CN105060892A - Composite tantalate microwave dielectric ceramic with near-zero frequency temperature coefficient - Google Patents
Composite tantalate microwave dielectric ceramic with near-zero frequency temperature coefficient Download PDFInfo
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- CN105060892A CN105060892A CN201510579921.2A CN201510579921A CN105060892A CN 105060892 A CN105060892 A CN 105060892A CN 201510579921 A CN201510579921 A CN 201510579921A CN 105060892 A CN105060892 A CN 105060892A
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Abstract
The invention discloses a composite tantalate microwave dielectric ceramic with a near-zero frequency temperature coefficient. The chemical formula of the composite tantalate microwave dielectric ceramic with the near-zero frequency temperature coefficient is 0.38ZnZrTa2O8+0.62TiO2. The composite tantalate microwave dielectric ceramic with the near-zero frequency temperature coefficient is prepared by weighing and matching chemical ram materials ZnO, ZrO2, TiO2 and Ta2O5, performing ball milling, drying and screening, pre-sintering the mixture at 1,000 to 1,100 DEG C, and combining the pre-sintered mixture into a clinker; performing secondary ball milling, drying, screening and pressing to mould a blank; sintering the blank at 1,250 to 1,350 DEG C; preserving the temperature for 2 to 6 hours, thus preparing the composite tantalate microwave dielectric ceramic with the near-zero frequency temperature coefficient. The composite tantalate microwave dielectric ceramic with the near-zero frequency temperature coefficient is a microwave dielectric material with a middle-and-high dielectric constant (50 to 55); the quality factor is higher than 20,000 GHz; the process is simple and pollution-free; the composite tantalate microwave dielectric ceramic with the near-zero frequency temperature coefficient has a wide application prospect.
Description
Technical field
The invention belongs to a kind of take composition as the multiphase ceramic compound of feature, particularly a kind of temperature coefficient of resonance frequency (τ
f) nearly zero compound tantalate microwave media ceramic and preparation method thereof.
Background technology
Microwave-medium ceramics is the critical material manufacturing the microwave devices such as microwave dielectric filter, resonator, polyrod antenna and Medium Wave Guide.In recent years, due to the fast development of microwave technology, the microwave telecommunication systems such as satellite communication system, forth generation cellular mobile communication system, TV receiving system propose requirements at the higher level to the miniaturization of microwave circuit and microwave device, lightweight, integrated and high reliability, the researchdevelopment of microwave-medium ceramics is made great progress, and various type material emerges in an endless stream.
AZrB
2o
8(A=Zn, Mg; B=Nb, Ta) be wolframite type stupalith, the concern of various countries investigator is received with the microwave dielectric property of its excellence.More typical material system is as MgZrNb
2o
8(ε
r~ 26, Q × f ~ 120,800GHz, τ
f~-50 × 10
-6/ DEG C), ZnZrNb
2o
8(ε
r~ 30, Q × f ~ 61,000GHz, τ
f~-52 × 10
-6/ DEG C), ZnZrTa
2o
8(ε
r~ 31, Q × f ~ 110,800GHz, τ
f~-32 × 10
-6/ DEG C).This kind of microwave dielectric material has Medium dielectric constant and higher quality factor, but its temperature coefficient of resonance frequency is comparatively large, and temperature stability is poor, limits its through engineering approaches in microwave device and applies.Therefore, the present invention chooses the ZnZrTa with high dielectric constant
2o
8compound tantalate microwave media ceramic, by the appropriate TiO that adulterates
2powder, to adjust its temperature factor (making its frequency-temperature coefficient nearly zero), obtains the Novel microwave dielectric ceramic system that temperature stability is high.
Summary of the invention
Object of the present invention overcomes ZnZrTa
2o
8the shortcoming that compound tantalate microwave media ceramic temperature stability is bad, by adding a certain amount of TiO
2and obtain the NEW TYPE OF COMPOSITE tantalate microwave media ceramic that temperature coefficient of resonance frequency is nearly zero, specific inductivity is 50 ~ 55, quality factor are high, can be used for the manufacture of the microwave devices such as intermediary's low-loss microwave resonator, microwave-medium substrate, microwave antenna.
The present invention is achieved by following technical solution.
A compound tantalate microwave media ceramic for near-zero frequency temperature coefficient, chemical formula is 0.38ZnZrTa
2o
8+ 0.62TiO
2.
