injection moulded to obtain base substrate；Degreasing is carried out to base substrate；Base substrate after degreasing is sintered.The barium zinc niobium base dielectric resonator even density of the present invention, dimensional accuracy are high, have high-k and stability and plastic complex-shaped dielectric resonator.

Description

Ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment [technical field]
The present invention relates to the preparation technical fields of resonator, more particularly to a kind of ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment.
[background technique]
Dielectric resonator is a most basic microwave component, it may be constructed the microwave circuits such as filter, oscillator and antenna using dielectric resonator, it is widely used in the modern communications such as mobile communication, satellite communication, military radar, global positioning system, Bluetooth technology, WLAN, is the key foundation device of modern communication technology.Applied to the dielectric resonator of microwave circuit, other than indispensable mechanical strength, also needs to meet following dielectric properties requirement: (1) there is relatively high permittivity ε at microwave frequenciesr, generally require εr> 20, in order to microwave device miniaturization, it is integrated；(2) there is extremely low dielectric loss, i.e., very high quality factor (Q × f), to guarantee excellent selecting frequency characteristic and reduce the insertion loss of device in high frequency under microwave resonance frequency；(3) close to zero temperature coefficient of resonance frequency (τf), to guarantee the high stability of device resonance frequency in temperature change environment.
Barium zinc niobium ceramics (Ba (Zn1/3Nb2/3)O3, BZN) and there is complex perovskite structure, it is one kind in the very high microwave-medium ceramics of X-band (7~8GHz) Q value, it is extremely important dielectric material in the microwave high-frequencies such as satellite communication field.However, BZN ceramics have relatively high τfValue (~30ppm/ DEG C) limit its practical application.So far there are many researchers to reduce the τ of BZN by exploring a variety of different chemical formulationsfIt is worth zero.For example, in soluble solids (1-x) Ba (Zn1/3Nb2/3)O3-xSr(Zn1/3Nb2/3)O3It is middle to replace Ba to realize τ with part SrfValue is zero, at this time x=0.7, however as τfThe reduction Qf value of value also becomes smaller therewith.Reduce τfResearch also in (1-x) Ba (Zn1/3Nb2/3)O3-(x)Ba(Ni1/3Nb2/3)O3(BZN-BNN) and (1-x) Ba (Zn1/3Nb2/3)O3-(x)Ba(Co1/3Nb2/3)O3(BZN-BCoN) it is carried out in system.Pure phase Ba (Co1/3Nb2/3) O3 changes in 1425 DEG C of recurring structures, is transformed into from 1:2 ordered structure unordered Structure, transition temperature are more slightly higher than pure BZN (~1375 DEG C).So forming orderly solid solution phase in BZN-BCoN by 1300~1400 DEG C of long term annealing processing；Although the τ reported on documentfThe signal component value for being zero is less consistent, from x=0.4 to x=0.7.Ba(Ni1/3Nb2/3)O3Disordering temperature document on there is the value that contradicts, 1500 DEG C of > are changed to from 1400 DEG C.Usually there is secondary miscellaneous phase in the X-ray map of the phase, may melt or volatilize with the part NiO under high temperature and is related.The volatilization that conventional solid-state method component mixes Ni under uneven and high temperature may be the inconsistent reason of the system order.It is x=0.7 for (1-x) BZN-xBNN its tf signal component value for being zero, for the ceramics in 1500 DEG C of densified sintering products, Q value is~5700 (10GHz).
Although injection molding research and applying and constantly developing, again to ceramic (being mainly used in structural ceramics, aluminium oxide, zirconium oxide etc.) from polymer to metal.But for the injection moulding of barium zinc niobium base media ceramic resonator study and produce almost without.Moulding process in the prior art is mainly dry-pressing formed.Dry-pressing formed principle is: being sintered after media ceramic powder adding additives are granulated, are pressed by mold.This technique preparation media resonator has the following disadvantages: during (1) compression moulding, existing inside and outside rub causes the pressure loss to make each position unbalance stress of green compact 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 pressing mode has unidirectional compacting and two-way compacting, as seen in figure la and lb, the uniformity of density will affect the dielectric properties of dielectric resonator to its Density Distribution situation, and then also will affect the working performance of filter；(2) it is limited to pressing mode, dielectric resonator is largely column (or analogous shape), not all geomery can be prepared with dry pressing, for example complex-shaped resonator demoulding is difficult to realize, the big resonator of draw ratio can not be also made by suppressing, because being easy occur low density area because of Density inhomogeneity, and then resonator in sintering process be caused to deform, low precision is made, desired shape or size also need to be machined out acquisition in order to obtain.
In conclusion, there is the Density inhomogeneity of prepared microwave dielectric ceramic materials resonator, causing microwave dielectric ceramic materials resonator dielectric properties poor in the microwave-medium ceramics of the dry pressing preparation generallyd use in the prior art；Meanwhile dry pressing can not prepare complex-shaped resonator.
[summary of the invention]
The present invention provides a kind of ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment, It is able to solve the problem limited in the forming shape that the dry-pressing formed Density Distribution being easy to appear in the process is uneven, dimensional accuracy is low, quality factor q × f value is lower, performance is unstable and can prepare of barium zinc niobium base dielectric resonator in the prior art.
