CN103553609B - High-quality factor microwave medium ceramic material, preparation method and microwave device - Google Patents
High-quality factor microwave medium ceramic material, preparation method and microwave device Download PDFInfo
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- CN103553609B CN103553609B CN201310527079.9A CN201310527079A CN103553609B CN 103553609 B CN103553609 B CN 103553609B CN 201310527079 A CN201310527079 A CN 201310527079A CN 103553609 B CN103553609 B CN 103553609B
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Abstract
The invention discloses a kind of high-quality factor microwave medium ceramic material, preparation method and microwave device, material comprises: (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, wherein B is the oxide compound of barium element and antimony element; The present invention adopts (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15oxide compound in conjunction with barium element and antimony element makes microwave dielectric ceramic materials, with existing Ba
5nb
4o
15deng ceramic phase ratio, effectively can improve the final quality factor of material, the needs making material can be applicable to microwave communication industry to expand to high frequency, and frequency resonance temperature factor τ
fcan regulate, and quality factor are still stablized after regulating, be beneficial to the design of device, meet the application demand of temperature match curing conditions, be applicable to field of microwave communication and develop to high frequency, be also applicable to alternating temperature Application Areas, and the raw material sources that the present invention relates to are extensive, affordable, technique is simple, and the industrialization being applicable to microwave-medium ceramics device is produced.
Description
Technical field
The present invention relates to the microwave-medium ceramics technical field of the microwave devices such as micro-wave communication dielectric resonator, vibrator, be specifically related to a kind of high-quality factor microwave medium ceramic material, preparation method and application.
Background technology
Microwave-medium ceramics is widely used in the microwave devices such as dielectric resonator, dielectric filter, duplexer, microwave-medium antenna, dielectric resonator oscillator, Medium Wave Guide transmission line.As the critical material in microwave communication, the properties of microwave-medium ceramics determines the performance of overall modern communication technology system to a great extent.
In prior art, Ba
5nb
4o
15the specific inductivity of microwave-medium ceramics is ε
r=39, quality factor q × f=23700GHz, temperature coefficient of resonance frequency τ
f=78ppm/ DEG C of (S.Kambaetc.HighfrequencydielectricpropertiesofA
5b
4o
15microwaveceramics, JournalofAppliedPhysics, 200189 (7) 3900-3906).In order to reduce Ba
5nb
4o
15the resonance temperature coefficient τ of microwave-medium ceramics
f, occurred that employing Ta replaces Nb and regulates Ba
5nb
4o
15resonance temperature coefficient τ
fmethod, but the method regulation range is limited, otherwise can affect quality factor.Chinese patent CN200710008980.X adopts Sb part to replace Nb reduction Ba
5nb
4o
15the resonance temperature coefficient τ of microwave-medium ceramics
fbut, as resonance temperature coefficient τ
fwhen nearly zero, quality factor q × f severe exacerbation.Chinese patent application 201210478550 discloses and adopts BaNb
2o
6resonance temperature coefficient τ
fregulate the scheme of nearly zero, but at lower resonance temperature coefficient τ
funder condition, quality factor q × f is still undesirable.But based on the importance of this material, the microwave-medium ceramics of exploitation high-quality is whole microwave communication field problem demanding prompt solution.
Therefore, need a kind of microwave dielectric ceramic materials, this material has higher quality factor, and frequency resonance temperature factor τ
fcan regulate, and after regulating, quality factor are still stablized, be applicable to field of microwave communication and develop to high frequency, be also applicable to alternating temperature Application Areas.
Summary of the invention
In view of this, the object of this invention is to provide a kind of high-quality factor microwave medium ceramic material, preparation method and microwave device, microwave dielectric ceramic materials has higher quality factor, and frequency resonance temperature factor τ
fcan regulate, and after regulating, quality factor are still stablized, be applicable to field of microwave communication and develop to high frequency, be also applicable to alternating temperature Application Areas.
High-quality factor microwave medium ceramic material of the present invention, comprising: (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, wherein B is the oxide compound of barium element and antimony element.