The compound tantalate microwave media ceramic of this near-zero frequency temperature coefficient adopts traditional simple solid reaction process synthesis, has following steps:
(1) by chemical feedstocks ZnO, ZrO
2, TiO
2, Ta
2o
5press 0.38ZnZrTa respectively
2o
8+ 0.62TiO
2stoichiometric ratio weigh batching;
(2) powder that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Again by the raw material stoving after ball milling, cross 40 mesh sieves, obtain evengranular powder;
(3) the powder pre-burning at 1000 ~ 1100 DEG C after step (2) being processed, is incubated 3 hours, synthesis frit;
(4) in the frit after step (3) preheating, additional mass percent is the polyvinyl alcohol of 1.05%, puts into ball grinder, adds zirconia ball and deionized water, ball milling 12 hours, cross 80 mesh sieves, then compression moulding is base substrate after drying;
(5) by the base substrate after shaping for step (4) in 1250 ~ 1350 DEG C of sintering, be incubated 2 ~ 6 hours, make the compound tantalate microwave media ceramic of frequency-temperature coefficient nearly zero.
Chemical feedstocks ZnO, ZrO of described step (1)
2, TiO
2and Ta
2o
5purity be greater than 99.9%.
The mass ratio of the ceramic powder of described step (2) or step (4) and zirconia ball, deionized water is 1: 1: 2.
Described step (2) or step (4) adopt planetary ball mill to carry out ball milling, and drum's speed of rotation is 400 revs/min.
The raw material of described step (2) or step (4) is dried in infrared drying oven, and bake out temperature is 100 DEG C.
The base substrate of described step (4) is the right cylinder of Φ 10mm × 5mm, adopts powder compressing machine compression moulding.
NEW TYPE OF COMPOSITE tantalate microwave media ceramic provided by the present invention belongs to the microwave dielectric material of Medium dielectric constant (50 ~ 55), and its temperature coefficient of resonance frequency is nearly zero, quality factor are higher than 20,000GHz is microwave dielectric ceramic materials more rare in the world at present.Therefore, compound tantalate microwave medium ceramic material of the present invention be the microwave device such as microwave dielectric resonator and wave filter manufacture and design the possibility that provides more choices, have very large using value at microwave telecommunication system.Its preparation technology is simple simultaneously, and process is pollution-free, has broad application prospects.
Embodiment
Below by specific embodiment, the invention will be further described, raw materials usedly in specific examples is commercially available analytical reagent (purity is greater than 99.9%), and concrete implementation step is as follows.
(1) by raw material ZnO, ZrO
2, TiO
2, Ta
2o
5difference 0.38: 0.38: 0.62: 0.38 weigh batching in molar ratio;
(2) put into ball grinder after being mixed by the powder of above-mentioned preparation, add zirconia ball and deionized water, ball milling 4 hours on planetary ball mill, the mass ratio of powder, zirconia ball and deionized water is 1: 1: 2; Raw material after ball milling is placed in infrared drying oven to dry at 100 DEG C, crosses 40 mesh sieves after drying, obtain evengranular powder;
(3) by the pre-burning at 1000 ~ 1100 DEG C of the above-mentioned powder mixed, 3 hours are incubated, synthesis frit;
(4) in the frit after pre-burning, additional mass percent is the polyvinyl alcohol of 1.05%, put into ball grinder, add zirconia ball and deionized water, the mass ratio of powder, zirconia ball and deionized water is 1: 1: 2, ball milling 12 hours, 100 DEG C of oven dry in infrared drying oven, cross 80 mesh sieves, then are pressed into the cylindrical green body of Φ 10mm × 5mm with powder compressing machine with the pressure of 150MPa;
(5) by above-mentioned shaping after base substrate in 1250 ~ 1350 DEG C of sintering, be incubated 2 ~ 6 hours, make the compound tantalate microwave media ceramic of frequency-temperature coefficient nearly zero;
(6) its microwave dielectric property is tested by Agilent8720ES network analyzer in conjunction with ESPECMC-710F mini type high temperature case;
Main technologic parameters and the microwave dielectric property thereof of specific embodiment refer to table 1.
Table 1
The present invention is not limited to above-described embodiment, and the change of some details is possible, but therefore this do not run counter to scope and spirit of the present invention.
Claims (6)
1. a compound tantalate microwave media ceramic for near-zero frequency temperature coefficient, chemical formula is 0.38ZnZrTa
2o
8+ 0.62TiO
2.