In order to solve the above technical problems, one technical scheme adopted by the invention is that: a kind of composition of raw materials of barium zinc niobium base dielectric resonator is provided, which includes the component of following weight percentage:
Barium zinc niobium based ceramic powder body 76%-85%；
Organic binder 15%-24%.
Wherein, the organic binder includes binder, surfactant and plasticizer；Weight percent of the binder in the organic binder is 50%-90%；Weight percent of the surfactant in the organic binder is 1%-5%；Weight percent of the plasticizer in the organic binder is 3%-22%.
Wherein, the binder is selected from least one of paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates and ethylene ethyl acrylate copolymer.
Wherein, the surfactant is selected from least one of stearic acid, octanoic acid and microcrystalline wax.
Wherein, the plasticizer is low melting point plasticizer.
Wherein, the plasticizer is selected from least one of dibutyl phthalate, diethyl phthalate and o-phthalic acid dibutyl ester.
To solve above-mentioned technical problem, another technical solution used in the present invention is: providing a kind of preparation method of barium zinc niobium base dielectric resonator, the preparation method is the following steps are included: mixing barium zinc niobium based ceramic powder body and organic binder to obtain mixed material, wherein, the weight percentage of the barium zinc niobium based ceramic powder body is 76%-85%, and the weight percentage of the organic binder is 15%-24%；The mixed material is heated, so that the mixed material forms melt；It is injection moulded the melt to obtain green body using injection (mo(u)lding) machine；Degreasing is carried out to the green body, to remove organic binder；Green body after degreasing is sintered to obtain dielectric resonator.
Wherein, in the step of barium zinc niobium based ceramic powder body and organic binder being mixed to obtain mixed material, the barium zinc niobium based ceramic powder body is mixed on kneading machine with the organic binder, incorporation time 4-8 Hour.
Wherein, the mixed material is heated, so that the heating temperature is 150 DEG C -250 DEG C in the step of mixed material forms melt.
Wherein, the melt was injection moulded in the step of obtaining green body using injection (mo(u)lding) machine, the melt is injected in metal die, cooling and demolding obtains the green body after 2-5 minutes.
Wherein, the step of carrying out degreasing to the green body includes: to carry out oil extraction degreasing to the green body；The green body after degreasing is extracted to oil and carries out thermal debinding.
Wherein, the step of carrying out oil extraction degreasing to the green body includes: that the green body is put into nonpolar solvent, and the temperature of the nonpolar solvent is 30-50 DEG C, degreasing time 12-36 hours；The green body is taken out from nonpolar solvent, is placed in baking oven and is dried, wherein drying temperature is 50-70 DEG C, drying time 4-12 hour.
Wherein, the nonpolar solvent is selected from least one of gasoline, carbon disulfide, dimethylbenzene, ether, benzene, chloroform, carbon tetrachloride and naphtha.
Wherein, oil is extracted in the step of green body after degreasing carries out thermal debinding, the green body is placed in electric furnace, be warming up to 500-600 DEG C with the heating rate of 0.5-5 DEG C/min, keep the temperature 2-3 hours.
Wherein, in the step of being sintered the green body after thermal debinding to obtain dielectric resonator, the sintering temperature is 900-1400 DEG C, keeps the temperature 2-6 hours.
Wherein, the organic binder includes binder, surfactant and plasticizer；Weight percent of the binder in the organic binder is 50%-90%；Weight percent of the surfactant in the organic binder is 1%-5%；Weight percent of the plasticizer in the organic binder is 3%-22%.
To solve above-mentioned technical problem, another technical solution that the present invention uses is: providing a kind of barium zinc niobium base dielectric resonator, it is characterized in that, the dielectric resonator is made by following preparation method: barium zinc niobium based ceramic powder body and organic binder are mixed to obtain mixed material, wherein, the weight percentage of the barium zinc niobium based ceramic powder body is 76%-85%, and the weight percentage of the organic binder is 15%-24%；The mixed material is heated, so that the mixed material forms melt；Using injection (mo(u)lding) machine by the melt Injection moulding obtains green body；Degreasing is carried out to the green body, to remove organic binder；Green body after degreasing is sintered to obtain dielectric resonator.
Wherein, the organic binder includes binder, surfactant and plasticizer；Weight percent of the binder in the organic binder is 50%-90%；Weight percent of the surfactant in the organic binder is 1%-5%；Weight percent of the plasticizer in the organic binder is 3%-22%.
Wherein, the step of carrying out degreasing to the green body includes: to carry out oil extraction degreasing to the green body；The green body after degreasing is extracted to oil and carries out thermal debinding.
Wherein, the step of carrying out oil extraction degreasing to the green body includes: that the green body is put into nonpolar solvent, and the temperature of the nonpolar solvent is 30-50 DEG C, degreasing time 12-36 hours；The green body is taken out from nonpolar solvent, is placed in baking oven and is dried, wherein drying temperature is 50-70 DEG C, drying time 4-12 hour.
