CN103626488B - Microwave ceramic dielectric material and preparation method thereof - Google Patents
Microwave ceramic dielectric material and preparation method thereof Download PDFInfo
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Abstract
A kind of microwave ceramic dielectric material, comprise principal crystalline phase, property-modifying additive and sintering fusing assistant, the structural formula of principal crystalline phase is: xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65; Property-modifying additive is MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture; Sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO.Above-mentioned microwave ceramic dielectric material, principal crystalline phase uniform particles, grain refining, make above-mentioned microwave ceramic dielectric material can at 1100 ~ 1250 DEG C of sintering, and still can keep higher Qf value while saving production cost, be 35000 ~ 45000GHz, dielectric constant K, τ
fin certain limit continuously adjustabe (K value: 35 ~ 48, τ f:0 ± 20ppm/ DEG C).The present invention also provides a kind of preparation method of microwave ceramic dielectric material.
Description
Technical field
The present invention relates to media ceramic field, particularly relate to a kind of microwave ceramic dielectric material and preparation method thereof.
Background technology
Microwave ceramics is the core material of microwave device.Recently for over ten years, because microwave technology equipment is to miniaturization and integrated, especially to the fast development in the large output of the product for civilian use, low price direction, add that electronic ceramics is in rapid progress the most in the last thirty years, make the research of microwave ceramics and practically to develop rapidly, having have developed large quantities of microwave ceramic dielectric material being applicable to various microwave frequency band at present.Be applied to the media ceramic of microwave circuit, meet specific inductivity K and temperature coefficient of resonance frequency τ
funder the prerequisite required, require that material has higher quality factor q to improve signal to noise ratio.In recent years, along with mobile communication, satellite communication particularly the developing rapidly of digital satellite television, people to be widely used in the fields such as mobile communication base station, digital TV receiving system and military radar there is Medium dielectric constant, the research of microwave-medium ceramics of high quality factor gets more and more.MTiO
3-LnAlO
3(M:Sr, Ca; Ln:La, Nd, Sm) system material is the one studying more.But traditional microwave ceramic dielectric material is when having higher Qf value, sintering temperature is all higher, is 1300 ~ 1500 DEG C, which greatly limits their application.
Summary of the invention
Based on this, being necessary for traditional microwave ceramic dielectric material problem that sintering temperature is high when having higher Qf value, providing a kind of and there is higher Qf value and can the microwave ceramic dielectric material of intermediate sintering temperature.
A kind of preparation method of microwave ceramic dielectric material is provided further.
A kind of microwave ceramic dielectric material, comprise principal crystalline phase, property-modifying additive and sintering fusing assistant, the structural formula of described principal crystalline phase is: xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65; Described property-modifying additive is MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture; Described sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO.
Wherein in an embodiment, in described microwave ceramic dielectric material, the molar content of described principal crystalline phase is 92 ~ 97%, and the molar content of described property-modifying additive is 0.5 ~ 4.5%, and the molar content of described sintering fusing assistant is 1.5 ~ 5.4%.
Wherein in an embodiment, in described microwave ceramic dielectric material, described MnO
2molar content be 0.2 ~ 1.5%, described Nb
2o
5molar content be 0.2 ~ 1%, the molar content of described MgO is 0.1 ~ 1%, described Y
2o
3molar content be 0 ~ 1%.
Wherein in an embodiment, in described microwave ceramic dielectric material, described SiO
2molar content be 0.3 ~ 1.5%, the molar content of described ZnO is 0.5 ~ 1.5%, described Li
2the molar content of O is 0.2 ~ 0.8%, described K
2the molar content of O is 0 ~ 0.6%, and the molar content of described BaO is 0.5 ~ 1%.
Above-mentioned microwave ceramic dielectric material, principal crystalline phase uniform particles, grain refining, property-modifying additive adopts MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture, sintering fusing assistant adopt SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO, makes above-mentioned microwave ceramic dielectric material can at 1100 ~ 1250 DEG C of sintering, and still can keep higher Qf value while saving production cost, be 35000 ~ 45000GHz.
