CN110483035A - A kind of microwave dielectric ceramic materials and its preparation method and application, a kind of filter ceramic material - Google Patents
A kind of microwave dielectric ceramic materials and its preparation method and application, a kind of filter ceramic material Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 132
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 229910018293 LaTiO3 Inorganic materials 0.000 claims abstract description 10
- 229910005639 SnTiO3 Inorganic materials 0.000 claims abstract description 10
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 9
- 229910003122 ZnTiO3 Inorganic materials 0.000 claims abstract description 7
- 229910015805 BaWO4 Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 121
- 238000010304 firing Methods 0.000 claims description 104
- 238000000034 method Methods 0.000 claims description 97
- 238000000498 ball milling Methods 0.000 claims description 55
- 238000010438 heat treatment Methods 0.000 claims description 48
- 238000011282 treatment Methods 0.000 claims description 48
- 238000002156 mixing Methods 0.000 claims description 46
- 238000012545 processing Methods 0.000 claims description 37
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 31
- 229910052709 silver Inorganic materials 0.000 claims description 31
- 239000004332 silver Substances 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 21
- 238000005245 sintering Methods 0.000 claims description 17
- 238000004513 sizing Methods 0.000 claims description 13
- 239000011230 binding agent Substances 0.000 claims description 12
- 238000013461 design Methods 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 8
- 238000007906 compression Methods 0.000 claims description 6
- 230000010287 polarization Effects 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims 1
- 239000012776 electronic material Substances 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 description 45
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 18
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 10
- 238000004321 preservation Methods 0.000 description 10
- 239000000292 calcium oxide Substances 0.000 description 9
- 239000000395 magnesium oxide Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- 238000004891 communication Methods 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 230000007717 exclusion Effects 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 239000002002 slurry Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention provides a kind of microwave dielectric ceramic materials and its preparation method and application and a kind of filter ceramic materials, belong to technical field of electronic materials.Microwave dielectric ceramic materials provided by the invention are prepared in terms of mass parts by component A, B component, component C, D component and component E, and wherein component A is BaTi4O9, B component Ba2Ti9O20, component C BaWO4, D group is divided into ZnTiO3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Mixture, component E is by CaO, MgO and SiO2It is successively sintered and is cooled down to obtain.The dielectric constant of microwave dielectric ceramic materials provided by the invention is higher, and dielectric loss is small, and quality factor q is higher, and frequency-temperature coefficient is smaller.
Description
Technical field
The present invention relates to technical field of electronic materials more particularly to a kind of microwave dielectric ceramic materials and preparation method thereof and
Using a kind of, filter ceramic material.
Background technique
Microwave dielectric ceramic materials, which refer to, dielectric material and to be completed one or more applied to being used as in microwave frequency band circuit
The ceramic material of function.Microwave-medium ceramics are used as resonator, filtering as a kind of novel electron material in modern communications
Device, dielectric substrate, diectric antenna, dielectric guided wave circuit etc..With microwave telecommunication devices, digital audio-video, satellite communication, military thunder
Up to toward high-end development, this requirement to microwave dielectric ceramic materials is also continuously improved.
The dielectric constant of microwave current medium ceramic material is low, and insertion loss is higher, is unable to satisfy the demand of people, existing
Having the method that microwave dielectric ceramic materials are improved in technology is usually to research and develop new material, the dielectric of microwave dielectric ceramic materials
Constant is still to be improved, and loss value still has to be reduced.
Summary of the invention
The present invention provides a kind of microwave dielectric ceramic materials and its preparation method and application, a kind of filter ceramics material
Material, microwave dielectric ceramic materials provided by the invention have the characteristics that dielectric constant is high, loss value is low.
The present invention provides a kind of microwave dielectric ceramic materials, which is characterized in that in terms of mass parts, the microwave-medium pottery
Ceramic material is prepared by component A, B component, component C, D component and component E, and wherein component A is BaTi4O9, the quality of component A
Score is 65~75%；B component is Ba2Ti9O20, the mass fraction of B component is 20%~24%；Component C is BaWO4, component C
Mass fraction be 0.2%~5.5%；D group is divided into ZnTiO3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3
Mixture, the mass fraction of D component is 0.001%~1%；Component E is by CaO, MgO and SiO2Successively it is sintered and is cooled down
It arrives, the mass fraction of component E is 4%~10%.
Preferably, ZnTiO in the D component3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Quality
Than for 26~27:24~25:15.5~16.5:15.5~16.5:8~9:8~9.
Preferably, SiO in the component E2, CaO and MgO mass ratio be 9~11:2~4:1.