To solve above-mentioned technical problem, one technical scheme adopted by the invention is that: a kind of cavity body filter is provided, the cavity body filter includes cavity, dielectric resonator described in cover board and above-described embodiment, the cover board covers the cavity to form resonant cavity, and the dielectric resonator installation is in the cavity.
To solve above-mentioned technical problem, the technical solution that the present invention also uses is: providing a kind of radio frequency remote equipment, the radio frequency remote equipment includes: RF transceiver module, cavity body filter described in power amplifier module and fourth aspect, the RF transceiver module is connect with the power amplifier module, and the power amplifier module is connect with the cavity body filter.
The beneficial effects of the present invention are: being in contrast to the prior art, barium zinc niobium base dielectric resonator of the invention and its composition of raw materials and preparation method, by adding more organic binder, the mixed material of barium zinc niobium based ceramic powder body and organic binder is set to form toughness melt after the heating, so as to form dielectric resonator by injection molding method, the dielectric resonator that thus available Density Distribution is uniform, dimensional accuracy is high, and the cost of material is low, preparation process is simple.And also there is high quality factor Q × f value and stability, the barium zinc niobium base dielectric resonator Q value that the present invention is injection moulded preparation is 20000~26000 or so (higher than dry-pressing formed 15000~25000), in addition, complex-shaped barium zinc niobium may be implemented by injection moulding The mass production of base dielectric resonator.
[Detailed description of the invention]
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 the flow diagram of the preparation method embodiment of barium zinc niobium base dielectric resonator of the present invention；
Fig. 3 a is the electron microscope scanning figure after the barium zinc niobium base dielectric resonator port corrosion of dry-pressing formed preparation；
Fig. 3 b is the electron microscope scanning figure after the barium zinc niobium base dielectric resonator port corrosion of injection moulding preparation；And
Fig. 4 is the structure composition block diagram of one preferred embodiment of radio frequency remote equipment of the present invention.
[specific embodiment]
The present invention is described in detail with reference to the accompanying drawings and examples.
The present invention provides a kind of shaping raw material formula of barium zinc niobium base dielectric resonator, which includes the component of following weight percentage: the barium zinc niobium based ceramic powder body of 76%-85% and the organic binder of 15%-24%.
In the shaping raw material formula of dielectric resonator of the invention, the weight percent content of organic binder is 15%-24%, in the compression moulding composition of raw materials of traditional dielectric resonator, the weight percent content of organic binder is 5% or less, compare with for dry-pressing formed composition of raw materials, the weight percent content of organic binder in the present invention is more, the more organic binder of content enables to the mixed material of barium zinc niobium based ceramic powder body and organic binder that can form toughness melt after the heating, thus shaping raw material formula of the invention is allow to form dielectric resonator by injection molding mode.
Specifically, the chemical expression of barium zinc niobium base composite microwave medium ceramic are as follows:
[(1-x)Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+xBa(Ni1-yCoy)1/3Nb2/3O3]+aB2O3+ bCuO, wherein indicates atom vacancy, 0≤x≤0.7,0≤y≤1.0,0≤a≤0.5mol%, 0≤b≤1.0mol%.
The organic binder of the present embodiment includes binder, surfactant and plasticizer.
Wherein, binder is mainly used for bonding barium zinc niobium based ceramic powder body, weight percent of the binder in organic binder is 50%-90%, and binder is selected from least one of paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates and ethylene ethyl acrylate copolymer.
Surfactant is selected from least one of stearic acid, octanoic acid and microcrystalline wax, and weight percent of the surfactant in organic binder is 1%-5%.
Weight percent of the plasticizer in organic binder is 3%-22%, the effect of plasticizer is to increase flexibility and increase viscosity, and in the present embodiment, plasticizer is low melting point plasticizer, so as to melt at a lower temperature, to be uniformly mixed with the mixed material of fusing.Specifically, plasticizer is selected from least one of dibutyl phthalate, diethyl phthalate and o-phthalic acid dibutyl ester.
For example, in one embodiment, the weight percentage of the barium zinc niobium based ceramic powder body in the shaping raw material formula of dielectric resonator is 76%, and the weight percentage of organic binder is 24%.
Specifically, in organic binder, the weight percent of binder is 50%, and the weight percent of surfactant is 5%, and the weight percent of plasticizer is 22%.
In another embodiment, the weight percentage of the barium zinc niobium based ceramic powder body in the shaping raw material formula of dielectric resonator is 85%, and the weight percentage of organic binder is 15%.
Specifically, in organic binder, the weight percent of binder is 90%, and the weight percent of surfactant is 1%, and the weight percent of plasticizer is 3%.
In another embodiment, the weight percentage of the barium zinc niobium based ceramic powder body in the shaping raw material formula of dielectric resonator is 80%, and the weight percentage of organic binder is 20%.
Specifically, in organic binder, the weight percent of binder is 80%, and the weight percent of surfactant is 3%, and the weight percent of plasticizer is 15%.
It is in contrast to the prior art, barium zinc niobium base dielectric resonator of the invention and its composition of raw materials and preparation method, by adding more organic binder, the mixed material of barium zinc niobium based ceramic powder body and organic binder is set to form toughness melt after the heating, so as to form dielectric resonance by injection molding method Device, thus the dielectric resonator that available Density Distribution is uniform, dimensional accuracy is high, and the cost of material is low, preparation process is simple.