Further, in the oxide compound of described barium element and antimony element, BaO and Sb
2o
5mol ratio be: BaO:Sb
2o
5=0.85-1.15;
Further, in the oxide compound of described barium element and antimony element, BaO and Sb
2o
5mol ratio be: BaO:Sb
2o
5=0.9-1;
Further, 0.07≤x≤0.15;
Further, B is BaSb
2o
6, x=0.1
The invention also discloses a kind of preparation method of high-quality factor microwave medium ceramic material, comprise the following steps:
A. (Ba is prepared
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder:
B. prepare the ceramics powder of B, B is the oxide compound of barium element and antimony element, wherein BaO and Sb
2o
5mol ratio is: BaO:Sb
2o
5=0.85-1.15;
C. by (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, take (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder and B ceramic powder also form mixed powder;
Further, in step a, by (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15stoichiometric ratio take barium compound, strontium compound, niobium compound and antimony compounds and adopt wet ball-milling method mixing and ball milling, within 1 ~ 6 hour, obtain (Ba 900 DEG C ~ 1200 DEG C insulations after drying in an oven
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder;
In step b, take barium compound and antimony compounds by the stoichiometric ratio of B and add in ball grinder and adopt wet ball-milling method mixing and ball milling, after drying in an oven, within 1 ~ 6 hour, obtain B ceramic powder 900 DEG C ~ 1200 DEG C insulations.
Further, described barium compound is barium carbonate or nitrate of baryta, and strontium compound is Strontium carbonate powder or strontium nitrate, and niobium compound is Niobium Pentxoxide or nitric acid niobium, and antimony compounds is antimonous oxide or antimony peroxide.
The invention also discloses a kind of microwave device, make single-dielectric-layer structure by microwave dielectric ceramic materials; Or, the multilayered structure be made up of microwave dielectric ceramic materials and electrode materials.
The invention has the beneficial effects as follows: high-quality factor microwave medium ceramic material of the present invention, adopt (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15oxide compound in conjunction with barium element and antimony element makes microwave dielectric ceramic materials, with existing Ba
5nb
4o
15deng ceramic phase ratio, effectively can improve the final quality factor of material, the needs making material can be applicable to microwave communication industry to expand to high frequency, and frequency resonance temperature factor τ
fcan regulate, and quality factor are still stablized after regulating, be beneficial to the design of device, meet the application demand of temperature match curing conditions, be applicable to field of microwave communication and develop to high frequency, be also applicable to alternating temperature Application Areas, and the raw material sources that the present invention relates to are extensive, affordable, technique is simple, and the industrialization being applicable to microwave-medium ceramics device is produced.Embodiment
High-quality factor microwave medium ceramic material of the present invention, comprising: (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, wherein B is the oxide compound of barium element and antimony element.
In the present embodiment, in the oxide compound of described barium element and antimony element, BaO and Sb
2o
5mol ratio be: BaO:Sb
2o
5=0.85-1.15;
In the present embodiment, in the oxide compound of described barium element and antimony element, BaO and Sb
2o
5mol ratio be: BaO:Sb
2o
5=0.9-1.05;
In the present embodiment, 0.07≤x≤0.15;
In the present embodiment, B is BaSb
2o
6, x=0.1
The invention also discloses a kind of preparation method of high-quality factor microwave medium ceramic material, comprise the following steps:
A. (Ba is prepared
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder:
B. prepare the ceramics powder of B, B is the oxide compound of barium element and antimony element, wherein BaO and Sb
2o
5mol ratio is: BaO:Sb
2o
5=0.85-1.15;
C. by (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, take (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder and B ceramic powder also form mixed powder.
In the present embodiment, in step a, by (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15stoichiometric ratio take barium compound, strontium compound, niobium compound and antimony compounds and adopt wet ball-milling method mixing and ball milling, within 1 ~ 6 hour, obtain (Ba 900 DEG C ~ 1200 DEG C insulations after drying in an oven
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder;
In step b, take barium compound and antimony compounds by the stoichiometric ratio of B and add in ball grinder and adopt wet ball-milling method mixing and ball milling, after drying in an oven, within 1 ~ 6 hour, obtain B ceramic powder 900 DEG C ~ 1200 DEG C insulations.
In the present embodiment, described barium compound is barium carbonate or nitrate of baryta, and strontium compound is Strontium carbonate powder or strontium nitrate, and niobium compound is Niobium Pentxoxide or nitric acid niobium, and antimony compounds is antimonous oxide or antimony peroxide.
The invention also discloses a kind of microwave device, make single-dielectric-layer structure by microwave dielectric ceramic materials; Or, the multilayered structure be made up of microwave dielectric ceramic materials and electrode materials;
To add in ball grinder after ball milling 3h after microwave dielectric material of the present invention being added proper amount of acetone, ethanol in proper amount, appropriate triolein, appropriate PVB and appropriate DBP, after defoaming machine de-bubble, curtain coating, cutting, printed wiring, other device embedding, lamination, sintering obtain this microwave device, and this microwave device can be the devices such as microwave base plate, multi-layer capacitor, LC wave filter, temperature compensation wave filter.