A preparation method for microwave ceramic dielectric material, comprises the following steps:
There is provided principal crystalline phase, property-modifying additive and sintering fusing assistant, the structural formula of described principal crystalline phase is xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65, and described property-modifying additive is MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture, described sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO;
By described principal crystalline phase, property-modifying additive and the mixing of sintering fusing assistant, add deionized water, grind and obtain mixture in 10 ~ 20 hours; And
In described mixture, add polyvinyl alcohol granulation, at 1100 ~ 1250 DEG C of sintering, 3 ~ 5 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material.
Wherein in an embodiment, described principal crystalline phase is prepared by following steps:
By structural formula xRTiO
3-(1-x) LnAlO
3stoichiometric ratio take RCO
3, Ln
2o
3, TiO
2and Al
2o
3obtain raw material, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65;
In described raw material, add deionized water, grind 10 ~ 20 hours, dry and obtain dry powder;
Described dry powder is heated to 1050 ~ 1150 DEG C, is incubated 2.5 ~ 5 hours, is cooled to room temperature, obtains described principal crystalline phase, the structural formula of described principal crystalline phase is xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65.
Wherein in an embodiment, in described microwave ceramic dielectric material, the molar content of described principal crystalline phase is 92 ~ 97%, and the molar content of described property-modifying additive is 0.5 ~ 4.5%, and the molar content of described sintering fusing assistant is 1.5 ~ 5.4%.
Wherein in an embodiment, in described microwave ceramic dielectric material, described MnO
2molar content be 0.2 ~ 1.5%, described Nb
2o
5molar content be 0.2 ~ 1%, the molar content of described MgO is 0.1 ~ 1%, described Y
2o
3molar content be 0 ~ 1%.
Wherein in an embodiment, in described microwave ceramic dielectric material, described SiO
2molar content be 0.3 ~ 1.5%, the molar content of described ZnO is 0.5 ~ 1.5%, described Li
2the molar content of O is 0.2 ~ 0.8%, described K
2the molar content of O is 0 ~ 0.6%, and the molar content of described BaO is 0.5 ~ 1%.
Wherein in an embodiment, be heated in the step of 1050 ~ 1150 DEG C by described dry powder, described heating rate is 3.5 ~ 6.4 DEG C/min.
The preparation method of above-mentioned microwave-medium ceramics is simple, at 1100 ~ 1250 DEG C of sintering, and can meet environmental requirement, nontoxic, environmentally safe.
Accompanying drawing explanation
Fig. 1 is preparation method's schema of the microwave ceramic dielectric material of an embodiment.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
A kind of microwave ceramic dielectric material, comprises principal crystalline phase, property-modifying additive and sintering fusing assistant.The structural formula of principal crystalline phase is: xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65.Property-modifying additive is MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture.Sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO.
Above-mentioned principal crystalline phase is stable, active high, uniform particles and grain refining, can save energy.Property-modifying additive and sintering fusing assistant adopt environment-friendly materials, nontoxic, pollution-free.
Preferably, in described microwave ceramic dielectric material, the molar content of principal crystalline phase is 92 ~ 97%.The molar content of property-modifying additive is 0.5 ~ 4.5%.The molar content of sintering fusing assistant is 1.5 ~ 5.4%.
Preferably, in described microwave ceramic dielectric material, MnO
2molar content be 0.2 ~ 1.5%.Nb
2o
5molar content be 0.2 ~ 1%.The molar content of MgO is 0.1 ~ 1%.Y
2o
3molar content be 0 ~ 1%.
Preferably, in described microwave ceramic dielectric material, SiO
2molar content be 0.3 ~ 1.5%.The molar content of ZnO is 0.5 ~ 1.5%.Li
2the molar content of O is 0.2 ~ 0.8%.K
2the molar content of O is 0 ~ 0.6%.The molar content of BaO is 0.5 ~ 1%.
The grain growing of above-mentioned microwave ceramic dielectric material sintering porcelain body evenly, fine and close, inclusion-free and few defect, principal crystalline phase uniform particles, grain refining, property-modifying additive adopts MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture, sintering fusing assistant adopt SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO, makes above-mentioned microwave ceramic dielectric material can at 1100 ~ 1250 DEG C of sintering, and cost-saving, still can keep higher Qf value, be 35000 ~ 45000GHz simultaneously.And dielectric constant K, τ
fin certain limit continuously adjustabe (K value: 35 ~ 48, τ f:-20 ~ 20ppm/ DEG C).Above-mentioned microwave ceramic dielectric material for the manufacture of element, stable performance.