Preferably, the component E preparation method the following steps are included:
It after silica, calcium oxide and magnesia are mixed, is sintered, then cooling obtains component E；The sintering
Processing includes 7 stages successively carried out, specially the first heating stage, the second temperature rise period, third constant temperature stage, the 4th liter
Thermophase, the 5th constant temperature stage, the 6th temperature rise period, the 7th constant temperature stage；The cooling treatment includes two successively carried out
Stage, including the first cooling stage and the second cooling stage；The design parameter of the sintering processes and cooling treatment such as 1 institute of table
Show:
Table 1 prepares the sintering processes and cooling treatment parameter when component E
Preferably, the group of the microwave dielectric ceramic materials becomes any one in following 1~composition of composition 5:
Form 1:A component 65%, B component 24%, component C 0.2%, D component 0.8%, component E 10%；
Form 2:A component 66%, B component 23%, component C 2.3%, D component 0.7%, component E 8%；
Form 3:A component 68%, B component 22%, component C 3.4%, D component 0.6%, component E 6%；
Form 4:A component 69%, B component 21%, component C 4.5%, D component 0.5%, component E 5%；
Form 5:A component 70%, B component 20%, component C 5.5%, D component 0.5%, component E 4%.
The present invention also provides the preparation methods of microwave dielectric ceramic materials described in above-mentioned technical proposal, including following step
It is rapid:
(1) binder after component A, B component, component C, D component and component E mixing and ball milling, will be added to be granulated, obtains
Powder；
(2) powder is subjected to compression process, obtains green body；
(3) it is cooled down after the green body being carried out firing processing, obtains microwave dielectric ceramic materials.
Preferably, compacting includes the four-stage successively carried out in described (2), specially matched moulds stage, in sizing exhaust
Grade stage, sizing are vented ultimate stage and packing stage；Wherein
The time of matched moulds stage is 6~8s, and pressure is 40~60kg/cm2；
The time of sizing exhaust intermediate stage is 1.5~2.5s, and pressure is 140~160kg/cm2；
The time that sizing is vented the ultimate stage is 2.5~3.5s, and pressure is 250~500kg/cm2；
The time of packing stage is 4.5~5.5s, and pressure is 450~500kg/cm2。
Preferably, firing processing and cooling include three kinds of methods in described (3),
First method: firing processing includes 6 stages successively carried out, specially the 1st temperature rise period, the 2nd heating rank
Section, the 3rd temperature rise period, the 4th temperature rise period, the 5th temperature rise period and the 6th constant temperature stage；Cooling treatment includes two successively carried out
A stage, specially the 1st cooling stage and the 2nd cooling stage；The design parameter of the firing and cooling treatment is as shown in table 2:
Table 2 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
Second method: firing processing includes 7 stages successively carried out, specially the 1st ' temperature rise period, the 2nd ' heating
Stage, the 3rd ' constant temperature stage, the 4th ' temperature rise period, the 5th ' temperature rise period, the 6th ' constant temperature stage and the 7th ' temperature rise period；The burning
Design parameter at processing and cooling treatment is as shown in table 3:
Table 3 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
The third method: it is burnt into 8 stages including successively carrying out that handle, the specially the 1st " temperature rise period, the 2nd " heating
Stage, the 3rd " temperature rise period, the 4th " constant temperature stage, the 5th " temperature rise period, the 6th " temperature rise period, the 7th " temperature rise period and the 8th " is permanent
Thermophase；The design parameter of the firing processing and cooling treatment is as shown in table 4:
Table 4 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
The present invention also provides sides described in microwave dielectric ceramic materials described in above-mentioned technical proposal or above-mentioned technical proposal
Application of the microwave dielectric ceramic materials that method is prepared in filter.
The present invention also provides a kind of filter ceramic material, the filter ceramic material is as described in above-mentioned technical proposal
The microwave dielectric ceramic materials that microwave dielectric ceramic materials or above-mentioned technical proposal the method are prepared are successively through silk-screen
Uniformly silver paste, silver ink firing and polarization is painted to obtain.
The present invention provides a kind of microwave dielectric ceramic materials, and in terms of mass parts, the microwave dielectric ceramic materials are by A group
Point, B component, component C, D component and component E be prepared, wherein component A is BaTi4O9, the mass fraction of component A is 65~
75%；B component is Ba2Ti9O20, the mass fraction of B component is 20%~24%；Component C is BaWO4, the mass fraction of component C
It is 0.2%~5.5%；D group is divided into ZnTiO3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Mixture, D
The mass fraction of component is 0.001%~1%；Component E is by CaO, MgO and SiO2It is successively sintered and is cooled down to obtain, component E
Mass fraction is 4%~10%.Microwave dielectric ceramic materials provided by the invention pass through control component A, B component, component C, D group
Point and component E ingredient and dosage, effectively increase the dielectric constant of microwave dielectric ceramic materials, and reduce loss value,
Middle component E can not only reduce sintering temperature when preparing microwave dielectric ceramic materials as fluxing agent, and can effectively mention
The microwave dielectric property of microwave ceramics medium is risen, dielectric constant is improved, controls temperature drift range.Embodiment the result shows that, the present invention
The dielectric constant of the microwave dielectric ceramic materials of offer is higher, and dielectric loss is small, and quality factor q is higher, frequency-temperature coefficient compared with
It is small.