Following table is specific embodiments of the invention, and parameter is that final microwave device detects gained:
Microwave dielectric ceramic materials in above-described embodiment adopts following three kinds of technological processs to obtain:
In above-described embodiment, embodiment two, four, six, eight raw material adopts nitrate of baryta, Niobium Pentxoxide, strontium nitrate, antimony peroxide to be raw material, and embodiment one, three, five, seven raw material adopts barium carbonate, Strontium carbonate powder, antimonous oxide, nitric acid niobium;
Preparation technology one
Comprise the following steps:
A. (Ba is prepared
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder:
By (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15stoichiometric ratio take barium compound, strontium compound, niobium compound and antimony compounds and adopt wet ball-milling method mixing and ball milling, within 6 hours, obtain (Ba 900 DEG C of insulations after drying in an oven
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder;
B. prepare the ceramics powder of B, B is the oxide compound of barium element and antimony element, wherein BaO and Sb
2o
5mol ratio presses above-described embodiment, and the oxide compound taking barium element and antimony element by the stoichiometric ratio of B adds in ball grinder and adopts wet ball-milling method mixing and ball milling, within 1 hour, obtains B ceramic powder after drying in an oven 1200 DEG C of insulations;
C. by (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, take (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder and B ceramic powder also form mixed powder.
Preparation technology two
Comprise the following steps:
A. (Ba is prepared
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder:
By (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15stoichiometric ratio take barium compound, strontium compound, niobium compound and antimony compounds and adopt wet ball-milling method mixing and ball milling, within 1 hour, obtain (Ba 1200 DEG C of insulations after drying in an oven
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder;
B. prepare the ceramics powder of B, B is the oxide compound of barium element and antimony element, wherein BaO and Sb
2o
5mol ratio presses above-described embodiment, and the oxide compound taking barium element and antimony element by the stoichiometric ratio of B adds in ball grinder and adopts wet ball-milling method mixing and ball milling, within 6 hours, obtains B ceramic powder after drying in an oven 900 DEG C of insulations;
C. by (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, take (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder and B ceramic powder also form mixed powder.
Preparation technology three
Comprise the following steps:
A. (Ba is prepared
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder:
By (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15stoichiometric ratio take barium compound, strontium compound, niobium compound and antimony compounds and adopt wet ball-milling method mixing and ball milling, within 3 hours, obtain (Ba 1000 DEG C of insulations after drying in an oven
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder; Adopt deionized water as ball-milling medium;
B. prepare the ceramics powder of B, B is the oxide compound of barium element and antimony element, wherein BaO and Sb
2o
5mol ratio presses above-described embodiment, and the oxide compound taking barium element and antimony element by the stoichiometric ratio of B adds in ball grinder and adopts wet ball-milling method mixing and ball milling, within 3 hours, obtains B ceramic powder after drying in an oven 1000 DEG C of insulations; Adopt ethanol as ball-milling medium.
C. by (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, take (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder and B ceramic powder also form mixed powder.
As can be seen from the above table:
Embodiment one shows (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15microwave property is excellent, and quality factor q × f can reach 45600GHz, but frequency resonance frequency-temperature coefficient is poor, is τ
f=51ppm/ DEG C, is not suitable for being applied in the environment of alternating temperature.
Embodiment two ~ eight shows that B pottery mixes the frequency resonance frequency-temperature coefficient that significantly can reduce material monolithic, when incorporation is 0.1mol, and the frequency resonance frequency-temperature coefficient of material nearly zero; Particularly when the barium element of B and oxide mol ratio corresponding to antimony element are m
baO: m
sb2O5=1, namely B is BaSb
2o
6time, over-all properties is optimum, DIELECTRIC CONSTANT ε
r=37.5, quality factor q × f can reach 39200GHz, simultaneously temperature coefficient of resonance frequency τ
f=1ppm/ DEG C.
According to the parameter comparison of above-described embodiment, it is high that microwave dielectric material of the present invention has quality factor, the advantage that temperature coefficient of resonance frequency is adjustable.Embodiment 5,6 and 8 all obtains good microwave dielectric material, and particularly embodiment 8 over-all properties is best, quality factor q × f=39200GHz, temperature coefficient of resonance frequency τ
fnearly zero, other embodiments show slightly not enough compared with embodiment 8, but still meet implementing process of the present invention and requirement.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (7)
1. a high-quality factor microwave medium ceramic material, is characterized in that: comprising: (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein 0.07≤x≤0.15, wherein B is the oxide compound of barium element and antimony element; In the oxide compound of described barium element and antimony element, BaO and Sb
2o
5mol ratio be: BaO:Sb
2o
5=0.85-1.15.