In addition, above-mentioned microwave ceramic dielectric material, has the features such as environmental protection, material scatter is high, moulding process is good.
Refer to Fig. 1, the preparation method of the microwave ceramic dielectric material of an embodiment, comprises the following steps:
S110, by structural formula xRTiO
3-(1-x) LnAlO
3stoichiometric ratio take RCO
3, Ln
2o
3, TiO
2and Al
2o
3obtain raw material, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65.
By RCO
3, Ln
2o
3, TiO
2and Al
2o
3mixing, RCO
3, Ln
2o
3, TiO
2and Al
2o
3between molar relationship meet structural formula xRTiO
3-(1-x) LnAlO
3, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65.
S120, in described raw material, add deionized water, grind 10 ~ 20 hours, dry and obtain dry powder.
In the present embodiment, grinding adopts zirconia ball to do grinding medium.Zirconia ball has smooth work sphere, is particularly suitable for the excellent pin-type sand mill etc. of vertical mixing mill, Horizontal stirring mill, vibration mill and various high linear speed.
In the present embodiment, described oven dry adopts bread furnace or spray tower to dry.
S130, described dry powder is heated to 1050 ~ 1150 DEG C, is incubated 2.5 ~ 5 hours, is cooled to room temperature, obtains described principal crystalline phase.
Wherein, the structural formula of principal crystalline phase is xRTiO
3-(1-x) LnAlO
3, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65.
In the present embodiment, be heated in the step of 1050 ~ 1150 DEG C by described dry powder, heating rate is 3.5 ~ 6.4 DEG C/min.Intensification and insulating process carry out in microwave sintering kiln or the long stove of high temp tunnel.Room temperature is 0 ~ 40 DEG C.
The preparation method of the principal crystalline phase of step S110 ~ step S130 is quick pre-burning solid phase method technique, compared with conventional solid-state method technique, quick burn-in process time shorten more than 1/3rd, and the principal crystalline phase uniform particles obtained, grain refining, stable and there is high reactivity, save the energy.
Be appreciated that the preparation method of principal crystalline phase is not limited to step S110 ~ step S130, other preparation methods, obtain above-mentioned principal crystalline phase as long as last.
S140, by described principal crystalline phase, property-modifying additive and sintering fusing assistant mixing, add deionized water, grind and obtain mixture in 10 ~ 20 hours.
Wherein, property-modifying additive is MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture.
Sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO.
Preferably, in described microwave ceramic dielectric material, the molar content of described principal crystalline phase is 92 ~ 97%, and the molar content of described property-modifying additive is 0.5 ~ 4.5%, and the molar content of described sintering fusing assistant is 1.5 ~ 5.4%.
Preferably, in described microwave ceramic dielectric material, MnO
2molar content be 0.2 ~ 1.5%, Nb
2o
5molar content be the molar content of 0.2 ~ 1%, MgO be 0.1 ~ 1%, Y
2o
3molar content be 0 ~ 1%.
Be appreciated that and work as Y
2o
3when molar content in described microwave ceramic dielectric material is 0, property-modifying additive is MnO
2, Nb
2o
5with the mixture of MgO.
Preferably, in described microwave ceramic dielectric material, SiO
2molar content be 0.3 ~ 1.5%, the molar content of described ZnO is 0.5 ~ 1.5%, described Li
2the molar content of O is 0.2 ~ 0.8%, described K
2the molar content of O is 0 ~ 0.6%, and the molar content of described BaO is 0.5 ~ 1%.
Be appreciated that and work as K
2when the molar content of O in described microwave ceramic dielectric material is 0, sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO.
Property-modifying additive and sintering fusing assistant adopt environment-friendly materials, nontoxic, pollution-free.
S150, in described mixture, add polyvinyl alcohol granulation, at 1100 ~ 1250 DEG C of sintering, 3 ~ 5 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material.
In the present embodiment, polyvinyl alcohol is binding agent.
It should be noted that, if directly provide principal crystalline phase, then step S110 ~ step S130 can omit.
The preparation method of above-mentioned microwave-medium ceramics is simple, at 1100 ~ 1250 DEG C of sintering, and can meet environmental requirement, nontoxic, environmentally safe.