Specific embodiment
The present invention provides a kind of microwave dielectric ceramic materials, and in terms of mass parts, the microwave dielectric ceramic materials are by A group
Divide, B component, component C, D component and component E are prepared.
In the present invention, the component A is BaTi4O9, the mass fraction of component A is in the microwave dielectric ceramic materials
65%~75%, preferably 65%~70%.
In the present invention, the B component is Ba2Ti9O20, the mass fraction of B component in the microwave dielectric ceramic materials
It is 20%~24%, preferably 20%, 21%, 22%, 23% or 24%.
In the present invention, the component C is BaWO4, the mass fraction of component C is in the microwave dielectric ceramic materials
0.2%~5.5%, preferably 0.5%~5%, more preferably 1%~4%.
In the present invention, the D group is divided into ZnTiO3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3's
Mixture, ZnTiO in the D component3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Mass ratio be preferably
26~27:24~25:15.5~16.5:15.5~16.5:8~9:8~9, more preferably 26.3:24.7:16:16:8.2:
8.8.The mass fraction of D component is 0.001%~1%, preferably 0.01~1% in the microwave dielectric ceramic materials, into one
Step preferably 0.1%~1%, more preferably 0.5%~1%.
In the present invention, the component E is by CaO, MgO and SiO2It is successively sintered and is cooled down to obtain, the SiO2, CaO and
The mass ratio of MgO is preferably 9~11:2~4:1, more preferably 10:3:1.The matter of component E in the microwave dielectric ceramic materials
Measuring score is 4%~10%, preferably 4.5%~9.5%, more preferably 4%~9%.In the present invention, the component E is made
For fluxing agent, sintering temperature when preparing microwave dielectric ceramic materials can be effectively reduced, and add component E, it can be effective
The microwave dielectric property of microwave ceramics medium is promoted, dielectric constant is improved, controls temperature drift range.
In the present invention, the raw material in component A, B component, component C, D component and component E is commercial goods.
In the present invention, the preparation method of the component E preferably includes following steps:
It after silica, calcium oxide and magnesia are mixed, is sintered, then cooling obtains fluxing agent；The burning
Knot processing includes 7 stages successively carried out, specially the first heating stage, the second temperature rise period, third constant temperature stage, the 4th
Temperature rise period, the 5th constant temperature stage, the 6th temperature rise period, the 7th constant temperature stage；The cooling treatment includes two successively carried out
A stage, including the first cooling stage and the second cooling stage；The design parameter of the sintering processes and cooling treatment such as 1 institute of table
Show:
Table 1 prepares the sintering processes and cooling treatment parameter when component E
In the present invention, the sintering processes and cooling treatment parameter when preparing component E are preferably as shown in table 1-1:
Table 1-1 prepares the sintering processes and cooling treatment parameter when component E
For the present invention by above-mentioned sintering and cooling treatment, the component E being prepared can be effectively reduced system as fluxing agent
Sintering temperature when standby microwave dielectric ceramic materials, and component E is added, the microwave that can effectively promote microwave ceramics medium is situated between
Electrical property improves dielectric constant, controls temperature drift range.
In the present invention, any one in the preferably following 1~composition of composition 5 of the composition of the microwave dielectric ceramic materials
Kind:
Form 1:A component 65%, B component 24%, component C 0.2%, D component 0.8%, component E 10%；
Form 2:A component 66%, B component 23%, component C 2.3%, D component 0.7%, component E 8%；
Form 3:A component 68%, B component 22%, component C 3.4%, D component 0.6%, component E 6%；
Form 4:A component 69%, B component 21%, component C 4.5%, D component 0.5%, component E 5%；
Form 5:A component 70%, B component 20%, component C 5.5%, D component 0.5%, component E 4%.
The present invention also provides the preparation methods of microwave dielectric ceramic materials described in above-mentioned technical proposal, including following step
It is rapid:
(1) binder after component A, B component, component C, D component and component E mixing and ball milling, will be added to be granulated, obtains
Powder；
(2) powder is subjected to compression process, obtains green body；
(3) it is cooled down after the green body being carried out firing processing, obtains microwave-medium ceramics.
The present invention after component A, B component, component C, D component and component E mixing and ball milling, will be added binder and is granulated,
Obtain powder.In the present invention, the ratio of grinding media to material of the mixing and ball milling is preferably 1.5~2.5:1, more preferably 2:1 Ball-milling Time
Preferably 35~40h, more preferably 36h.The present invention preferably after the completion of ball milling, successively carries out sieving and drying and processing, described
The mesh number of sieving sieve is preferably 300 mesh.After the completion of drying, binder is added into the powder after drying and makes by the present invention
Grain processing.In the present invention, the binder is preferably the polyvinyl alcohol water solution of mass concentration 8%；The binder and powder
The mass ratio of grain is preferably 5~7:100, more preferably 6:100；Described be granulated is preferably mist projection granulating.