The present invention also provides a kind of preparation methods of barium zinc niobium base dielectric resonator.Referring to Fig. 2, Fig. 2 be the flow diagram of the preparation method embodiment of barium zinc niobium base dielectric resonator of the present invention, specifically, the preparation method the following steps are included:
S101, barium zinc niobium based ceramic powder body and organic binder are mixed to obtain mixed material, wherein the weight percentage of barium zinc niobium based ceramic powder body is 76%-85%, and the weight percentage of organic binder is 15%-24%.
Specifically, the chemical expression of the barium zinc niobium base media ceramic are as follows:
[(1-x)Ba(Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+xBa(Ni1-yCoy)1/3Nb2/3O3]+aB2O3+ bCuO, wherein indicates atom vacancy, 0≤x≤0.7,0≤y≤1.0,0≤a≤0.5mol%, 0≤b≤1.0mol%.
The formula of barium zinc niobium base determines that main prepare by solid phase method is studied, and after with honest material, first passes around ball milling, ball-milling medium is zirconia ball, and Ball-milling Time is 4-12 hours.Then it is calcined, calcination temperature is 1000 DEG C -1200 DEG C.Then ball mill is put into the powder calcined and carries out ball milling, this time the medium of ball milling is still zirconia ball, and Ball-milling Time is still 4-12 hours, also, the PVA binder of 2%-5% is added in mechanical milling process.Then it is granulated on spray tower, then prilling powder is put into mold and is pressed, pressure 100MPa-200MPa re-sinters test material performance itself after compression moulding, to obtain required dielectric material -- barium zinc niobium based ceramic powder body.
The organic binder of the present embodiment includes binder, surfactant and plasticizer.Wherein, binder is mainly used for bonding barium zinc niobium based ceramic powder body, weight percent of the binder in organic binder is 50%-90%, and binder is selected from least one of paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates and ethylene ethyl acrylate copolymer.
Surfactant is selected from least one of stearic acid, octanoic acid and microcrystalline wax, and weight percent of the surfactant in organic binder is 1%-5%.
Weight percent of the plasticizer in organic binder is 3%-22%, and the effect of plasticizer is to increase flexibility and increase viscosity, and in the present embodiment, plasticizer is low melting point plasticizer, so as to lower At a temperature of melt, to be uniformly mixed with the mixed material of fusing.Specifically, plasticizer is selected from least one of dibutyl phthalate, diethyl phthalate and o-phthalic acid dibutyl ester.
In this step, barium zinc niobium based ceramic powder body and being blended on kneading machine for organic binder carry out, and incorporation time 4-8 hours.
S102, mixed material is heated, so that mixed material forms melt.
Since the content of the organic binder in mixed material is more, thus the melt formed in step S102 has toughness, is conducive to subsequent injections and forms.Wherein, the temperature of heating is 150 DEG C -250 DEG C.
S103, melt is injection moulded using injection (mo(u)lding) machine to obtain green body.
In step S103, by the metal die of melt injection injection (mo(u)lding) machine, cooling and demolding obtains green body after 2-5 minutes.This step forms dielectric resonator by injection molding mode, may be implemented that Density Distribution is uniform, dimensional accuracy is high, the mass production of complex-shaped barium zinc niobium base dielectric resonator.
S104, degreasing is carried out to green body, to remove organic binder.
In step S104, the organic binder in green body is removed, to prevent organic binder from having an impact to the effect of dielectric resonator.The step of degreasing, which specifically includes, successively carries out nonpolar solvent extraction degreasing and thermal debinding for green body.
Wherein, nonpolar capacity extraction skimming processes are as follows: the green body that injection moulding obtains is put into the nonpolar solvents such as gasoline, carbon disulfide, dimethylbenzene, ether, stupid, chloroform, carbon tetrachloride, naphtha, part organic binder is removed with dissolution, the temperature of nonpolar solvent is 30-50 DEG C, degreasing time is 12-36 hours, then green body is taken out from nonpolar solvent, is placed in baking oven and is dried, drying temperature is 50-70 DEG C, and drying time is 4-12 hours.Nonpolar solvent extraction skimming processes in the step are very important, because if directly carrying out, heat is de- since organic binder ingredient is excessively high in idiosome, and leads to fragmentation of the sample in skimming processes.
The process of thermal debinding is as follows: the green body after drying being put into electric furnace and carries out thermal debinding, to remove remaining organic binder.During being somebody's turn to do, idiosome is warming up to 550 DEG C with the heating rate of 0.5~5 DEG C/min, then keeps the temperature 2~3 hours.
S105, the green body after degreasing is sintered to obtain dielectric resonator.
In step s105, sintering temperature keeps the temperature 2-6 hours between 900-1400 DEG C.