Table 1 is the microwave dielectric ceramic materials prepared of an embodiment and numbering thereof.
Table 1
Use Agilent network analyzer, adopt flat band method test material to be numbered the specific inductivity of the microwave dielectric ceramic materials of 1 ~ 6, with closing cell method test Qf value and τ
f, it the results are shown in Table 2.
Table 2
Associative list 1, table 2 can be found out, along with the increase of the molar content of principal crystalline phase in microwave dielectric ceramic materials, dielectric constant K continuously adjustabe, Qf value also increases thereupon.When in microwave dielectric ceramic materials, the molar content of principal crystalline phase is 97%, and the molar content of property-modifying additive is 1.1%, and when the molar content of sintering fusing assistant is 1.9, Qf value is maximum, is 41800GHZ.
Table 3 is the microwave dielectric ceramic materials prepared of an embodiment and numbering thereof.
Table 3
Use Agilent network analyzer, adopt flat band method test material to be numbered the specific inductivity of the microwave dielectric ceramic materials of 7 ~ 12, with closing cell method test Qf value and τ
f, it the results are shown in Table 4.
Table 4
Associative list 3, table 4 can be found out, along with the increase of the molar content of principal crystalline phase in microwave dielectric ceramic materials, specific inductivity continuously adjustabe, Qf value also increases thereupon.When in microwave dielectric ceramic materials, the molar content of principal crystalline phase is 96%, and the molar content of property-modifying additive is 1.6%, and when the molar content of sintering fusing assistant is 2.4%, Qf value is maximum, is 43600GHZ.
It is below specific embodiment.
Embodiment 1
By the CaCO of 0.55mol
3, the La of 0.225mol
2o
3, the TiO of 0.55mol
2and the Al of 0.225mol
2o
3mixing, is that mill is situated between with zirconia ball, adds deionized water, grind 10 hours, dry obtain dry powder with bread furnace.Dry powder was risen to 1050 DEG C by room temperature through 3 hours in microwave sintering kiln, and 1050 DEG C of insulations 2.5 hours, be down to room temperature, obtain principal crystalline phase, its structural formula was 0.55CaTiO
3-0.45LaAlO
3.
By the MnO of 0.01mol
2, the Nb of 0.01mol
2o
5, the Y of MgO and 0.015mol of 0.01mol
2o
3be mixed to get property-modifying additive.
By the SiO of 0.01mol
2, the Li of the ZnO of 0.01mol, 0.005mol
2the K of O, 0.005mol
2the BaO of O and 0.005mol is mixed to get sintering fusing assistant.
By the principal crystalline phase of 0.92mol, above-mentioned property-modifying additive and the mixing of sintering fusing assistant, be that mill is situated between with zirconia ball, add deionized water, grind and obtain mixture in 10 hours.In mixture, add polyvinyl alcohol granulation, at 1100 DEG C of sintering, 3 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material.
Embodiment 2
By the CaCO of 0.65mol
3, the La of 0.175mol
2o
3, the TiO of 0.65mol
2and the Al of 0.175mol
2o
3mixing, is that mill is situated between with zirconia ball, adds deionized water, grind 20 hours, dry obtain dry powder with spray tower.Dry powder was risen to 1150 DEG C by room temperature through 5 hours in the long stove of high temp tunnel, and 1150 DEG C of insulations 5 hours, be down to room temperature, obtain principal crystalline phase, its structural formula was 0.65CaTiO
3-0.35LaAlO
3.
By the MnO of 0.005mol
2, the Nb of 0.005mol
2o
5and the MgO of 0.005mol is mixed to get property-modifying additive.
By the SiO of 0.003mol
2, the Li of the ZnO of 0.005mol, 0.002mol
2the BaO of O and 0.005mol is mixed to get sintering fusing assistant.
By the principal crystalline phase of 0.97mol, above-mentioned property-modifying additive and the mixing of sintering fusing assistant, be that mill is situated between with zirconia ball, add deionized water, grind and obtain mixture in 20 hours.In mixture, add polyvinyl alcohol granulation, at 1250 DEG C of sintering, 5 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material.