After obtaining powder, the powder is carried out compression process by the present invention, obtains green body.In the present invention, the compacting
Processing preferably includes the four-stage successively carried out, and specially matched moulds stage, sizing exhaust intermediate stage, sizing is vented ultimate rank
Section and packing stage；Wherein
The time of matched moulds stage is 6~8s, and preferably 7s, pressure is 40~60kg/cm2, preferably 50kg/cm2；
The time of sizing exhaust intermediate stage is 1.5~2.5s, and preferably 2s, pressure is 140~160kg/cm2, preferably
For 150kg/cm2；
The time that sizing is vented the ultimate stage is 2.5~3.5s, and preferably 2s, pressure is 250~500kg/cm2, preferably
For 300~450kg/cm2, further preferably 350~400kg/cm2；
The time of packing stage is 4.5~5.5s, and preferably 5s, pressure is 450~500kg/cm2。
Compression process is divided into the aforementioned four stage by the present invention, and by the time in aforementioned four stage and pressure control upper
It states in range, is conducive to reduce gap, the blank density and thickness for obtaining compacting are uniform by squeezing sphere.
After the completion of compression process, the present invention cools down after carrying out firing processing to green body, and the firing processing and cooling include
Three kinds of methods,
First method: firing processing preferably includes 6 stages successively carried out, specially the 1st temperature rise period, the 2nd liter
Thermophase, the 3rd temperature rise period, the 4th temperature rise period, the 5th temperature rise period and the 6th constant temperature stage；Cooling treatment includes successively carrying out
Two stages, specially the 1st cooling stage and the 2nd cooling stage；The design parameter of the firing and cooling treatment is preferably such as
Shown in table 2:
Table 2 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
In the first method, the green body firing and cooling parameter are further preferred as shown in table 2-1 by the present invention:
Table 2-1 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
Second method: firing processing preferably includes 7 stages successively carried out, specially the 1st ' temperature rise period, the 2nd '
Temperature rise period, the 3rd ' constant temperature stage, the 4th ' temperature rise period, the 5th ' temperature rise period, the 6th ' constant temperature stage and the 7th ' temperature rise period；Institute
The design parameter for stating firing processing and cooling treatment is preferably as shown in table 3:
Table 3 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
In the second approach, the green body firing and cooling parameter are further preferred as shown in table 3-1 by the present invention:
Table 3-1 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
The third method: firing processing preferably includes 8 stages successively carrying out, and the specially the 1st " temperature rise period, the 2nd "
Temperature rise period temperature rise period, the 3rd " temperature rise period, the 4th " constant temperature stage, the 5th " temperature rise period, the 6th " temperature rise period, the 7th " and
8 " constant temperature stages；The design parameter of the firing processing and cooling treatment is preferably as shown in table 4:
Table 4 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
For the present invention in the third method, the green body firing and cooling parameter are further preferred as shown in table 4-1:
Table 4-1 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
The microwave dielectric ceramic materials that above-mentioned three kinds of process for calcining provided by the invention are prepared all have preferable property
Can, dielectric constant is higher, is lost low.In above-mentioned three kinds of process for calcining provided by the invention, 0~150 DEG C is moisture exclusion process；
150 DEG C~450 DEG C are the processes for excluding binder；450 DEG C~600 DEG C are that further thoroughly exclusion binder and green body are opened
Beginning solidification process；600 DEG C~900 DEG C are green body solidification process；900 DEG C~1080 DEG C are that fluxing agent component E and other groups separate
Begin the process melted；1080 DEG C~1320 DEG C are that all compounds carry out physical-chemical reaction process；1320 DEG C advantageously ensure that
Various compound physical chemical reactions are thorough and carry out crystallization；1st cooling stage is the rapid cooling stage, is beneficial to prevent secondary
Inverse trichite is raw.In the present invention, all constant temperature stages advantageously ensure that the uniform thorough exclusion waste of furnace temperature, and such as moisture glues
Tie agent.
The present invention also provides sides described in microwave dielectric ceramic materials described in above-mentioned technical proposal or above-mentioned technical proposal
Application of the microwave dielectric ceramic materials that method is prepared in filter.
The present invention also provides a kind of filter ceramic material, the filter ceramic material is as described in above-mentioned technical proposal
The microwave dielectric ceramic materials that microwave dielectric ceramic materials or above-mentioned technical proposal the method are prepared are successively through wire brush
Silver paste, silver ink firing and polarization obtain.In the present invention, the silver slurry layer thickness of the wire brush silver paste is preferably 40~50 μm, more preferably
It is 45 μm.In the present invention, the silver ink firing preferably carries out in silver ink firing special furnace, and the silver ink firing preferably includes successively carry out five
A stage, specially the first silver ink firing stage, the second silver ink firing stage, third silver ink firing stage, the 4th silver ink firing stage and the 5th silver ink firing rank
Section；The temperature in the first silver ink firing stage is preferably 20~165 DEG C, and the time is preferably 35~45min, more preferably 40min, institute
Stating for the first silver ink firing stage is drying section；The temperature in the second silver ink firing stage is preferably 165~460 DEG C, and the time is preferably 35~
45min, more preferably 40min, the second silver ink firing stage are low-temperature zone；The temperature in the third silver ink firing stage is preferably 460
~600 DEG C, the time is preferably 55~65min, more preferably 60min, and the third silver ink firing stage is high temperature section；Described 4th burns
The temperature in silver-colored stage is preferably 600~750 DEG C, and the time is preferably 80~100min, more preferably 90min；5th silver ink firing
The temperature in stage is preferably 25~35min, more preferably 30min, and the time is preferably 25~35min, more preferably 30min.This
Invention silver paste in the 4th silver ink firing stage is melted and Ceramic bond, and silver paste and ceramics sufficiently combine, are attached in the 5th silver ink firing stage
.After the completion of silver ink firing, cooling treatment is preferably carried out, the temperature after cooling is preferably room temperature, and the rate of the cooling is preferred
For 20~30 DEG C/min, more preferably 24~26 DEG C/min.The present invention preferably by cooling rate control within the above range, have
It is excluded conducive to by exhaust gas.
