CN103193489B - Preparation method and using method of additive capable of increasing microwave ceramic Q value - Google Patents
Preparation method and using method of additive capable of increasing microwave ceramic Q value Download PDFInfo
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- CN103193489B CN103193489B CN201310124235.7A CN201310124235A CN103193489B CN 103193489 B CN103193489 B CN 103193489B CN 201310124235 A CN201310124235 A CN 201310124235A CN 103193489 B CN103193489 B CN 103193489B
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Abstract
The invention discloses a preparation method and a using method of an additive capable of increasing microwave ceramic Q value. A mixed additive is prepared by wrapping ZnO microparticles by La(NO3)2 nanoparticles; and the mixed additive is added into microwave ceramic raw material powder to synthesize microwave ceramic with Q value up to 6600, 10 GHz. The mixed additive is simple in preparation process, high in synthesis speed, high in wrapping ratio, low in cost, stable in performance and convenient to use, so the mixed additive has a wide market prospect in the field of microwave ceramic.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, be specifically related to a kind of preparation method and using method thereof that improves the additive of microwave ceramics Q value.
Background technology
Microwave ceramics refers to and is applied in microwave frequency band circuit as dielectric material and completes the pottery of one or more functions, and it is widely used in the fields such as mobile communication, satellite communication and military radar.Along with science and technology development with rapid changepl. never-ending changes and improvements, the swift and violent increase of communication information amount, and the requirement of people to radio communication, oneself becomes the inexorable trend of current development communication technologies to use the microwave telecommunication systems such as satellite communication and direct satellite broadcasting TV.But microwave current media ceramic exists the deficiency that Q value is not high enough, firing temperature is higher, seriously limited it at Novel movable signal equipment, the application in mobile communication base station.Therefore, the Q value of the sintering temperature of reduction microwave ceramics and raising microwave ceramics is the difficult problem during microwave ceramics is produced always.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of technique is simple, production cost is low, synthesis rate is fast, can obviously improves preparation method and the using method thereof of the additive of microwave ceramics Q value.
For solving above technical problem, technical scheme of the present invention is: a kind of preparation method who improves microwave ceramics Q value additive, is characterized in that comprising the steps:
The first step: take respectively analytically pure micron ZnO and nanometer La (NO
3)
3powder, measures a certain amount of distilled water and pours in the container that fills ZnO powder, then with ultrasonic cleaner, disperses 15 minutes, obtains A solution; Measuring a certain amount of distilled water pours into and fills La (NO
3)
3in the container of powder, then with glass stick, be stirred to La (NO
3)
3powder dissolves completely, obtains B solution;
Second step: put into magnetic force in A solution, then to put into bath temperature be the container of 60～80 ℃, be placed on magnetic agitation applicator platform and stir, then B solution is poured in A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, be adjusted to pH value to 9, controlling the reaction times is 30～70 minutes;
The 4th step: mixed solution C is taken out, standing 24 hours, then use suction filtration machine suction filtration, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in crucible, adopt conventional heating means calcining, then porphyrize obtains additive powder.
ZnO and La (NO in the described the first step
3)
3press Zn
+ 2with La
+ 3mol ratio be that 4:1 prepares burden.
In the described the first step, distilled water and ZnO mol ratio are 135:1, distilled water and La (NO
3)
3mol ratio is 272:1.
In described the 5th step, calcining temperature is 750 ℃, and soaking time is 15 minutes.
Granularity≤1.3 μ the m of additive powder in described the 5th step.
Encapsulation ratio >=65% of additive powder in described the 5th step.
The using method of above-mentioned additive, is characterized in that: additive is joined in microwave ceramics raw material, after ball milling, dry, pre-burning, ball milling, dry, granulation, moulding, sintering, obtain the microwave ceramics of high Q value.
The add-on of described additive is 1.2～1.8% of microwave ceramics raw material weight.
Described calcined temperature is 1080 ℃, and soaking time is 6 hours; Sintering temperature is 1220～1280 ℃, and soaking time is 4 hours
Described Ball-milling Time is 4 hours.
Innovation of the present invention is to utilize nano particle parcel micron particle to prepare mixed additive, then joined in microwave ceramics material powder, synthesizing Q value can be up to 6600, the microwave ceramics of 10GHz, this mixed additive preparation technology is simple, resultant velocity is fast, encapsulation ratio is high, cost is low, stable performance, easy to use, therefore in microwave ceramics field, has broad application prospects.
Accompanying drawing explanation
Fig. 1 is La
2o
3the SEM photo of nano particle parcel ZnO micron particle.
Embodiment
By embodiment, the present invention is further detailed explanation below.
