CN103193489A - 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 PDF

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Publication number
CN103193489A
CN103193489A CN2013101242357A CN201310124235A CN103193489A CN 103193489 A CN103193489 A CN 103193489A CN 2013101242357 A CN2013101242357 A CN 2013101242357A CN 201310124235 A CN201310124235 A CN 201310124235A CN 103193489 A CN103193489 A CN 103193489A
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additive
powder
preparation
solution
hours
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CN103193489B (en
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吴坚强
彭悦
吴迪
王群
郭彗锋
曹良足
孙丽
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Jingdezhen Ceramic Institute
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Jingdezhen Ceramic Institute
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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

A kind of preparation method and using method thereof that improves the additive of microwave ceramics Q value
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 be applied in the microwave frequency band circuit as dielectric material and finishes the pottery of one or more functions, and it is widely used in fields such as mobile communication, satellite communication and military radar.Along with the development that science and technology is maked rapid progress, the swift and violent increase of communication information amount, and people are to the requirement of radio communication, oneself becomes the inexorable trend of current development communication technologies to use microwave telecommunication systems such as satellite communication and direct satellite broadcasting TV.But the microwave current media ceramic exists the deficiency that the Q value is not high enough, firing temperature is higher, has seriously limited it at novel mobile communication equipment, the application in the 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 provides that a kind of technology is simple, production cost is low, synthesis rate is fast, can obviously improve 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 by weighing analytically pure micron ZnO and nanometer La (NO respectively 3) 3Powder is measured a certain amount of distilled water and is poured in the container that fills the ZnO powder, disperses 15 minutes with ultrasonic cleaner then, obtains A solution; Measuring a certain amount of distilled water pours into and fills La (NO 3) 3In the container of powder, be stirred to La (NO with glass stick then 3) 3The powder dissolving obtains B solution fully;
Second step: in A solution, put into magnetic force, put into bath temperature again and be 60～80 ℃ container, place on the magnetic agitation applicator platform and stir, then B solution is poured in the A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, transfer to pH value to 9, the control reaction times is 30～70 minutes;
The 4th step: mixed solution C is taken out, left standstill 24 hours, use suction filtration machine suction filtration then, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in the crucible, adopt conventional heating means calcining, porphyrize obtains the additive powder then.
ZnO and La (NO in the described the first step 3) 3Press Zn + 2With La + 3Mol ratio be that 4:1 prepares burden.
Distilled water and ZnO mol ratio are 135:1 in the described the first step, distilled water and La (NO 3) 3Mol ratio is 272:1.
Calcining temperature is 750 ℃ in described the 5th step, 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 the microwave ceramics raw material, behind ball milling, drying, pre-burning, ball milling, drying, 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
The described ball milling time is 4 hours.
Innovation part of the present invention is to utilize nano particle parcel micron particle to prepare mixed additive, it is joined in the microwave ceramics material powder then, synthesizing the 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 has broad application prospects in the microwave ceramics field.
Description of drawings
Fig. 1 is La 2O 3The SEM photo of nano particle parcel ZnO micron particle.
Embodiment
The present invention is further detailed explanation with embodiment below.
Embodiment one:
The 1st step: press Zn + 2With La + 3Mol ratio is 4:1, takes by weighing analytically pure micron ZnO and nanometer La (NO respectively 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 the ZnO powder, disperses 15 minutes with ultrasonic cleaner then, 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, be stirred to La (NO with glass stick then 3) 3The powder dissolving obtains B solution fully;
The 2nd step: in A solution, put into magnetic force, put into bath temperature again and be 60 ℃ container, place on the magnetic agitation applicator platform and stir, then B solution is poured in the A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, transfer to pH value to 9, the control reaction times is 40 minutes;
The 4th step: mixed solution C is taken out, left standstill 24 hours, use suction filtration machine suction filtration then, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in the crucible, adopt conventional heating means calcining, calcining temperature is 750 ℃ of insulations 15 minutes, porphyrize degree of obtaining≤1.2 μ m then, and encapsulation ratio is 68% additive powder.