After the completion of silver ink firing, the present invention is polarised silver/ceramic composite that silver ink firing obtains, the polarization process
It is preferred that carrying out in the total phenotype piezoelectric ceramics high voltage polarization equipment of ET2673D-4, the polarized electric field is preferably 2~6kV/
Mm, temperature are preferably 100~180 DEG C, and the time is preferably 15~25min, more preferably 20min.
After the completion of polarization, the present invention preferably carries out drying and processing, obtains filter ceramic material.In the present invention, described
The temperature of drying is preferably 60~150 DEG C, and the time is preferably 10~20min, more preferably 15min.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.
Embodiment 1-1
Component A, B component, component C, D component and component E are mixed, wherein component A is BaTi4O9, the quality point of component A
Number is 65%；B component is Ba2Ti9O20, the mass fraction of B component is 24%, component C BaWO4, the mass fraction of component C is
0.2%, D group are divided into ZnTiO3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Mixture, in the D component
ZnTiO3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Mass ratio be 26.3:24.7:16:16:8.2:
8.8；The mass fraction of D component is 0.8%, and component E is fluxing agent, and the mass fraction of component E is 10%, the preparation side of component E
Method are as follows: by CaO, MgO and SiO2Mixture be successively sintered and cooling treatment, obtain component E, the SiO2, CaO and MgO
Mass ratio be 10:3:1, sintering and cooling treatment process are as follows: rise to 100 DEG C by room temperature, heating rate is 50 DEG C/h；By 100
450 DEG C DEG C are raised to, heating rate is 115 DEG C/h；In 450 DEG C of heat preservation 2h；900 DEG C are risen to by 450 DEG C, heating rate is 115 DEG C/
h；In 900 DEG C of heat preservation 1h；1060 DEG C are risen to by 900 DEG C, heating rate is 155 DEG C/h；In 1060 DEG C of heat preservation 1h；It is fast by 1060 DEG C
Speed cools to 600 DEG C, and rate of temperature fall is 455 DEG C/h；Then room temperature is naturally cooled to.
Ball milling after component A, B component, component C, D component and component E are mixed, the ratio of grinding media to material of ball milling are 2:1, Ball-milling Time
It for 36h, after ball milling, is screened through 300 mesh screens, then extracting screen underflow is dried, adding mass concentration is 8% polyvinyl alcohol
Aqueous solution is that binder carries out mist projection granulating, obtains powder.
After obtaining powder, is suppressed using intelligent mo(u)ldenpress 150T, obtain green body.Pressing process divides four-stage:
(1), it molds within the 0th~7 second, pressure 50kg/cm2It is formed the primary stage；(2), the 7th~9 second, pressure 150kg/cm2In sizing exhaust
Grade stage, molecule particles deformation, the every nook and cranny for excluding gas, accumulating filling mold again；(3), the 9th~12 second, pressure
250kg/cm2It is formed the ultimate stage, every nook and cranny compacting, even density；(4), the 12nd~17 second packing stage, packing stage
Pressure is 480kg/cm2, the dwell time is determined according to product size, elimination stress ensures indeformable after green body takes out；Then exist
Die sinking in 17~25 seconds takes base, notices that protection is kept off scarce green body and ensured completely.
After the completion of compacting, by obtained green body carry out firing and cooling treatment, according to first method carry out firing and it is cold
But it handles: being raised to 400 DEG C by room temperature, heating rate is 95 DEG C/h；600 DEG C are raised to by 400 DEG C, heating rate is 43 DEG C/h；By
600 DEG C are raised to 900 DEG C, and heating rate is 100 DEG C/h；1300 DEG C are raised to by 900 DEG C, heating rate is 80 DEG C/h；By 1300 DEG C
1320 DEG C are raised to, heating rate is 20 DEG C/h；In 1320 DEG C of heat preservation 2h；By 1320 DEG C of fast coolings to 900 DEG C, rate of temperature fall is
420 DEG C/h, then room temperature is naturally cooled to, obtain microwave dielectric ceramic materials.
Embodiment 1-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
Point ingredient it is identical as embodiment 1-1, component A, B component, component C, D component and component E mass fraction be followed successively by 66%,
23%, 2.3%, 0.7% and 8%.