The dielectric resonator of BZN sill is prepared with dry pressing and injection moulding method respectively, the dielectric resonator Q value of dry pressing preparation is 15000~25000, frequency is 2.3~2.6G, dielectric resonator Q value prepared by injection moulding is 20000~26000 or so, and frequency is 2.3~2.7G (note: being using the sample (60) of same a batch preparation as inspection and correlation data).The dielectric resonator performance for being injection moulded preparation is more stable.
Compared with the existing technology, the preparation method of barium zinc niobium base dielectric resonator provided by the invention, enable to production barium zinc niobium base dielectric resonator Density Distribution is uniform, dimensional accuracy is high, it is also equipped with high dielectric constant and high-performance stability simultaneously, and also there is high dielectric constant and stability, in addition, the mass production of complex-shaped barium zinc niobium base dielectric resonator may be implemented by injection moulding.
Injection molding technique has the advantage that (1) forming process has mechanization and high degree of automation, high production efficiency, short molding cycle, blank strength high; managing and controlling conveniently in production process, it is easy to accomplish high-volume, large-scale production；(2) can the various complex geometries of near-net-shape and the small parts that have particular/special requirement, make sintered ceramic product without being machined out or processing less；(3) product molded has high dimensional accuracy and surface smoothness.
Several specific embodiments carry out the performance parameter of barium zinc niobium base dielectric resonator device manufacturing process and finished product resonating device during the present invention will be described in detail below.
Embodiment one
The present embodiment main material material formula uses chemical formula: 0.5Ba (Ni0.5Co0.5)1/3Nb2/3O3For chemical composition, it is respectively compared the performance of the dielectric resonator of dry pressing and injection moulding preparation, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrIt is 35, quality factor (Q × f) value is 100800GHz, temperature coefficient of resonance frequency τfIt is+4.8ppm/ DEG C.After dry pressing mainly passes through granulation, compression moulding, it is sintered to obtain dielectric resonator, simple process.Injection molding technique preparation BZN base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: BZN based ceramic powder body and organic binder are uniformly mixed and obtain injection molding mixture, the content of heterogeneity is related with the granularity of powder, pattern, density in mixing, so its design of mixture of different powder is different；It is directed to BZN base media ceramic, is injection moulded In mixture, the weight percentage of BZN based ceramic powder body is 78%, and the weight percentage of organic binder is 22%；Organic binder is made of binder, surfactant and plasticizer, each component weight percentage are as follows: binder 80%；Surfactant 5%；Plasticizer: 15%.
(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, and demoulding obtains molding blank in 2 minutes after injection mold.
(3) oil extraction degreasing: the green body that injection moulding obtains is put into oil, dissolution removing part organic binder, oily temperature is at 30 DEG C, and degreasing time was at 24 hours, green body after oil extraction degreasing is sufficiently dry in an oven, and directly heat is de- will lead to sample fragmentation in skimming processes.
(4) thermal debinding: the green body after drying is put into electric furnace, is carried out thermal debinding, is removed remaining organic binder, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is kept the temperature 2 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1300 DEG C, is kept the temperature 2 hours, is obtained dielectric resonator.
60 dielectric resonators are prepared with dry-pressing and injection molding technique respectively, and their performance are tested, performance such as table 1:
Table 1: the performance of injection moulding and dry-pressing formed preparation media resonator
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 performance is stablized.
As can be seen that injection moulding is compared with dry pressing preparation from Fig. 3 a and Fig. 3 b, even grain size, particle size is small, this performance and stability final for BZN base dielectric resonator product influences correlation.
Embodiment two
The present embodiment main material material formula uses chemical formula: [0.3Ba (Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3] it is chemical composition, it is respectively compared Jie of dry pressing and injection moulding preparation The performance of matter resonator, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrIt is 32, quality factor (Q × f) value is 91200GHz, temperature coefficient of resonance frequency τfIt is -2.5ppm/ DEG C.After dry pressing mainly passes through granulation, compression moulding, it is sintered to obtain dielectric resonator, simple process.Injection molding technique preparation BZN base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: BZN based ceramic powder body and organic binder are uniformly mixed and obtain injection molding mixture, the content of heterogeneity is related with the granularity of powder, pattern, density in mixing, so its design of mixture of different powder is different；It is directed to BZN base media ceramic, in injection molding mixture, Ba2Ti9O20The weight percentage of based ceramic powder body is 75%, and the weight percentage of organic binder is 25%；Organic binder is made of binder, surfactant and plasticizer, each component weight percentage are as follows: binder 80%；Surfactant 5%；Plasticizer: 15%.
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is between 180 DEG C, and demoulding obtains molding blank in 2 minutes after injection mold.
(3) oil extraction degreasing: the green body that injection moulding obtains is put into oil, dissolution removing part organic binder, oily temperature is at 30 DEG C, and degreasing time was at 24 hours, green body after oil extraction degreasing is sufficiently dry in an oven, and directly heat is de- will lead to sample fragmentation in skimming processes.
(4) thermal debinding: the green body after drying is put into electric furnace, is carried out thermal debinding, is removed remaining organic binder, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is kept the temperature 2 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1280 DEG C, is kept the temperature 4 hours, is obtained dielectric resonator.