Embodiment 3
By the SrCO of 0.6mol
3, the Sm of 0.2mol
2o
3, the TiO of 0.6mol
2and the Al of 0.2mol
2o
3mixing, is that mill is situated between with zirconia ball, adds deionized water, grind 15 hours, dry obtain dry powder with spray tower.Dry powder was risen to 1100 DEG C by room temperature through 4 hours in the long stove of high temp tunnel, and 1100 DEG C of insulations 4 hours, be down to room temperature, obtain principal crystalline phase, its structural formula was 0.6SrTiO
3-0.4SmAlO
3.
By the MnO of 0.005mol
2, the Nb of 0.005mol
2o
5, the Y of MgO and 0.01mol of 0.005mol
2o
3be mixed to get property-modifying additive.
By the SiO of 0.01mol
2, the Li of the ZnO of 0.01mol, 0.004mol
2the K of O, 0.005mol
2the BaO of O and 0.006mol is mixed to get sintering fusing assistant.
By the principal crystalline phase of 0.94mol, above-mentioned property-modifying additive and the mixing of sintering fusing assistant, be that mill is situated between with zirconia ball, add deionized water, grind and obtain mixture in 15 hours.In mixture, add polyvinyl alcohol granulation, at 1150 DEG C of sintering, 4 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material.
Embodiment 4
By the SrCO of 0.55mol
3, the Sm of 0.225mol
2o
3, the TiO of 0.55mol
2and the Al of 0.225mol
2o
3mixing, is that mill is situated between with zirconia ball, adds deionized water, grind 10 hours, dry obtain dry powder with bread furnace.Dry powder was risen to 1050 DEG C by room temperature through 3 hours in microwave sintering kiln, and 1050 DEG C of insulations 2.5 hours, be down to room temperature, obtain principal crystalline phase, its structural formula was 0.55SrTiO
3-0.45SmAlO
3.
By the MnO of 0.01mol
2, the Nb of 0.01mol
2o
5, the Y of MgO and 0.015mol of 0.01mol
2o
3be mixed to get property-modifying additive.
By the SiO of 0.01mol
2, the Li of the ZnO of 0.01mol, 0.005mol
2the K of O, 0.005mol
2the BaO of O and 0.005mol is mixed to get sintering fusing assistant.
By the principal crystalline phase of 0.92mol, above-mentioned property-modifying additive and the mixing of sintering fusing assistant, be that mill is situated between with zirconia ball, add deionized water, grind and obtain mixture in 10 hours.In mixture, add polyvinyl alcohol granulation, at 1100 DEG C of sintering, 3 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material.
Embodiment 5
By the SrCO of 0.65mol
3, the Sm of 0.175mol
2o
3, the TiO of 0.65mol
2and the Al of 0.175mol
2o
3mixing, is that mill is situated between with zirconia ball, adds deionized water, grind 20 hours, dry obtain dry powder with spray tower.Dry powder was risen to 1150 DEG C by room temperature through 5 hours in the long stove of high temp tunnel, and 1150 DEG C of insulations 5 hours, be down to room temperature, obtain principal crystalline phase, its structural formula was 0.65SrTiO
3-0.35SmAlO
3.
By the MnO of 0.005mol
2, the Nb of 0.005mol
2o
5and the MgO of 0.005mol is mixed to get property-modifying additive.
By the SiO of 0.003mol
2, the Li of the ZnO of 0.005mol, 0.002mol
2the BaO of O and 0.005mol is mixed to get sintering fusing assistant.
By the principal crystalline phase of 0.97mol, above-mentioned property-modifying additive and the mixing of sintering fusing assistant, be that mill is situated between with zirconia ball, add deionized water, grind and obtain mixture in 20 hours.In mixture, add polyvinyl alcohol granulation, at 1250 DEG C of sintering, 5 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (4)
1. a microwave ceramic dielectric material, comprise principal crystalline phase, property-modifying additive and sintering fusing assistant, it is characterized in that, the structural formula of described principal crystalline phase is: xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65; Described property-modifying additive is MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture; Described sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO; In described microwave ceramic dielectric material, the molar content of described principal crystalline phase is 92 ~ 97%, and the molar content of described property-modifying additive is 0.5 ~ 4.5%, and the molar content of described sintering fusing assistant is 1.5 ~ 5.4%, in described microwave ceramic dielectric material, described MnO
2molar content be 0.2 ~ 1.5%, described Nb
2o
5molar content be 0.2 ~ 1%, the molar content of described MgO is 0.1 ~ 1%, described Y
2o
3molar content be 0 ~ 1%, in described microwave ceramic dielectric material, described SiO
2molar content be 0.3 ~ 1.5%, the molar content of described ZnO is 0.5 ~ 1.5%, described Li
2the molar content of O is 0.2 ~ 0.8%, described K
2the molar content of O is 0 ~ 0.6%, and the molar content of described BaO is 0.5 ~ 1%.