Then according to the method for embodiment 1-1 by component A, B component, component C, D component and component E mix after ball milling, make
Grain, compacting, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 1-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
Point ingredient it is identical as embodiment 1-1, component A, B component, component C, D component and component E mass fraction be followed successively by 68%,
22%, 3.4%, 0.6% and 6%.
Then according to the method for embodiment 1-1 by component A, B component, component C, D component and component E mix after ball milling, make
Grain, compacting, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 1-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
Point ingredient it is identical as embodiment 1-1, component A, B component, component C, D component and component E mass fraction be followed successively by 69%,
21%, 4.5%, 0.5% and 5%.
Then according to the method for embodiment 1-1 by component A, B component, component C, D component and component E mix after ball milling, make
Grain, compacting, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 1-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
Point ingredient it is identical as embodiment 1-1, component A, B component, component C, D component and component E mass fraction be followed successively by 70%,
20%, 5.5%, 0.5% and 4%.
Then according to the method for embodiment 1-1 by component A, B component, component C, D component and component E mix after ball milling, make
Grain, compacting, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 2-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 1-1
System, firing and cooling are to be burnt into and cooling method are different, burnt using second method from the difference of embodiment 1-1
At and cooling treatment: be raised to 500 DEG C by room temperature, heating rate is 80 DEG C/h；600 DEG C are raised to by 500 DEG C, heating rate 66
℃/h；In 600 DEG C of heat preservation 1h；900 DEG C are raised to by 600 DEG C, heating rate is 75 DEG C/h；1250 DEG C are raised to by 900 DEG C, heating speed
Rate is 85 DEG C/h；1h is kept the temperature at 1250 DEG C；1320 DEG C are raised to by 1250 DEG C, heating rate is 70 DEG C/h；By 1320 DEG C of natures
It is cooled to room temperature, obtains microwave dielectric ceramic materials.
Embodiment 2-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 2-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 2-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 2-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 2-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 2-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 2-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 2-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 3-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 1-1
System, firing and cooling are to be burnt into and cooling method are different, burnt using the third method from the difference of embodiment 1-1
At and cooling treatment: be raised to 150 DEG C by room temperature, heating rate is 90 DEG C/h；450 DEG C are raised to by 150 DEG C, heating rate 100
℃/h；600 DEG C are raised to by 450 DEG C, heating rate is 75 DEG C/h；In 600 DEG C of heat preservation 1h；900 DEG C are raised to by 600 DEG C, heating speed
Rate is 75 DEG C/h；1080 DEG C are raised to by 900 DEG C, heating rate is 90 DEG C/h；1320 DEG C are raised to by 1080 DEG C, heating rate 80
℃/h；Room temperature is naturally cooled to by 1320 DEG C, obtains microwave dielectric ceramic materials.
Embodiment 3-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 3-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 3-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 3-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 3-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 3-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 3-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 3-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 4-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling after component A, B component, component C, D component and component E are mixed, is made after then mixing again with binder
Grain, obtains powder, the process for preparing powder is identical as embodiment 1-1.
After obtaining powder, powder is suppressed, obtains green body.Pressing process divides four-stage, different from embodiment 1-1
, in the phase III of compacting, 9~12 seconds, pressure 350kg/cm2, remaining pressing conditions and embodiment 1-1 are all the same.
After the completion of compacting, green body is sintered and cooling treatment, sintering and cooling means are identical as embodiment 1-1, obtain
To microwave dielectric ceramic materials.
Embodiment 4-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 4-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 4-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 4-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 4-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 4-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 4-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 4-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 5-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 4-1
System, firing and cooling, the difference with embodiment 4-1 is, is burnt into different with the method that cools down, is burnt using second method
At and cooling treatment: be raised to 500 DEG C by room temperature, heating rate is 80 DEG C/h；600 DEG C are raised to by 500 DEG C, heating rate 66
℃/h；In 600 DEG C of heat preservation 1h；900 DEG C are raised to by 600 DEG C, heating rate is 75 DEG C/h；1250 DEG C are raised to by 900 DEG C, heating speed
Rate is 85 DEG C/h；1h is kept the temperature at 1250 DEG C；1320 DEG C are raised to by 1250 DEG C, heating rate is 70 DEG C/h；By 1320 DEG C of natures
It is cooled to room temperature, obtains microwave dielectric ceramic materials.