60 dielectric resonators are prepared with dry-pressing and injection molding technique respectively, and their performance are tested, performance such as table 2:
Table 2: the performance of injection moulding and dry-pressing formed preparation media resonator
The dielectric resonator for being injection moulded preparation as can be seen from Table 2 is more excellent than performance prepared by traditional dry pressing, And performance is stablized.
Embodiment three
The present embodiment main material material formula uses chemical formula: [0.3Ba (Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3]+0.5mol%B2O3, it is respectively compared the performance of the dielectric resonator of dry pressing and injection moulding preparation, the dielectric properties relative dielectric constant ε of the present embodiment main material itselfrIt is 33, quality factor (Q × f) value is 83000GHz, temperature coefficient of resonance frequency τfIt is 0ppm/ DEG C.After dry pressing mainly passes through granulation, compression moulding, it is sintered to obtain dielectric resonator, simple process.Injection molding technique preparation BZN base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: BZN based ceramic powder body and organic binder are uniformly mixed and obtain injection molding mixture, the content of heterogeneity is related with the granularity of powder, pattern, density in mixing, so its design of mixture of different powder is different；It is directed to BZN base media ceramic, in injection molding mixture, the weight percentage of BZN based ceramic powder body is 75%, and the weight percentage of organic binder is 25%；Organic binder is made of binder, surfactant and plasticizer, each component weight percentage are as follows: binder 80%；Surfactant 5%；Plasticizer: 15%.
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is between 180 DEG C, and demoulding obtains molding blank in 2 minutes after injection mold.
(3) oil extraction degreasing: the green body that injection moulding obtains is put into oil, dissolution removing part organic binder, oily temperature is at 30 DEG C, and degreasing time was at 24 hours, green body after oil extraction degreasing is sufficiently dry in an oven, and directly heat is de- will lead to sample fragmentation in skimming processes.
(4) thermal debinding: the green body after drying is put into electric furnace, is carried out thermal debinding, is removed remaining organic binder, is warming up to 550 DEG C with the heating rate of 0.5 DEG C/min, is kept the temperature 2 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1100 DEG C, is kept the temperature 3 hours, is obtained dielectric resonator.
60 dielectric resonators are prepared with dry-pressing and injection molding technique respectively, and their performance are tested, performance such as table 3:
Table 3: the performance of injection moulding and dry-pressing formed preparation media resonator
The dielectric resonator for being injection moulded preparation as can be seen from Table 3 is more excellent than performance prepared by traditional dry pressing, and performance is stablized.
Example IV
The present embodiment main material material formula uses chemical formula: 0.5Ba (Ni0.5Co0.5)1/3Nb2/3O3For chemical composition, injection molding technique preparation BZN base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: BZN based ceramic powder body and organic binder are mixed on kneading machine, mixing obtains uniformly mixed injection molding mixture in 4 minutes, in the injection molding mixture, the weight percentage of BZN based ceramic powder body is 76%, and the weight percentage of organic binder is 24%；Organic binder is made of binder, surfactant and plasticizer, each component weight percentage are as follows: binder 50%；Surfactant 5%；Plasticizer: 22%.
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is 250 DEG C, and demoulding obtains molding blank in 2 minutes after injection mold.
(3) oil extraction degreasing: the green body that injection moulding obtains is put into oil, dissolution removing part organic binder, the temperature of oil is at 30 DEG C, degreasing time 12 hours, green body after oil extraction degreasing is in an oven, it is 12 hours dry at a temperature of 50 DEG C, keep it sufficiently dry, directly heat is de- will lead to sample fragmentation in skimming processes.
(4) thermal debinding: the green body after drying is put into electric furnace, is carried out thermal debinding, is removed remaining organic binder, is warming up to 500 DEG C with the heating rate of 0.5 DEG C/min, is kept the temperature 3 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 900 DEG C, is kept the temperature 6 hours, is obtained dielectric resonator.
Embodiment five
The present embodiment main material material formula uses chemical formula: [0.3Ba (Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3] it is chemical composition, injection molding technique preparation BZN base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: BZN based ceramic powder body and organic binder are mixed on kneading machine, mixing obtains uniformly mixed injection molding mixture in 8 minutes, in the injection molding mixture, the weight percentage of BZN based ceramic powder body is 85%, and the weight percentage of organic binder is 15；Organic binder is made of binder, surfactant and plasticizer, each component weight percentage are as follows: binder 90%；Surfactant 1%；Plasticizer: 3%.
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is 150 DEG C, and demoulding obtains molding blank in 3 minutes after injection mold.
(3) oil extraction degreasing: the green body that injection moulding obtains is put into oil, dissolution removing part organic binder, the temperature of oil is at 40 DEG C, degreasing time 36 hours, green body after oil extraction degreasing is in an oven, it is 8 hours dry at a temperature of 60 DEG C, keep it sufficiently dry, directly heat is de- will lead to sample fragmentation in skimming processes.
(4) thermal debinding: the green body after drying is put into electric furnace, is carried out thermal debinding, is removed remaining organic binder, is warming up to 550 DEG C with the heating rate of 3 DEG C/min, is kept the temperature 2.5 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1400 DEG C, is kept the temperature 2 hours, is obtained dielectric resonator.
