CN104961459A - Temperature-stable type magnesium titanate base microwave dielectric ceramic - Google Patents
Temperature-stable type magnesium titanate base microwave dielectric ceramic Download PDFInfo
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- CN104961459A CN104961459A CN201510363642.2A CN201510363642A CN104961459A CN 104961459 A CN104961459 A CN 104961459A CN 201510363642 A CN201510363642 A CN 201510363642A CN 104961459 A CN104961459 A CN 104961459A
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- ball milling
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Abstract
The invention discloses temperature-stable type magnesium titanate base microwave dielectric ceramic. The target composition expression of the temperature-stable type magnesium titanate base microwave dielectric ceramic is 0.9MgTiO3-0.1(K0.5La0.5)TiO3. Firstly, MgO and TiO2 are mixed according to the stoichiometry equation MgTiO3, and presintering is carried out at 800-1000 DEG C after ball milling, drying and screening are carried out; secondly,La2O3, K2CO3 and TiO2 are mixed according to the stoichiometry equation(K0.5La0.5)TiO3, and presintering is carried out at 1000-1200 DEG C after ball milling, drying and screening are carried out; thirdly, the two kinds of powder obtained after presintering are mixed according to the mole ratio of 9:1 and pressed into a green body after ball milling, drying, screening and pelleting are carried out; fourthly, the green body is sintered at 1250 DEG C-1350 DEG C, and the temperature-stable type magnesium titanate base microwave dielectric ceramic is prepared. The QF value of the temperature-stable type magnesium titanate base microwave dielectric ceramic reaches 31,000-68,000 GHz, and the temperature coefficient (tao f) of resonance frequency reaches -7.9--0.7*10<-6>/DEG C. The ceramic system is simple in preparing technology and superior in microwave dielectric performance, has saved energy cost, conforms to the low-carbon environment-friendly concept and has wide application prospects.
Description
Technical field
The invention relates to composition is the ceramic composition of feature, particularly a kind of New temperature stable form magnesium titanate base microwave medium ceramics material.
Background technology
The development of modern communication technology, day by day urgent to the miniaturization of components and parts, integrated and modular requirement, have higher requirement to microwave dielectric material, microwave-medium ceramics has become one of most active research field of function ceramics in recent years.Wherein, magnesium titanate (MgTiO
3) ceramic as a kind of traditional microwave dielectric material, in millimere-wave band, still there is the excellent microwave dielectric property such as low-k, ultra high quality factor, but there is temperature stability difference (τ
f~-50ppm/ DEG C), the shortcoming of sintering temperature high (> 1400 DEG C).
Because microwave device needs to work at different temperature, and the stability of its carrier signal function at different temperatures will be ensured, just necessarily require the resonant frequency of microwave dielectric material not vary with temperature, or change is less.Therefore, the temperature coefficient of resonance frequency of nearly zero just becomes the major criterion weighing material property.Therefore, microwave dielectric material especially MgTiO
3the research of base microwave medium ceramic material temperature stability has become a large focus.Meanwhile, MgTiO
3pottery has high sintering temperature, and preparation process energy consumption is large, does not meet the theory of low-carbon environment-friendly.Therefore, a kind of MgTiO with temperature stability and low-loss feature is studied
3base microwave medium ceramic material to reduce the needs of its sintering temperature day by day urgent.
Summary of the invention
Object of the present invention, is the temperature stability difference (τ overcoming prior art
f~-50ppm/ DEG C), the shortcoming of sintering temperature high (> 1400 DEG C), there is provided a kind of and there is excellent microwave dielectric property, especially make temperature coefficient of resonance frequency nearly zero, the novel magnesium titanate base temperature-stable microwave-medium ceramics and preparation method thereof in high performance microwave device application can be met.