Embodiment 5-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 5-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 5-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 5-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 5-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 5-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 5-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 5-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 6-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 4-1
System, firing and cooling, the difference with embodiment 4-1 is, is burnt into different with the method that cools down, is burnt using the third method
At and cooling treatment: be raised to 150 DEG C by room temperature, heating rate is 90 DEG C/h；450 DEG C are raised to by 150 DEG C, heating rate 100
℃/h；600 DEG C are raised to by 450 DEG C, heating rate is 75 DEG C/h；In 600 DEG C of heat preservation 1h；900 DEG C are raised to by 600 DEG C, heating speed
Rate is 75 DEG C/h；1080 DEG C are raised to by 900 DEG C, heating rate is 90 DEG C/h；1320 DEG C are raised to by 1080 DEG C, heating rate 80
℃/h；Room temperature is naturally cooled to by 1320 DEG C, obtains microwave dielectric ceramic materials.
Embodiment 6-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 6-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 6-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 6-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 6-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 6-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 6-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 6-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 7-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling after component A, B component, component C, D component and component E are mixed, is made after then mixing again with binder
Grain, obtains powder, the process for preparing powder is identical as embodiment 1-1.
After obtaining powder, powder is suppressed, obtains green body.Pressing process divides four-stage, different from embodiment 1-1
, in the phase III of compacting, 9~12 seconds, pressing pressure 500kg/cm2, remaining pressing conditions and embodiment 1-1 are homogeneous
Together.
After the completion of compacting, green body is sintered and cooling treatment, sintering and cooling means are identical as embodiment 1-1, obtain
To microwave dielectric ceramic materials.
Embodiment 7-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 7-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 7-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 7-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 7-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 7-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 7-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 7-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 8-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 7-1
System, firing and cooling, the difference with embodiment 7-1 is, is burnt into different with the method that cools down, is burnt using second method
At and cooling treatment: be raised to 500 DEG C by room temperature, heating rate is 80 DEG C/h；600 DEG C are raised to by 500 DEG C, heating rate 66
℃/h；In 600 DEG C of heat preservation 1h；900 DEG C are raised to by 600 DEG C, heating rate is 75 DEG C/h；1250 DEG C are raised to by 900 DEG C, heating speed
Rate is 85 DEG C/h；1h is kept the temperature at 1250 DEG C；1320 DEG C are raised to by 1250 DEG C, heating rate is 70 DEG C/h；By 1320 DEG C of natures
It is cooled to room temperature, obtains microwave dielectric ceramic materials.
Embodiment 8-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 8-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 8-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 8-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 8-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 8-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 8-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 8-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 9-1
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-1.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 9-1
System, firing and cooling, the difference with embodiment 9-1 is, is burnt into different with the method that cools down, is burnt using the third method
At and cooling treatment: be raised to 150 DEG C by room temperature, heating rate is 90 DEG C/h；450 DEG C are raised to by 150 DEG C, heating rate 100
℃/h；600 DEG C are raised to by 450 DEG C, heating rate is 75 DEG C/h；In 600 DEG C of heat preservation 1h；900 DEG C are raised to by 600 DEG C, heating speed
Rate is 75 DEG C/h；1080 DEG C are raised to by 900 DEG C, heating rate is 90 DEG C/h；1320 DEG C are raised to by 1080 DEG C, heating rate 80
℃/h；Room temperature is naturally cooled to by 1320 DEG C, obtains microwave dielectric ceramic materials.
Embodiment 9-2
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-2.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 9-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 9-3
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-3.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 9-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 9-4
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-4.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 9-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
Embodiment 9-5
Component A, B component, component C, D component and component E are mixed, wherein component A, B component, component C, D component and E group
The ingredient and dosage divided is identical as embodiment 1-5.
Ball milling is granulated, presses after mixing component A, B component, component C, D component and component E according to the method for embodiment 9-1
System, firing and cooling, obtain microwave dielectric ceramic materials.
The performance for the microwave dielectric ceramic materials that above-described embodiment obtains is tested, test result is as shown in table 5:
The performance for the microwave dielectric ceramic materials that 5 embodiment of table obtains
If the resonance frequency of microwave dielectric material varies with temperature, the carrier signal of filter will also be varied with temperature and be floated
It moves, the service performance of communication equipment is influenced, therefore it is required that dielectric material is necessary to ensure that resonance frequency cannot be with variation of ambient temperature
It is too big.By experimental data it is found that microwave dielectric ceramic materials provided by the invention are in -40 DEG C~100 DEG C of operating temperature, material
The frequency-temperature coefficient of material≤8ppm/ DEG C illustrates the resonance frequency of microwave dielectric ceramic materials provided by the invention close to zero
It is smaller.
In addition, by above-mentioned data it is found that microwave dielectric ceramic materials provided by the invention dielectric constant with higher, Q
Value is higher, and medium insertion loss is smaller, makes the product device being prepared using microwave dielectric ceramic materials of the present invention
As the size of filter can be smaller.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of microwave dielectric ceramic materials, which is characterized in that in terms of mass parts, the microwave dielectric ceramic materials by component A,
B component, component C, D component and component E are prepared, and wherein component A is BaTi4O9, the mass fraction of component A is 65~75%；
B component is Ba2Ti9O20, the mass fraction of B component is 20%~24%；Component C is BaWO4, the mass fraction of component C is
0.2%~5.5%；D group is divided into ZnTiO3、SnTiO3、LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Mixture, D group
The mass fraction divided is 0.001%~1%；Component E is by CaO, MgO and SiO2Mixture be successively sintered and cooled down to obtain, E
The mass fraction of component is 4%~10%.