At microwave ceramics (Zr 0.8Sn 0.2) TiO 4In add the additive of 1.2 wt %, be incubated 6 hours, ball milling 4 hours, drying, granulation, moulding, 1220 ℃ of sintered heat insulatings obtain ε=38.5, Q=4800, ζ f=-3.4 after 4 hours microwave ceramics through ball milling 4 hours, drying, 1080 ℃ of pre-burnings.
At microwave ceramics (Mg 0.95Ca 0.05) TiO 4In add the additive of 1.2 wt %, be incubated 6 hours, ball milling 4 hours, drying, granulation, moulding, 1260 ℃ of sintered heat insulatings obtain ε=20.6, Q=6500, ζ f=-3.2 after 4 hours microwave ceramics through ball milling 4 hours, drying, 1080 ℃ of pre-burnings.
Embodiment two:
The 1st step: press Zn + 2With La + 3Mol ratio is 4:1, takes by weighing analytically pure micron ZnO and nanometer La (NO respectively 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 the ZnO powder, disperses 15 minutes with ultrasonic cleaner then, 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, be stirred to La (NO with glass stick then 3) 3The powder dissolving obtains B solution fully;
The 2nd step: in A solution, put into magnetic force, put into bath temperature again and be 70 ℃ container, place on the magnetic agitation applicator platform and stir, then B solution is poured in the A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, transfer to pH value to 9, the control reaction times is 50 minutes;
The 4th step: mixed solution C is taken out, left standstill 24 hours, use suction filtration machine suction filtration then, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in the crucible, adopt conventional heating means calcining, calcining temperature is 750 ℃ of insulations 15 minutes, porphyrize degree of obtaining≤1.3 μ m then, and encapsulation ratio is 70% additive powder.
At microwave ceramics (Zr 0.8Sn 0.2) TiO 4In add the additive of 1.5 wt %, be incubated 6 hours, ball milling 4 hours, drying, granulation, moulding, 1220 ℃ of sintered heat insulatings obtain ε=38.3, Q=5200, ζ f=-4.2 after 4 hours microwave ceramics through ball milling 4 hours, drying, 1080 ℃ of pre-burnings.
At microwave ceramics (Mg 0.95Ca 0.05) TiO 4In add the additive of 1.5 wt %, be incubated 6 hours, ball milling 4 hours, drying, granulation, moulding, 1260 ℃ of sintered heat insulatings obtain ε=20.4, Q=6600, ζ f=-4.3 after 4 hours microwave ceramics through ball milling 4 hours, drying, 1080 ℃ of pre-burnings.
Embodiment three:
The 1st step: press Zn + 2With La + 3Mol ratio is 4:1, takes by weighing analytically pure micron ZnO and nanometer La (NO respectively 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 the ZnO powder, disperses 15 minutes with ultrasonic cleaner then, 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, be stirred to La (NO with glass stick then 3) 3The powder dissolving obtains B solution fully;
The 2nd step: in A solution, put into magnetic force, put into bath temperature again and be 80 ℃ container, place on the magnetic agitation applicator platform and stir, then B solution is poured in the A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, transfer to pH value to 9, the control reaction times is 50 minutes;
The 4th step: mixed solution C is taken out, left standstill 24 hours, use suction filtration machine suction filtration then, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in the crucible, adopt conventional heating means calcining, calcining temperature is 750 ℃ of insulations 15 minutes, porphyrize degree of obtaining≤1.2 μ m then, and encapsulation ratio is 72% additive powder.
At microwave ceramics (Zr 0.8Sn 0.2) TiO 4In add the additive of 1.7 wt %, be incubated 6 hours, ball milling 4 hours, drying, granulation, moulding, 1220 ℃ of sintered heat insulatings obtain ε=38.1, Q=5000, ζ f=-4.5 after 4 hours microwave ceramics through ball milling 4 hours, drying, 1080 ℃ of pre-burnings.
At microwave ceramics (Mg 0.95Ca 0.05) TiO 4In add the additive of 1.7 wt %, be incubated 6 hours, ball milling 4 hours, drying, granulation, moulding, 1260 ℃ of sintered heat insulatings obtain ε=20.2, Q=6400, ζ f=-3.5 after 4 hours microwave ceramics through ball milling 4 hours, drying, 1080 ℃ of pre-burnings.
Above-mentioned microwave ceramics dielectric properties detection method is: at first the cylindrical ceramic sample is polished at sand paper, then it is cleaned in alcohol with ultrasonic wave.Adopt the open type chamber method transverse electric field (TE of microwave frequency 011Mould) dielectric properties of analytic sample, test frequency are 4～7GHz, obtain the sample temperature coefficient of resonance frequency by the measuring media resonant frequency with the variation of temperature rate, and the temperature range of measurement is 25～75 ℃.
More than listed only be the preferred embodiment of addictive preparation method of the present invention and application, can not limit the present invention's interest field certainly with this, therefore the equivalent variations of doing according to the present patent application claim still belongs to the scope that the present invention is contained.

