CN103553610B - Low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device - Google Patents
Low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device Download PDFInfo
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Abstract
The invention discloses a low-temperature sintered microwave dielectric ceramic material, a preparation method and a microwave device. The material comprises (Ba (1-a)Sra)5 (Nb (1-b) Sbb) 4O15 and zinc borosilicate glass, wherein a is not larger than 0.05 and b is not larger than 0.1. The material disclosed by the invention overcomes the problem in the prior art that a copper element is introduced to increase the dielectric loss, the material is insoluble in such solvents as water, ethanol and the like, generates no gelation reaction with such adhesives as PVA (Polyvinyl Alcohol), PVB (Polyvinyl Butyral) and the like and meets the LTCC (Low Temperature Co-Fired Ceramic) process requirements, and the material disclosed by the invention is high in quality factor, adjustable in frequency resonance temperature coefficient, capable of being prepared to a microwave device with a multilayer or single-layer dielectric layer structure and is more suitable for application in the field of high-frequency and high-temperature microwave communication; the related raw materials are wide in source, low in cost, simple in process, low in production cost and suitable for industrial production of microwave dielectric ceramic devices; and the microwave dielectric material is low in dielectric loss, high in quality factor, adjustable in frequency resonance temperature coefficient and capable of meeting the requirements of the application field of high frequency, variable temperature and high reliability.
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 low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device.
Background technology
Along with modern communication technology is to the active demand of the components and parts of miniaturization, integrated, modularization and low cost, LTCC (LowTemperature Co-fired Ceramics, the LTCC) technology with excellent electricity, machinery, thermal characteristics and high reliability has become the general choice technology of communication components and parts manufacture.The maximum feature of LTCC technology is to adopt metal (as Ag) as multilayer wiring conductor material, improves signal transmission rate and reliability, and multiple microwave electron components and parts can be embedded in sintering in substrate and improve packing density at double.The components and parts adopting this technology to prepare have that dielectric loss is low, reliability is high, low cost and other advantages, have a wide range of applications.
Because the fusing point of metal A g electrode is at 960 DEG C, in order to realize with ceramic co-fired, LTCC technology requires that the sintering temperature of pottery is lower than 900 DEG C.Current great majority have the microwave-medium ceramics sintering temperature of excellent properties higher than 1200 DEG C, have the Ba of excellent microwave dielectric property
5nb
4o
15pottery is also like this.It is reported, 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, but sintering temperature is higher than 1380 DEG C of (S.Kamba etc.Highfrequency dielectric properties of A
5b
4o
15microwave ceramics, Journal of AppliedPhysics, 200189 (7) 3900-3906).Low temperature co-fired in order to what realize with Ag electrode, the people such as Kin.J.R are at " Journal of the American Society " 85 volumes " Microwave Dielectric Propertiesof Low-Fired Ba in 2002
5nb
4o
15" one the article pointed out and add low melting point oxide B at pottery
2o
3sintering temperature can be down to 900 DEG C, quality factor q × f=18700GHz, temperature coefficient of resonance frequency also can be made close to zero simultaneously.But adopt such scheme to prepare LTCC and still there is more deficiency, be in particular in B
2o
3soluble in water, ethanol equal solvent, and with the binding agent generation gelling reactions such as the most frequently used PVA, PVB, make ceramic powder can not obtain highdensity ceramic diaphragm after curtain coating.Chinese patent application 201210478550 discloses and adopts CuO and B
2o
3pre-fired mixture reduces sintering temperature, achieves good result, but due to the existence of copper in this material, loss is increased, and quality factor reduce.
Therefore, need a kind of low-temperature sintered microwave dielectric ceramic material, not containing copper, and can improve with Ba further
5nb
4o
15the microwave material dielectric properties of ceramic main, water insoluble, the ethanol equal solvent of this material simultaneously, and not with the binding agent generation gelling reactions such as PVA, PVB, meet LTCC processing requirement, highdensity ceramic diaphragm can be obtained, and wide material sources, cost is low, and the industrialization being applicable to microwave-medium ceramics device is produced.
Summary of the invention
In view of this, the object of the invention is to provide a kind of low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device, not containing copper, and can improve with Ba further
5nb
4o
15the microwave material dielectric properties of ceramic main, water insoluble, the ethanol equal solvent of this material simultaneously, and not with the binding agent generation gelling reactions such as PVA, PVB, meet LTCC processing requirement, highdensity ceramic diaphragm can be obtained, and wide material sources, cost is low, and the industrialization being applicable to microwave-medium ceramics device is produced.
Low-temperature sintered microwave dielectric ceramic material disclosed by the invention, comprises (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15with zinc boron glass, wherein a≤0.05, b≤0.1.