The present invention is achieved by the scheme of following technology:
A kind of temperature-stable magnesium titanate base microwave medium ceramics, target synthetics expression formula is 0.9MgTiO
3-0.1 (K
0.5la
0.5) TiO
3;
The preparation method of this temperature-stable magnesium titanate base microwave medium ceramics, has following steps:
(1) by chemical feedstocks MgO, TiO
2stoichiometrically formula MgTiO
3prepare burden, put into polyester pellet grinding jar, after adding deionized water and zirconium ball, ball milling 8-16 hour;
(2) raw material after step (1) ball milling is put into infrared drying oven in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(3) moderate oven put into by the powder after step (2) being sieved, and in 800 ~ 1000 DEG C of pre-burnings, is incubated 2 ~ 8 hours;
(4) by La
2o
3, K
2cO
3and TiO
2stoichiometrically formula (K
0.5la
0.5) TiO
3prepare burden, put into polyester pellet grinding jar, after adding deionized water and zirconium ball, ball milling 8 ~ 16 hours;
(5) raw material after step (4) ball milling is put into infrared drying oven, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(6) moderate oven put into by the powder after step (5) being sieved, and in 1000 ~ 1200 DEG C of pre-burnings, is incubated 2 ~ 8 hours;
(7) powder that step (3) and (6) obtain is prepared burden according to the ratio that mol ratio is 9:1, put into polyester pellet grinding jar, after adding deionized water and zirconium ball, ball milling 8 ~ 16 hours;
(8) raw material after step (7) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(9) paraffin being 8% ~ 10% using the additional mass percent of powder after step (8) is sieved carries out granulation as tackiness agent, crosses 80 mesh sieves, makes green compact with powder compressing machine with the pressure of 4 ~ 8MPa;
(10) by the green compact of step (8) in 1250 DEG C-1350 DEG C sintering, be incubated 2 ~ 8 hours, make the ceramics as low-loss microwave medium of magnesium titanate base temperature-stable.
Described step (1), (4) or (7) adopt planetary ball mill to carry out ball milling, and drum's speed of rotation is 400 revs/min.
The green compact diameter of described step (9) is 10mm, and thickness is 5mm.
The preferred sintering temperature of described step (10) is 1300 DEG C.
The present invention is with MgO, TiO
2, La
2o
3, K
2cO
3for the ceramics as low-loss microwave medium 0.9MgTiO of magnesium titanate base temperature-stable prepared by raw material
3-0.1 (K
0.5la
0.5) TiO
3, its sintering temperature is 1250 ~ 1350 DEG C.Under microwave frequency band, record Qf value reach 31000 ~ 68000GHz, temperature coefficient of resonance frequency (τ
f) reach-7.9 ~-0.7 × 10
-6/ DEG C.This ceramic systems preparation technology is simple, and microwave dielectric property is superior, reduces MgTiO
3the sintering temperature of system, has saved energy cost, meets the theory of low-carbon environment-friendly, is with a wide range of applications.
Embodiment
The present invention is greater than MgO, TiO of 99% with purity
2and the La that purity is greater than 99.5%
2o
3, K
2cO
3for initial feed, prepare microwave-medium ceramics by simple solid phase method.Specific embodiments is as follows:
(1) by MgO, TiO
2stoichiometrically formula MgTiO
3prepare burden, proportioning raw materials is: 3.35302g MgO, 6.64698g TiO
2.The mixed powder of 10g is put into polyester pellet grinding jar, adds 200ml deionized water, add the zirconium ball of 150g, ball milling 12 hours on planetary ball mill, rotating speed is 400 revs/min;
(2) raw material after step (1) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(3) moderate oven put into by the powder after step (2) being sieved, and in 900 DEG C of pre-burnings, is incubated 4 hours;
(4) by La
2o
3, K
2cO
3, TiO
2stoichiometrically formula (K
0.5la
0.5) TiO
3prepare burden, proportioning raw materials is: 1.32156g La
2o
3, 0.56060g K
2cO
3, 1.29636g TiO
2the mixed powder of about 3g is put into polyester pellet grinding jar, adds the zirconium ball of 200ml deionized water and 150g, ball milling 12 hours;
(5) raw material after step (4) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(6) moderate oven put into by the powder after step (5) being sieved, and in 1100 DEG C of pre-burnings, is incubated 4 hours;
(7) powder step (3) and (6) obtained is ratio batching 8g, i.e. 6.83227g93MCT, the 1.16773g (K of 9:1 respectively according to mol ratio
0.5la
0.5) TiO
3, put into polyester pellet grinding jar, add the zirconium ball of 200ml deionized water and 150g, ball milling 12 hours;
(8) raw material after step (7) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(9) paraffin being 8% using the additional mass percent of powder after step (8) is sieved carries out granulation as tackiness agent, crosses 80 mesh sieves, makes green compact with powder compressing machine with the pressure of 4MPa;
(10) by the green compact of step (8) in 1250 ~ 1350 DEG C of sintering, be incubated 6 hours, make low-loss microwave-medium ceramics of temperature-stable.