Claims (10)

1. the preparation method that can improve microwave ceramics Q value additive is characterized in that comprising the steps:
The first step: take by weighing analytically pure micron ZnO and nanometer La (NO respectively 3) 3Powder is measured a certain amount of distilled water and is poured in the container that fills the ZnO powder, disperses 15 minutes with ultrasonic cleaner then, obtains A solution; Measuring a certain amount of distilled water pours into and fills La (NO 3) 3In the container of powder, be stirred to La (NO with glass stick then 3) 3The powder dissolving obtains B solution fully;
Second step: in A solution, put into magnetic force, put into bath temperature again and be 60～80 ℃ container, place on the magnetic agitation applicator platform and stir, then B solution is poured in the A solution, obtain mixed solution C;
The 3rd step: dropwise add ammoniacal liquor in mixed solution C, transfer to pH value to 9, the control reaction times is 30～70 minutes;
The 4th step: mixed solution C is taken out, left standstill 24 hours, use suction filtration machine suction filtration then, and washing precipitate repeatedly, dry throw out;
The 5th step: throw out is packed in the crucible, adopt conventional heating means calcining, porphyrize obtains the additive powder then.
2. according to the preparation method of the described additive of claim 1, it 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 the preparation method of the described additive of claim 1, it is characterized in that: distilled water and ZnO mol ratio are 135:1 in the described the first step, distilled water and La (NO 3) 3Mol ratio is 272:1.
4. according to the preparation method of the described additive of claim 1, it is characterized in that: calcining temperature is 750 ℃ in described the 5th step, and soaking time is 15 minutes.
5. according to the preparation method of the described additive of claim 1, it is characterized in that: the granularity≤1.3 μ m of additive powder in described the 5th step.
6. according to the preparation method of the described additive of claim 1, it is characterized in that: encapsulation ratio 〉=65% of additive powder in described the 5th step.
7. according to the using method of the arbitrary described additive of claim 1-6, it is characterized in that: additive is joined in the microwave ceramics raw material, behind ball milling, drying, pre-burning, ball milling, drying, granulation, moulding, sintering, obtain the microwave ceramics of high Q value.
8. the using method of additive according to claim 7, it 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, it is characterized in that: described calcined temperature is 1080 ℃, 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, it is characterized in that: the described ball milling time is 4 hours.
CN201310124235.7A 2013-04-11 2013-04-11 Preparation method and using method of additive capable of increasing microwave ceramic Q value Expired - Fee Related CN103193489B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104230350A (en) * 2014-09-18 2014-12-24 景德镇陶瓷学院 Preparation and usage method of additive for increasing Q value of microwave ceramic through microwave ceramic material wrapping

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515779A (en) * 2011-12-07 2012-06-27 中国科学院过程工程研究所 Rare earth oxide composite additive for zinc oxide varistor and preparation method thereof
CN102863221A (en) * 2012-09-20 2013-01-09 广东风华高新科技股份有限公司 Method, sintering aid and materials for preparation of low-temperature cofired medium ceramic and application
CN102875159A (en) * 2012-09-20 2013-01-16 广东风华高新科技股份有限公司 Method for preparing low-temperature cofired dielectric ceramic and material and sintering aid of low-temperature cofired dielectric ceramic
CN102976741A (en) * 2012-11-23 2013-03-20 天长市昭田磁电科技有限公司 Preparation method of manganese zinc MnZn soft magnetic ferrite material containing modified nanocarbon

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515779A (en) * 2011-12-07 2012-06-27 中国科学院过程工程研究所 Rare earth oxide composite additive for zinc oxide varistor and preparation method thereof
CN102863221A (en) * 2012-09-20 2013-01-09 广东风华高新科技股份有限公司 Method, sintering aid and materials for preparation of low-temperature cofired medium ceramic and application
CN102875159A (en) * 2012-09-20 2013-01-16 广东风华高新科技股份有限公司 Method for preparing low-temperature cofired dielectric ceramic and material and sintering aid of low-temperature cofired dielectric ceramic
CN102976741A (en) * 2012-11-23 2013-03-20 天长市昭田磁电科技有限公司 Preparation method of manganese zinc MnZn soft magnetic ferrite material containing modified nanocarbon

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104230350A (en) * 2014-09-18 2014-12-24 景德镇陶瓷学院 Preparation and usage method of additive for increasing Q value of microwave ceramic through microwave ceramic material wrapping

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