2. high-quality factor microwave medium ceramic material according to claim 1, is characterized in that: in the oxide compound of described barium element and antimony element, BaO and Sb
2o
5mol ratio be: BaO:Sb
2o
5=0.9-1.05.
3. high-quality factor microwave medium ceramic material according to claim 2, is characterized in that: B is BaSb
2o
6, x=0.1.
4. a preparation method for high-quality factor microwave medium ceramic material, is characterized in that: comprise the following steps:
A. (Ba is prepared
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder:
B. prepare the ceramics powder of B, B is the oxide compound of barium element and antimony element, wherein BaO and Sb
2o
5mol ratio is: BaO:Sb
2o
5=0.85-1.15;
C. by (1-x) (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15-xB, wherein x≤0.3, take (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder and B ceramic powder also form mixed powder.
5. the preparation method of high-quality factor microwave medium ceramic material according to claim 4, is characterized in that: in step a, by (Ba
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15stoichiometric ratio take barium compound, strontium compound, niobium compound and antimony compounds and adopt wet ball-milling method mixing and ball milling, within 1 ~ 6 hour, obtain (Ba 900 DEG C ~ 1200 DEG C insulations after drying in an oven
0.98sr
0.02)
5(Nb
0.95sb
0.05)
4o
15ceramic powder;
In step b, take barium compound and antimony compounds by the stoichiometric ratio of B and add in ball grinder and adopt wet ball-milling method mixing and ball milling, after drying in an oven, within 1 ~ 6 hour, obtain B ceramic powder 900 DEG C ~ 1200 DEG C insulations.
6. the preparation method of high-quality factor microwave medium ceramic material according to claim 5, it is characterized in that: described barium compound is barium carbonate or nitrate of baryta, strontium compound is Strontium carbonate powder or strontium nitrate, niobium compound is Niobium Pentxoxide or nitric acid niobium, and antimony compounds is antimonous oxide or antimony peroxide.
7. a microwave device, is characterized in that: make single-dielectric-layer structure by the microwave dielectric ceramic materials described in the arbitrary claim of claims 1 to 3; Or, the multilayered structure be made up of the microwave dielectric ceramic materials described in the arbitrary claim of claims 1 to 3 and electrode materials.
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CN201310527079.9A CN103553609B (en) | 2013-10-30 | 2013-10-30 | High-quality factor microwave medium ceramic material, preparation method and microwave device |
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CN103553609A CN103553609A (en) | 2014-02-05 |
CN103553609B true CN103553609B (en) | 2015-12-02 |
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JP6249004B2 (en) * | 2015-10-06 | 2017-12-20 | Tdk株式会社 | Dielectric composition and electronic component |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102503374A (en) * | 2011-09-30 | 2012-06-20 | 桂林理工大学 | Microwave dielectric ceramic Ba(4-x)SrxLiSb3O12 capable of being sintered at low temperature and preparation method thereof |
CN102976751A (en) * | 2012-11-22 | 2013-03-20 | 云南云天化股份有限公司 | Low-temperature sintering microwave dielectric ceramic material and preparation method thereof |
-
2013
- 2013-10-30 CN CN201310527079.9A patent/CN103553609B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102503374A (en) * | 2011-09-30 | 2012-06-20 | 桂林理工大学 | Microwave dielectric ceramic Ba(4-x)SrxLiSb3O12 capable of being sintered at low temperature and preparation method thereof |
CN102976751A (en) * | 2012-11-22 | 2013-03-20 | 云南云天化股份有限公司 | Low-temperature sintering microwave dielectric ceramic material and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
"Ba5(Nb1–xSbx)4O15 微波介电陶瓷的低温烧结";张冲 等;《电子元件与材料》;20070831;第26卷(第8期);第55-58页 * |
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Effective date of registration: 20161019 Address after: 401220 Changshou District of Chongqing economic and Technological Development Zone United Road No. 22 Patentee after: Chongqing Yuntianhua hanen New Material Development Co Ltd Patentee after: Yutianhua Co., Ltd., Yunnan Address before: 650228 Dianchi Road, Yunnan, China, No. 1417, No. Patentee before: Yutianhua Co., Ltd., Yunnan |