2. microwave dielectric ceramic materials according to claim 1, which is characterized in that ZnTiO in the D component3、SnTiO3、
LaTiO3、NdTiO3、BaSm2Ti4O12And PrTiO3Mass ratio be 26~27:24~25:15.5~16.5:15.5~16.5:
8~9:8~9.
3. microwave dielectric ceramic materials according to claim 1, which is characterized in that SiO in the component E2, CaO and MgO
Mass ratio be 9~11:2~4:1.
4. microwave dielectric ceramic materials according to claim 1 or 3, which is characterized in that the preparation method packet of the component E
Include following steps:
By CaO, MgO and SiO2It after mixing, is sintered, then cooling obtains component E；The sintering processes include successively
7 stages carried out, specially the first heating stage, the second temperature rise period, third constant temperature stage, the 4th temperature rise period, the 5th
Constant temperature stage, the 6th temperature rise period, the 7th constant temperature stage；The cooling treatment includes two stages successively carried out, including the
One cooling stage and the second cooling stage；The design parameter of the sintering processes and cooling treatment is as shown in table 1:
Table 1 prepares the sintering processes and cooling treatment parameter when component E
5. microwave dielectric ceramic materials according to claim 1, which is characterized in that the composition of the microwave dielectric ceramic materials
For it is following composition 1~composition 5 in any one:
Form 1:A component 65%, B component 24%, component C 0.2%, D component 0.8%, component E 10%；
Form 2:A component 66%, B component 23%, component C 2.3%, D component 0.7%, component E 8%；
Form 3:A component 68%, B component 22%, component C 3.4%, D component 0.6%, component E 6%；
Form 4:A component 69%, B component 21%, component C 4.5%, D component 0.5%, component E 5%；
Form 5:A component 70%, B component 20%, component C 5.5%, D component 0.5%, component E 4%.
6. the preparation method of any one of Claims 1 to 5 microwave dielectric ceramic materials, comprising the following steps:
(1) binder after component A, B component, component C, D component and component E mixing and ball milling, will be added to be granulated, obtains powder
Grain；
(2) powder is subjected to compression process, obtains green body；
(3) it is cooled down after the green body being carried out firing processing, obtains microwave dielectric ceramic materials.
7. preparation method according to claim 6, which is characterized in that compacting includes four successively carried out in (2)
Stage, specially matched moulds stage, sizing exhaust intermediate stage, sizing are vented ultimate stage and packing stage；Wherein
The time of matched moulds stage is 6~8s, and pressure is 40~60kg/cm2；
The time of sizing exhaust intermediate stage is 1.5~2.5s, and pressure is 140~160kg/cm2；
The time that sizing is vented the ultimate stage is 2.5~3.5s, and pressure is 250~500kg/cm2；
The time of packing stage is 4.5~5.5s, and pressure is 450~500kg/cm2。
8. preparation method according to claim 6, which is characterized in that firing processing and cooling include three kinds in (3)
Method,
First method: firing processing includes 6 stages successively carrying out, specially the 1st temperature rise period, the 2nd temperature rise period, the
3 temperature rise periods, the 4th temperature rise period, the 5th temperature rise period and the 6th constant temperature stage；Cooling treatment includes two ranks successively carried out
Section, specially the 1st cooling stage and the 2nd cooling stage；The design parameter of the firing and cooling treatment is as shown in table 2:
Table 2 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
Second method: firing processing includes 7 stages successively carrying out, specially the 1st ' temperature rise period, the 2nd ' temperature rise period,
3rd ' constant temperature stage, the 4th ' temperature rise period, the 5th ' temperature rise period, the 6th ' constant temperature stage and the 7th ' temperature rise period；At the firing
The design parameter of reason and cooling treatment is as shown in table 3:
Table 3 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
The third method: it is burnt into 8 stages including successively carrying out that handle, the specially the 1st " temperature rise period, the 2nd " temperature rise period,
3rd " temperature rise period, the 4th " constant temperature stage, the 5th " temperature rise period, the 6th " temperature rise period, the 7th " temperature rise period and the 8th " constant temperature rank
Section；The design parameter of the firing processing and cooling treatment is as shown in table 4:
Table 4 prepares the firing processing and cooling treatment parameter of microwave dielectric ceramic materials
9. any one of any one of Claims 1 to 5 microwave dielectric ceramic materials or claim 6~8 the method system
Application of the standby obtained microwave dielectric ceramic materials in filter.
10. a kind of filter ceramic material, which is characterized in that the filter ceramic material is by any one of Claims 1 to 5 institute
State microwave dielectric ceramic materials that any one of microwave dielectric ceramic materials or claim 6~8 the method is prepared according to
It is secondary uniformly to paint silver paste, silver ink firing and polarization through silk-screen and obtain.
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