Further, also BaNb is comprised
2o
6;
Further,
This stupalith is ywt% [(1-x) (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15-xBaNb
2o
6]+zwt% zinc boron glass, wherein x≤0.3,0<z≤20, y+z=100.
Further, in described zinc boron glass, the molar percentage of zinc is 25% ~ 50%;
Further, x=0.05 ~ 0.3;
Further, x=0.05 ~ 0.2.
The invention also discloses a kind of preparation method of low-temperature sintered microwave dielectric ceramic material, comprise the following steps:
A. (Ba is prepared
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
B. BaNb is prepared
2o
6ceramic powder;
C. zinc boron glass powder is prepared;
D. (Ba is taken
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, BaNb
2o
6ceramic powder and zinc boron glass also form mixed powder.
Further, in step a, by (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, to add in ball grinder containing niobium compound, antimony containing 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
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
In step b, by BaNb
2o
6stoichiometric ratio take containing barium compound, add in ball grinder containing niobium compound and adopt wet ball-milling method mixing and ball milling, within 1 ~ 6 hour, obtain BaNb 900 DEG C ~ 1200 DEG C insulations after drying in an oven
2o
6ceramic powder;
In step c, be 25% ~ 50% take zinc compound and boron-containing compound by the molar percentage of zinc in zinc boron glass, the raw material taken is added in ball grinder and adopts wet ball-milling method mixing and ball milling, be melt into liquid glass at 1100 DEG C ~ 1500 DEG C after drying in an oven, and obtain low melting glass powder through shrend and pulverizing;
Further, described containing barium compound is barium carbonate or nitrate of baryta, be Strontium carbonate powder or strontium nitrate containing strontium compound, be Niobium Pentxoxide or nitric acid niobium containing niobium compound, antimony containing compounds is antimonous oxide or antimony peroxide, zinc compound is zinc oxide or zinc acetate, and boron-containing compound is boron-containing compound is boric acid or boron liver.
The invention also discloses a kind of microwave device, the multilayer be made up of described low-temperature sintered microwave dielectric ceramic material or single-layer medium Rotating fields.
The invention has the beneficial effects as follows: adopt the divalent strontium element of minor radius and the collaborative doping of 5 valency antimony elements to improve Ba
5nb
4o
15pottery prime factor, the zinc boron low melting glass cooling-down effect simultaneously adopted is obvious, overcome copper of the prior art and introduce increase dielectric loss, and this material is water insoluble, ethanol equal solvent, and not with the binding agent generation gelling reactions such as PVA, PVB, meet LTCC processing requirement, and quality factor of the present invention are high, frequency resonance temperature coefficient adjustable, can make the microwave device of multilayer or single-layer medium Rotating fields, is more suitable for the field of microwave communication application of high frequency and alternating temperature; The raw material sources related to are extensive, affordable, and technique is simple, has lower production cost, and the industrialization being applicable to microwave-medium ceramics device is produced; The dielectric loss of microwave dielectric material is low, quality factor are high, and temperature coefficient of resonance frequency is adjustable, meets the highly reliable Application Areas requirement of high frequency, alternating temperature.
Embodiment
Low-temperature sintered microwave dielectric ceramic material disclosed by the invention, comprises (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15with zinc boron glass, wherein a≤0.05, b≤0.1; Zinc boron low melting glass can significantly reduce (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15the sintering temperature of pottery, makes pottery to burn altogether with Ag electrode at low temperatures, and can not too much reduce dielectric material performance.
In the present embodiment, also comprise BaNb
2o
6; Adopt BaNb
2o
6the characteristic of negative frequency-temperature coefficient, the frequency resonance temperature factor of regulation system, improves the temperature reliability of device, makes device be applicable to alternating temperature application scenario.
In the present embodiment,
This stupalith is ywt% [(1-x) (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15-xBaNb
2o
6]+zwt% zinc boron glass, wherein x≤0.3,0<z≤20, y+z=100.
Further, in described zinc boron glass, the molar percentage of zinc is 25% ~ 50%;
Further, x=0.05 ~ 0.3;
Further, x=0.05 ~ 0.2.
The invention also discloses a kind of preparation method of low-temperature sintered microwave dielectric ceramic material, comprise the following steps:
A. (Ba is prepared
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
B. BaNb is prepared
2o
6ceramic powder;
C. zinc boron glass powder is prepared;
D. (Ba is taken
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, BaNb
2o
6ceramic powder and zinc boron glass also form mixed powder.