The compound tantalate microwave media ceramic of this near-zero frequency temperature coefficient adopts traditional simple solid reaction process synthesis, has following steps:
(1) by chemical feedstocks ZnO, ZrO
2, TiO
2, Ta
2o
5press 0.38ZnZrTa respectively
2o
8+ 0.62TiO
2stoichiometric ratio weigh batching;
(2) powder that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Again by the raw material stoving after ball milling, cross 40 mesh sieves, obtain evengranular powder;
(3) the powder pre-burning at 1000 ~ 1100 DEG C after step (2) being processed, is incubated 3 hours, synthesis frit;
(4) in the frit after step (3) preheating, additional mass percent is the polyvinyl alcohol of 1.05%, puts into ball grinder, adds zirconia ball and deionized water, ball milling 12 hours, cross 80 mesh sieves, then compression moulding is base substrate after drying;
(5) by the base substrate after shaping for step (4) in 1250 ~ 1350 DEG C of sintering, be incubated 2 ~ 6 hours, make the compound tantalate microwave media ceramic of frequency-temperature coefficient nearly zero.
2. the compound tantalate microwave media ceramic of a kind of near-zero frequency temperature coefficient according to claim 1, is characterized in that, chemical feedstocks ZnO, ZrO of described step (1)
2, TiO
2and Ta
2o
5purity be greater than 99.9%.
3. the compound tantalate microwave media ceramic of a kind of near-zero frequency temperature coefficient according to claim 1, it is characterized in that, the mass ratio of the ceramic powder of described step (2) or step (4) and zirconia ball, deionized water is 1: 1: 2.
4. the compound tantalate microwave media ceramic of a kind of near-zero frequency temperature coefficient according to claim 1, it is characterized in that, described step (2) or step (4) adopt planetary ball mill to carry out ball milling, and drum's speed of rotation is 400 revs/min.
5. the compound tantalate microwave media ceramic of a kind of near-zero frequency temperature coefficient according to claim 1, is characterized in that, the raw material of described step (2) or step (4) is dried in infrared drying oven, and bake out temperature is 100 DEG C.
6. the compound tantalate microwave media ceramic of a kind of near-zero frequency temperature coefficient according to claim 1, is characterized in that, the base substrate of described step (4) is the right cylinder of Φ 10mm × 5mm, adopts powder compressing machine compression moulding.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801104A (en) * | 2016-02-23 | 2016-07-27 | 天津大学 | High dielectric constant temperature stable type ceramic capacitor dielectric material |
| CN106904969A (en) * | 2017-02-28 | 2017-06-30 | 天津大学 | A kind of adjustable microwave dielectric ceramic with medium dielectric constant of temperature coefficient of resonance frequency |
| CN114213124A (en) * | 2021-12-14 | 2022-03-22 | 北京科技大学 | Microwave dielectric ceramic material with medium dielectric constant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864426A (en) * | 2014-01-21 | 2014-06-18 | 天津大学 | Medium-sintering temperature stable microwave dielectric ceramic material |
| CN104311024A (en) * | 2014-10-17 | 2015-01-28 | 中国矿业大学 | Microwave dielectric ceramic material with moderate dielectric constant and high quality factor and preparation method of microwave dielectric ceramic material |
-
2015
- 2015-09-11 CN CN201510579921.2A patent/CN105060892A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864426A (en) * | 2014-01-21 | 2014-06-18 | 天津大学 | Medium-sintering temperature stable microwave dielectric ceramic material |
| CN104311024A (en) * | 2014-10-17 | 2015-01-28 | 中国矿业大学 | Microwave dielectric ceramic material with moderate dielectric constant and high quality factor and preparation method of microwave dielectric ceramic material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801104A (en) * | 2016-02-23 | 2016-07-27 | 天津大学 | High dielectric constant temperature stable type ceramic capacitor dielectric material |
| CN105801104B (en) * | 2016-02-23 | 2018-11-27 | 天津大学 | A kind of high dielectric constant temperature-stable ceramic capacitor dielectric material |
| CN106904969A (en) * | 2017-02-28 | 2017-06-30 | 天津大学 | A kind of adjustable microwave dielectric ceramic with medium dielectric constant of temperature coefficient of resonance frequency |
| CN114213124A (en) * | 2021-12-14 | 2022-03-22 | 北京科技大学 | Microwave dielectric ceramic material with medium dielectric constant and preparation method thereof |
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Application publication date: 20151118 |