Embodiment mono-:
The 1st step: press Zn
+ 2with La
+ 3mol ratio is 4:1, takes respectively analytically pure micron ZnO and nanometer La (NO
3)
3powder, is 135:1 by distilled water and ZnO mol ratio, measures a certain amount of distilled water and pours in the container that fills ZnO powder, then with ultrasonic cleaner, disperses 15 minutes, obtains A solution; Press distilled water and La (NO
3)
3mol ratio is 272:1, measures a certain amount of distilled water and pours into and fill La (NO
3)
3in the container of powder, then with glass stick, be stirred to La (NO
3)
3powder dissolves completely, obtains B solution;
The 2nd step: put into magnetic force in A solution, then to put into bath temperature be the container of 60 ℃, be placed on magnetic agitation applicator platform and stir, then B solution is poured in A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, be adjusted to pH value to 9, controlling the reaction times is 40 minutes;
The 4th step: mixed solution C is taken out, standing 24 hours, then use suction filtration machine suction filtration, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in crucible, adopt the calcining of conventional heating means, calcining temperature is 750 ℃ of insulations 15 minutes, porphyrize degree of obtaining≤1.2 μ m then, the additive powder that encapsulation ratio is 68%.
At microwave ceramics (Zr
0.8sn
0.2) TiO
4in add the additive of 1.2 wt %, through ball milling 4 hours, dry, 1080 ℃ of pre-burning insulations 6 hours, ball milling 4 hours, dry, granulation, moulding, 1220 ℃ of sintered heat insulatings, after 4 hours, obtain the microwave ceramics of ε=38.5, Q=4800, ζ f=-3.4.
At microwave ceramics (Mg
0.95ca
0.05) TiO
4in add the additive of 1.2 wt %, through ball milling 4 hours, dry, 1080 ℃ of pre-burning insulations 6 hours, ball milling 4 hours, dry, granulation, moulding, 1260 ℃ of sintered heat insulatings, after 4 hours, obtain the microwave ceramics of ε=20.6, Q=6500, ζ f=-3.2.
Embodiment bis-:
The 1st step: press Zn
+ 2with La
+ 3mol ratio is 4:1, takes respectively analytically pure micron ZnO and nanometer La (NO
3)
3powder, is 135:1 by distilled water and ZnO mol ratio, measures a certain amount of distilled water and pours in the container that fills ZnO powder, then with ultrasonic cleaner, disperses 15 minutes, obtains A solution; Press distilled water and La (NO
3)
3mol ratio is 272:1, measures a certain amount of distilled water and pours into and fill La (NO
3)
3in the container of powder, then with glass stick, be stirred to La (NO
3)
3powder dissolves completely, obtains B solution;
The 2nd step: put into magnetic force in A solution, then to put into bath temperature be the container of 70 ℃, be placed on magnetic agitation applicator platform and stir, then B solution is poured in A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, be adjusted to pH value to 9, controlling the reaction times is 50 minutes;
The 4th step: mixed solution C is taken out, standing 24 hours, then use suction filtration machine suction filtration, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in crucible, adopt the calcining of conventional heating means, calcining temperature is 750 ℃ of insulations 15 minutes, porphyrize degree of obtaining≤1.3 μ m then, encapsulation ratio is 70% additive powder.
At microwave ceramics (Zr
0.8sn
0.2) TiO
4in add the additive of 1.5 wt %, through ball milling 4 hours, dry, 1080 ℃ of pre-burning insulations 6 hours, ball milling 4 hours, dry, granulation, moulding, 1220 ℃ of sintered heat insulatings, after 4 hours, obtain the microwave ceramics of ε=38.3, Q=5200, ζ f=-4.2.
At microwave ceramics (Mg
0.95ca
0.05) TiO
4in add the additive of 1.5 wt %, through ball milling 4 hours, dry, 1080 ℃ of pre-burning insulations 6 hours, ball milling 4 hours, dry, granulation, moulding, 1260 ℃ of sintered heat insulatings, after 4 hours, obtain the microwave ceramics of ε=20.4, Q=6600, ζ f=-4.3.