Embodiment six
The present embodiment main material material formula uses chemical formula: [0.3Ba (Zn0.99□0.01)1/3(Nb0.99Mo0.01)2/3O3+0.7Ba(Ni0.7Co0.3)1/3Nb2/3O3]+0.5mol%B2O3For chemical composition, injection molding technique preparation BZN base dielectric resonator is realized by following processing step:
(1) hybrid ceramic powder and organic binder: BZN based ceramic powder body and organic binder are mixed on kneading machine, mixing obtains uniformly mixed injection molding mixture in 6 minutes, in the injection molding mixture, the weight percentage of BZN based ceramic powder body is 80%, and the weight percentage of organic binder is 15%；Organic binder is made of binder, surfactant and plasticizer, each component weight percentage are as follows: binder 80%；Surfactant 3%；Plasticizer: 15%.
(2) be injection moulded: injection molding mixture is injection moulded on injection (mo(u)lding) machine and obtains green body, and injection temperature is 200 DEG C, and demoulding obtains molding blank in 5 minutes after injection mold.
(3) oil extraction degreasing: the green body that injection moulding obtains is put into oil, and dissolution removing part is organic viscous Agent is tied, for oily temperature at 50 DEG C, degreasing time 25 hours, the green body after oil extraction degreasing is in an oven, 4 hours dry at a temperature of 70 DEG C, keeps it sufficiently dry, directly heat is de- will lead to sample fragmentation in skimming processes.
(4) thermal debinding: the green body after drying is put into electric furnace, is carried out thermal debinding, is removed remaining organic binder, is warming up to 600 DEG C with the heating rate of 5 DEG C/min, is kept the temperature 2 hours.
(5) be sintered: the green body after thermal debinding is sintered, and sintering temperature is 1200 DEG C, is kept the temperature 4 hours, is obtained dielectric resonator.
The preparation method of barium zinc niobium base dielectric resonator provided in an embodiment of the present invention, enable to production barium zinc niobium base dielectric resonator Density Distribution is uniform, dimensional accuracy is high, it is also equipped with high dielectric constant and high-performance stability simultaneously, and also there is high dielectric constant and stability, in addition, the mass production of complex-shaped barium zinc niobium base dielectric resonator may be implemented by injection moulding.
In addition, the dielectric resonator is made by the preparation method of any of the above-described embodiment the present invention also provides a kind of dielectric resonator and a kind of cavity body filter.And about the technical characteristic of the parameters such as resonating device shape, structure within the scope of the understanding of those skilled in the art, details are not described herein again.
Cavity body filter then includes the resonator in above-described embodiment, the advantages that by resonator quality factor q with higher × f value and 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 structure of the other parts about cavity body filter and the technical characteristic of parameter, within the scope of the understanding of those skilled in the art, 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 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, and power amplifier module 520 is further connect with cavity body filter 530.
Radio frequency remote equipment works in descending time slot, the transmitting signal in two channels from RF transceiver module 510 enters cavity body filter 530 by power amplifier module 520,530 pairs of transmitting signals of cavity body filter complete filtering, are then emitted to antenna opening after power combing；In ascending time slot, the signal received from antenna opening enters power amplifier module 520 after filtering by cavity body filter 530 for radio frequency remote equipment work, gives RF transceiver module 510 corresponding receiving channel exporting after the amplification of power amplifier module 520.
Further, which can also include power module 540, which is used to power to the modules of the radio frequency remote equipment.
The foregoing is merely section Examples of the invention; it is not intended to limit protection scope of the present invention; it is all to utilize equivalent device or equivalent process transformation made by description of the invention and accompanying drawing content; it is applied directly or indirectly in other relevant technical fields, and is included within the scope of the present invention.

Claims (22)

  1. A kind of composition of raw materials of barium zinc niobium base medium ceramic material, which is characterized in that the component including following weight percentage:
    Barium zinc niobium based ceramic powder body 76%-85%；
    Organic binder 15%-24%.
  2. Composition of raw materials according to claim 1, which is characterized in that the organic binder includes binder, surfactant and plasticizer；
    Weight percent of the binder in the organic binder is 50%-90%；
    Weight percent of the surfactant in the organic binder is 1%-5%；
    Weight percent of the plasticizer in the organic binder is 3%-22%.
  3. Composition of raw materials according to claim 2, it is characterized in that, the binder is selected from least one of paraffin, ethane-acetic acid ethyenyl resin copolymer, polypropylene, random polypropylene, polystyrene, polymethacrylates and ethylene ethyl acrylate copolymer.
  4. Composition of raw materials according to claim 3, which is characterized in that the surfactant is selected from least one of stearic acid, octanoic acid and microcrystalline wax.
  5. Composition of raw materials according to claim 4, which is characterized in that the plasticizer is low melting point plasticizer.
  6. Composition of raw materials according to claim 5, which is characterized in that the plasticizer is selected from least one of dibutyl phthalate, diethyl phthalate and o-phthalic acid dibutyl ester.