(11) by the microwave dielectric property of network analyzer test resulting product.
Related process parameters and the microwave dielectric property thereof of specific embodiment refer to table 1.
Table 1
Claims (4)
1. a temperature-stable magnesium titanate base microwave medium ceramics, target synthetics expression formula 0.9MgTiO
3-0.1 (K
0.5la
0.5) TiO
3;
The preparation method of this temperature-stable magnesium titanate base microwave medium ceramics, has following steps:
(1) by chemical feedstocks MgO, TiO
2stoichiometrically formula MgTiO
3prepare burden, put into polyester pellet grinding jar, after adding deionized water and zirconium ball, ball milling 8-16 hour;
(2) raw material after step (1) ball milling is put into infrared drying oven in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(3) moderate oven put into by the powder after step (2) being sieved, and in 800 ~ 1000 DEG C of pre-burnings, is incubated 2 ~ 8 hours;
(4) by La
2o
3, K
2cO
3and TiO
2stoichiometrically formula (K
0.5la
0.5) TiO
3prepare burden, put into polyester pellet grinding jar, after adding deionized water and zirconium ball, ball milling 8 ~ 16 hours;
(5) raw material after step (4) ball milling is put into infrared drying oven, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(6) moderate oven put into by the powder after step (5) being sieved, and in 1000 ~ 1200 DEG C of pre-burnings, is incubated 2 ~ 8 hours;
(7) powder that step (3) and (6) obtain is prepared burden according to the ratio that mol ratio is 9:1, put into polyester pellet grinding jar, after adding deionized water and zirconium ball, ball milling 8 ~ 16 hours;
(8) raw material after step (7) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(9) paraffin being 8% ~ 10% using the additional mass percent of powder after step (8) is sieved carries out granulation as tackiness agent, crosses 80 mesh sieves, makes green compact with powder compressing machine with the pressure of 4 ~ 8MPa;
(10) by the green compact of step (8) in 1250 DEG C-1350 DEG C sintering, be incubated 2 ~ 8 hours, make the ceramics as low-loss microwave medium of magnesium titanate base temperature-stable.
2. a kind of temperature-stable magnesium titanate base microwave medium ceramics according to claim 1, it is characterized in that, described step (1), (4) or (7) adopt planetary ball mill to carry out ball milling, and drum's speed of rotation is 400 revs/min.
3. a kind of temperature-stable magnesium titanate base microwave medium ceramics according to claim 1, is characterized in that, the green compact diameter of described step (9) is 10mm, and thickness is 5mm.
4. a kind of temperature-stable magnesium titanate base microwave medium ceramics according to claim 1, is characterized in that, the preferred sintering temperature of described step (10) is 1300 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250434A (en) * | 2020-10-23 | 2021-01-22 | 厦门松元电子有限公司 | ZMAT series microwave ceramic material and preparation method and application thereof |
| CN112500153A (en) * | 2020-05-19 | 2021-03-16 | 江苏江佳电子股份有限公司 | Temperature coefficient adjustable low-loss dielectric constant microwave dielectric ceramic and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659399A (en) * | 2012-05-23 | 2012-09-12 | 南京工业大学 | Microwave dielectric ceramic and preparation method thereof |
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2015
- 2015-06-26 CN CN201510363642.2A patent/CN104961459A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659399A (en) * | 2012-05-23 | 2012-09-12 | 南京工业大学 | Microwave dielectric ceramic and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 骆春媛等: "MgTiO3基微波介质陶瓷的掺杂改性及低温烧结技术", 《材料导报A:综述篇》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112500153A (en) * | 2020-05-19 | 2021-03-16 | 江苏江佳电子股份有限公司 | Temperature coefficient adjustable low-loss dielectric constant microwave dielectric ceramic and preparation method thereof |
| CN112250434A (en) * | 2020-10-23 | 2021-01-22 | 厦门松元电子有限公司 | ZMAT series microwave ceramic material and preparation method and application thereof |
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