2. a preparation method for microwave ceramic dielectric material, is characterized in that, comprises the following steps:
There is provided principal crystalline phase, property-modifying additive and sintering solubility promoter, the structural formula of described principal crystalline phase is xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65, and described property-modifying additive is MnO
2, Nb
2o
5with mixture or the MnO of MgO
2, Nb
2o
5, MgO and Y
2o
3mixture, described sintering fusing assistant is SiO
2, ZnO, Li
2the mixture of O and BaO or SiO
2, ZnO, Li
2o, K
2the mixture of O and BaO, in described microwave ceramic dielectric material, described MnO
2molar content be 0.2 ~ 1.5%, described Nb
2o
5molar content be 0.2 ~ 1%, the molar content of described MgO is 0.1 ~ 1%, described Y
2o
3molar content be 0 ~ 1%, described SiO
2molar content be 0.3 ~ 1.5%, the molar content of described ZnO is 0.5 ~ 1.5%, described Li
2the molar content of O is 0.2 ~ 0.8%, described K
2the molar content of O is 0 ~ 0.6%, and the molar content of described BaO is 0.5 ~ 1%;
By described principal crystalline phase, property-modifying additive and the mixing of sintering fusing assistant, add deionized water, grind and obtain mixture in 10 ~ 20 hours; And
In described mixture, add polyvinyl alcohol granulation, at 1100 ~ 1250 DEG C of sintering, 3 ~ 5 hours removing polyvinyl alcohol, obtain described microwave ceramic dielectric material,
In described microwave ceramic dielectric material, the molar content of described principal crystalline phase is 92 ~ 97%, and the molar content of described property-modifying additive is 0.5 ~ 4.5%, and the molar content of described sintering fusing assistant is 1.5 ~ 5.4%.
3. the preparation method of microwave ceramic dielectric material as claimed in claim 2, it is characterized in that, described principal crystalline phase is prepared by following steps:
By structural formula xRTiO
3-(1-x) LnAlO
3stoichiometric ratio take RCO
3, Ln
2o
3, TiO
2and Al
2o
3obtain raw material, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65;
In described raw material, add deionized water, grind 10 ~ 20 hours, dry and obtain dry powder;
Described dry powder is heated to 1050 ~ 1150 DEG C, is incubated 2.5 ~ 5 hours, is cooled to room temperature, obtains described principal crystalline phase, the structural formula of described principal crystalline phase is xRTiO
3-(1-x) LnAlO
3, wherein, R is Ca or Sr, Ln is La or Sm, 0.55≤x≤0.65.
4. the preparation method of microwave ceramic dielectric material as claimed in claim 3, it is characterized in that, be heated in the step of 1050 ~ 1150 DEG C by described dry powder, described heating rate is 3.5 ~ 6.4 DEG C/min.
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| CN104193325B (en) * | 2014-08-28 | 2016-02-17 | 云南云天化股份有限公司 | A kind of ceramic powder, its preparation method, microwave dielectric ceramic powder and preparation method thereof |
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| CN111825445B (en) * | 2019-04-22 | 2023-02-17 | 中南大学深圳研究院 | High-dielectric-constant microwave dielectric ceramic material, preparation and application thereof |
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| CN110734284A (en) * | 2019-11-11 | 2020-01-31 | 深圳顺络电子股份有限公司 | medium high Q microwave medium ceramic material and preparation method thereof |
| CN111116186B (en) * | 2020-01-03 | 2022-02-22 | 山东国瓷功能材料股份有限公司 | Low-dielectric-constant two-phase composite microwave dielectric ceramic material and preparation method thereof |
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| CN112759383B (en) * | 2021-02-18 | 2022-10-28 | 山东国瓷功能材料股份有限公司 | Microwave dielectric ceramic with medium dielectric constant and preparation method thereof |
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