Embodiment tri-:
The 1st step: press Zn
+ 2with La
+ 3mol ratio is 4:1, takes respectively analytically pure micron ZnO and nanometer La (NO
3)
3powder, is 135:1 by distilled water and ZnO mol ratio, measures a certain amount of distilled water and pours in the container that fills ZnO powder, then with ultrasonic cleaner, disperses 15 minutes, obtains A solution; Press distilled water and La (NO
3)
3mol ratio is 272:1, measures a certain amount of distilled water and pours into and fill La (NO
3)
3in the container of powder, then with glass stick, be stirred to La (NO
3)
3powder dissolves completely, obtains B solution;
The 2nd step: put into magnetic force in A solution, then to put into bath temperature be the container of 80 ℃, be placed on magnetic agitation applicator platform and stir, then B solution is poured in A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, be adjusted to pH value to 9, controlling the reaction times is 50 minutes;
The 4th step: mixed solution C is taken out, standing 24 hours, then use suction filtration machine suction filtration, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in crucible, adopt the calcining of conventional heating means, calcining temperature is 750 ℃ of insulations 15 minutes, porphyrize degree of obtaining≤1.2 μ m then, encapsulation ratio is 72% additive powder.
At microwave ceramics (Zr
0.8sn
0.2) TiO
4in add the additive of 1.7 wt %, through ball milling 4 hours, dry, 1080 ℃ of pre-burning insulations 6 hours, ball milling 4 hours, dry, granulation, moulding, 1220 ℃ of sintered heat insulatings, after 4 hours, obtain the microwave ceramics of ε=38.1, Q=5000, ζ f=-4.5.
At microwave ceramics (Mg
0.95ca
0.05) TiO
4in add the additive of 1.7 wt %, through ball milling 4 hours, dry, 1080 ℃ of pre-burning insulations 6 hours, ball milling 4 hours, dry, granulation, moulding, 1260 ℃ of sintered heat insulatings, after 4 hours, obtain the microwave ceramics of ε=20.2, Q=6400, ζ f=-3.5.
Above-mentioned microwave ceramics dielectric properties detection method is: first cylindrical ceramic sample is polished on sand paper, then used ultrasonic wave to clean in alcohol.Adopt the transverse electric field (TE of microwave frequency for the method for open type chamber
011mould) dielectric properties of analytic sample, test frequency is 4～7GHz, by measuring media resonant frequency variation with temperature rate, obtains sample temperature coefficient of resonance frequency, the temperature range of measurement is 25～75 ℃.
Listed is only the preferred embodiment of addictive preparation method of the present invention and application above, certainly can not limit with this interest field of the present invention, and the equivalent variations of therefore doing according to the present patent application the scope of the claims, still belongs to the scope that the present invention is contained.
Claims (2)
1. the preparation method that can improve microwave ceramics Q value additive, is characterized in that comprising the steps:
The first step: take respectively analytically pure micron ZnO and nanometer La (NO
3)
3powder, measures a certain amount of distilled water and pours in the container that fills ZnO powder, then with ultrasonic cleaner, disperses 15 minutes, obtains A solution; Measuring a certain amount of distilled water pours into and fills La (NO
3)
3in the container of powder, then with glass stick, be stirred to La (NO
3)
3powder dissolves completely, obtains B solution;
Second step: put into magnetic force in A solution, then to put into bath temperature be the container of 60～80 ℃, be placed on magnetic agitation applicator platform and stir, then B solution is poured in A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, be adjusted to pH value to 9, controlling the reaction times is 30～70 minutes;
The 4th step: mixed solution C is taken out, standing 24 hours, then use suction filtration machine suction filtration, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in crucible, adopt conventional heating means calcining, then porphyrize obtains additive powder.
2. the preparation method of additive according to claim 1, is characterized in that: ZnO and La (NO in the described the first step
3)
3press Zn
+ 2with La
+ 3mol ratio be that 4:1 prepares burden.
3
.according to claim 1, the preparation method of additive, is characterized in that: in the described the first step, distilled water and ZnO mol ratio are 135:1 distilled water and La (NO
3)
3mol ratio is 272:1.
4
.according to claim 1, the preparation method of additive, is characterized in that: in described the 5th step, calcining temperature is 750 ℃, and soaking time is 15 minutes.
5
.according to claim 1, the preparation method of additive, is characterized in that: the granularity≤1.3 μ m of additive powder in described the 5th step.
6
.according to claim 1, the preparation method of additive, is characterized in that: encapsulation ratio>=65% of additive powder in described the 5th step.
7
.using method according to additive described in claim 1-6 any one, is characterized in that: additive is joined in microwave ceramics raw material, after ball milling, dry, pre-burning, ball milling, dry, granulation, moulding, sintering, obtain the microwave ceramics of high Q value.
8
.the using method of additive according to claim 7, is characterized in that: the add-on of described additive is 1.2～1.8% of microwave ceramics raw material weight.
9
.the using method of additive according to claim 7, is characterized in that: described calcined temperature is 1080 ℃, and soaking time is 6 hours; Sintering temperature is 1220～1260 ℃, and soaking time is 4 hours.
10
.the using method of additive according to claim 7, is characterized in that: described Ball-milling Time is 4 hours.
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