Further, in step a, by (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, to add in ball grinder containing niobium compound, antimony containing 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
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
In step b, by BaNb
2o
6stoichiometric ratio take containing barium compound, add in ball grinder containing niobium compound and adopt wet ball-milling method mixing and ball milling, within 1 ~ 6 hour, obtain BaNb 900 DEG C ~ 1200 DEG C insulations after drying in an oven
2o
6ceramic powder;
In step c, be 25% ~ 50% take zinc compound and boron-containing compound by the molar percentage of zinc in zinc boron glass, the raw material taken is added in ball grinder and adopts wet ball-milling method mixing and ball milling, be melt into liquid glass at 1100 DEG C ~ 1500 DEG C after drying in an oven, and obtain low melting glass powder through shrend and pulverizing;
In the present embodiment, described containing barium compound is barium carbonate or nitrate of baryta, be Strontium carbonate powder or strontium nitrate containing strontium compound, be Niobium Pentxoxide or nitric acid niobium containing niobium compound, antimony containing compounds is antimonous oxide or antimony peroxide, zinc compound is zinc oxide or zinc acetate, and boron-containing compound is boron-containing compound is boric acid or boron liver.
The invention also discloses a kind of multilayer or single-layer medium Rotating fields microwave device; The microwave dielectric material obtained through steps d to add in ball grinder after ball milling 3h after adding 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, 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, ten, 11,12,14 raw material adopts nitrate of baryta, Niobium Pentxoxide, zinc acetate, boric acid, strontium nitrate, antimony peroxide, and embodiment one, three, five, seven, nine, 11,13 raw material adopts barium carbonate, nitric acid niobium, zinc oxide, boron liver, Strontium carbonate powder and antimonous oxide; Above-mentioned raw materials is applicable to prepare (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, preparation BaNb
2o
6ceramic powder and prepare zinc boron glass powder; Do not repeat them here
Preparation technology one
Comprise the following steps:
A. (Ba is prepared
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder: by (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, to add in ball grinder containing niobium compound, antimony containing compounds and adopt deionized water as ball-milling medium mixing and ball milling 20 hours, ceramic powder is obtained in retort furnace pre-burning after drying in an oven, calcined temperature value 900 DEG C ~ 1200 DEG C, is incubated and obtains (Ba in 1 ~ 6 hour
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, according to the height of calcined temperature, suitably adjusts soaking time, for the finished product quality and have no significant effect;
B. BaNb is prepared
2o
6ceramic powder: by BaNb
2o
6stoichiometric ratio take containing barium compound, add in ball grinder containing niobium compound and adopt ethanol as ball-milling medium mixing and ball milling 12 hours, ceramic powder is obtained in retort furnace pre-burning after drying in an oven, calcined temperature value 900 DEG C ~ 1200 DEG C, soaking time value 1-6 hour obtains BaNb
2o
6ceramic powder; According to the height of calcined temperature, suitably adjust soaking time, for the finished product quality and have no significant effect;
C. zinc boron glass powder is prepared: be 25% ~ 50% take zinc compound and boron-containing compound by the molar percentage of zinc in zinc boron glass, the raw material taken is added in ball grinder and adopts n-propyl alcohol as ball-milling medium mixing and ball milling 20 hours, be melt into liquid glass at 1100 DEG C ~ 1500 DEG C after drying in an oven, and obtain low melting glass powder through shrend and pulverizing;
D. take ceramic powder and low melting glass by x value and z value and form mixed powder, then add massfraction be 25% acetone, 17% ethanol, 1% triolein, add in ball grinder after ball milling 3h after 1%PVB and 1%DBP, after defoaming machine de-bubble, obtain microwave device after curtain coating, cutting, print copper circuit, lamination, sintering.
As can be seen from the above table:
Embodiment one to embodiment five (embodiment one is the comparative example of not modification) shows the positive divalent strontium element and the positive 5 valency antimony elements collaborative doping Ba that adopt minor radius
5nb
4o
15, effectively can regulate the microwave dielectric property of material.Particularly the microwave property of the material of embodiment 3 is better, DIELECTRIC CONSTANT ε
r=37.1, quality factor q × f can reach 42600GHz, simultaneously temperature coefficient of resonance frequency τ
f=51ppm/ DEG C.
Embodiment six to embodiment eight shows BaNb
2o
6pottery significantly can regulate the temperature coefficient of resonance frequency of material, makes material be applicable to the occasion of temperature variation.Particularly work as BaNb
2o
6when ceramic content is 0.1mol, i.e. embodiment 7, temperature coefficient of resonance frequency τ
f=3ppm/ DEG C.