  7. A kind of preparation method of barium zinc niobium base medium ceramic material, which comprises the following steps:
    Barium zinc niobium based ceramic powder body and organic binder are mixed to obtain mixed material, wherein the weight percentage of the barium zinc niobium based ceramic powder body is 76%-85%, and the weight percentage of the organic binder is 15%-24%；
    The mixed material is heated, so that the mixed material forms melt；
    It is injection moulded the melt to obtain green body using injection (mo(u)lding) machine；
    Degreasing is carried out to the green body, to remove organic binder；
    Green body after degreasing is sintered to obtain dielectric resonator.
  8. Preparation method according to claim 7, it is characterized in that, in the step of barium zinc niobium based ceramic powder body and organic binder are mixed to obtain mixed material, the barium zinc niobium based ceramic powder body is mixed on kneading machine with the organic binder, and incorporation time is 4-8 hours.
  9. Preparation method according to claim 8, which is characterized in that heat the mixed material, so that the heating temperature is 150 DEG C -250 DEG C in the step of mixed material forms melt.
  10. Preparation method according to claim 9, which is characterized in that the melt was injection moulded in the step of obtaining green body using injection (mo(u)lding) machine, the melt is injected in metal die, cooling and demolding obtains the green body after 2-5 minutes.
  11. Preparation method according to claim 10, which is characterized in that include: to the step of green body progress degreasing
    Oil extraction degreasing is carried out to the green body；
    The green body after degreasing is extracted to oil and carries out thermal debinding.
  12. Preparation method according to claim 11, which is characterized in that carrying out the step of oil extracts degreasing to the green body includes:
    The green body is put into nonpolar solvent, the temperature of the nonpolar solvent is 30-50 DEG C, degreasing time 12-36 hours；
    The green body is taken out from nonpolar solvent, is placed in baking oven and is dried, wherein drying temperature is 50-70 DEG C, drying time 4-12 hour.
  13. Preparation method according to claim 12, which is characterized in that the nonpolar solvent is selected from least one of gasoline, carbon disulfide, dimethylbenzene, ether, benzene, chloroform, carbon tetrachloride and naphtha.
  14. Preparation method according to claim 13, which is characterized in that oil is extracted in the step of green body after degreasing carries out thermal debinding, the green body is placed in electric furnace, 500-600 DEG C is warming up to the heating rate of 0.5-5 DEG C/min, keeps the temperature 2-3 hours.
  15. Preparation method according to claim 14, which is characterized in that the green body after thermal debinding into In the step of row sintering is to obtain dielectric resonator, the sintering temperature is 900-1400 DEG C, keeps the temperature 2-6 hours.
  16. Preparation method according to claim 15, which is characterized in that the organic binder includes binder, surfactant and plasticizer；
    Weight percent of the binder in the organic binder is 50%-90%；
    Weight percent of the surfactant in the organic binder is 1%-5%；
    Weight percent of the plasticizer in the organic binder is 3%-22%.
  17. A kind of barium zinc niobium base dielectric resonator, which is characterized in that the dielectric resonator is made by following preparation method:
    Barium zinc niobium based ceramic powder body and organic binder are mixed to obtain mixed material, wherein the weight percentage of the barium zinc niobium based ceramic powder body is 76%-85%, and the weight percentage of the organic binder is 15%-24%；
    The mixed material is heated, so that the mixed material forms melt；
    It is injection moulded the melt to obtain green body using injection (mo(u)lding) machine；
    Degreasing is carried out to the green body, to remove organic binder；
    Green body after degreasing is sintered to obtain dielectric resonator.
  18. Barium zinc niobium base dielectric resonator according to claim 17, which is characterized in that the organic binder includes binder, surfactant and plasticizer；
    Weight percent of the binder in the organic binder is 50%-90%；
    Weight percent of the surfactant in the organic binder is 1%-5%；
    Weight percent of the plasticizer in the organic binder is 3%-22%.
  19. Barium zinc niobium base dielectric resonator according to claim 18, which is characterized in that include: to the step of green body progress degreasing
    Oil extraction degreasing is carried out to the green body；
    The green body after degreasing is extracted to oil and carries out thermal debinding.
  20. Barium zinc niobium base dielectric resonator according to claim 19, which is characterized in that carrying out the step of oil extracts degreasing to the green body includes:
    The green body is put into nonpolar solvent, the temperature of the nonpolar solvent is 30-50 DEG C, degreasing time 12-36 hours；
    The green body is taken out from nonpolar solvent, is placed in baking oven and is dried, wherein drying temperature is 50-70 DEG C, drying time 4-12 hour.
  21. A kind of cavity body filter, which is characterized in that the cavity body filter includes cavity, cover board and the described in any item dielectric resonators of claim 17-20, and the cover board covers the cavity to form resonant cavity, and the dielectric resonator installation is in the cavity.
  22. A kind of radio frequency remote equipment, it is characterized in that, the radio frequency remote equipment includes: RF transceiver module, cavity body filter described in power amplifier module and claim 21, and the RF transceiver module is connect with the power amplifier module, and the power amplifier module is connect with the cavity body filter.
CN201580079830.0A 2015-12-30 2015-12-30 Ceramic material and preparation method thereof, resonator, wave filter and radio frequency remote equipment Pending CN107614461A (en)

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