Embodiment nine to embodiment 14 shows that zinc boron glass has good temperature reduction performance, adds a small amount of zinc boron glass and not only makes material can burn altogether with Ag electrode at 900 DEG C, nor significantly can worsen material property.The temperature coefficient of resonance frequency τ of material
fby just becoming negative.Particularly embodiment 11 obtains material system and the preparation technology of excellent combination property.
Embodiment 14 obtains over-all properties low temperature co-fired microwave dielectric material the most excellent.Namely when a=0.02, b=0.05, x=0.1, z=5wt%, DIELECTRIC CONSTANT ε
r=35.5, quality factor q × f can reach 33600GHz, simultaneously temperature coefficient of resonance frequency τ
f=1ppm/ DEG C.
According to the parameter comparison of above-described embodiment, it is moderate that microwave dielectric material of the present invention has specific inductivity, and quality factor are high, the advantage that temperature coefficient of resonance frequency is adjustable.Embodiment three, seven and nine to ten four all obtains good microwave dielectric material, and particularly embodiment 14 over-all properties is best, quality factor q × f>30000GHz, temperature coefficient of resonance frequency τ
fnearly zero, other embodiments show slightly not enough compared with embodiment 14, 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 (2)
1. a preparation method for low-temperature sintered microwave dielectric ceramic material, is characterized in that: this stupalith is ywt% [(1-x) (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15-xBaNb
2o
6]+zwt% zinc boron glass, wherein 0.02≤a≤0.05,0.05≤b≤0.1, x≤0.3,0<z≤20, y+z=100; The preparation method of this stupalith comprises the following steps:
A. (Ba is prepared
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder; By (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, to add in ball grinder containing niobium compound, antimony containing 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
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
B. BaNb is prepared
2o
6ceramic powder; By BaNb
2o
6stoichiometric ratio take containing barium compound, add in ball grinder containing niobium compound and adopt wet ball-milling method mixing and ball milling, within 1 ~ 6 hour, obtain BaNb 900 DEG C ~ 1200 DEG C insulations after drying in an oven
2o
6ceramic powder;
C. zinc boron glass powder is prepared; Be 25% ~ 50% take zinc compound and boron-containing compound by the molar percentage of zinc in zinc boron glass, the raw material taken is added in ball grinder and adopts wet ball-milling method mixing and ball milling, be melt into liquid glass at 1100 DEG C ~ 1500 DEG C after drying in an oven, and obtain low melting glass powder through shrend and pulverizing;
D. (Ba is taken
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, BaNb
2o
6ceramic powder and zinc boron glass also form mixed powder.
2. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 1, is characterized in that: in described zinc boron glass, the molar percentage of zinc is 25% ~ 50%.
3. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 2, is characterized in that: x=0.05 ~ 0.3.
4. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 3, is characterized in that: x=0.05 ~ 0.2.
5. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 4, it is characterized in that: described containing barium compound is barium carbonate or nitrate of baryta, be Strontium carbonate powder or strontium nitrate containing strontium compound, be Niobium Pentxoxide or nitric acid niobium containing niobium compound, antimony containing compounds is antimonous oxide or antimony peroxide, zinc compound is zinc oxide or zinc acetate, and boron-containing compound is boric acid or boric anhydride.
6. a microwave device, is characterized in that: the multilayer that the low-temperature sintered microwave dielectric ceramic material prepared by the preparation method of the low-temperature sintered microwave dielectric ceramic material described in the arbitrary claim of claim 1-5 is made or single-layer medium Rotating fields.
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| CN107244916B (en) * | 2017-05-19 | 2020-05-12 | 电子科技大学 | Niobate-series low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN110171972B (en) * | 2019-01-04 | 2021-10-22 | 南京汇聚新材料科技有限公司 | Low-temperature sintered ceramic material |
| TWI728509B (en) * | 2019-10-16 | 2021-05-21 | 道登電子材料股份有限公司 | Low temperature co-fired ceramic paste and method for preparing high-frequency microwave dielectric unit therefrom |
| CN112010649A (en) * | 2020-09-08 | 2020-12-01 | 中物院成都科学技术发展中心 | Low-cost ceramic substrate large-scale preparation method for filter |
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| CN100534949C (en) * | 2007-11-16 | 2009-09-02 | 北京交通大学 | Yttrium niobate solid-phase reaction synthetic sintering method capable of being used for microwave dielectric ceramic |
| CN102976751B (en) * | 2012-11-22 | 2015-01-14 | 云南云天化股份有限公司 | Low-temperature sintering microwave dielectric ceramic material and preparation method thereof |
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Effective date of registration: 20170119 Address after: The 401220 Chongqing economic and Technological Zone Changshou District Qixin 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 |