CN103979952A - Method for preparing high-quality-factor magnesium titanate microwave dielectric ceramics by adopting annealing method - Google Patents
Method for preparing high-quality-factor magnesium titanate microwave dielectric ceramics by adopting annealing method Download PDFInfo
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- CN103979952A CN103979952A CN201410175153.XA CN201410175153A CN103979952A CN 103979952 A CN103979952 A CN 103979952A CN 201410175153 A CN201410175153 A CN 201410175153A CN 103979952 A CN103979952 A CN 103979952A
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- magnesium titanate
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Abstract
The invention discloses a method for preparing high-quality-factor magnesium titanate microwave dielectric ceramics by adopting an annealing method. An expression of a target compound is MgTiO3, MgO and TiO2 are used as raw materials, a simple solid phase method is adopted, presintering is carried out at 850 to 1000 DEG C, and sintering is carried out at 1250 DEG C to 1450 DEG C; then, a method of carrying out annealing at 1100 DEG C to 1250 DEG C is adopted for improving the quality factor of products. The high-quality-factor magnesium titanate microwave dielectric ceramics have the characteristics that the dielectric constant [epsilon]r is 17.3 to 17.9, the quality factor Q*f is 240000 to 270000GHz, and the resonant frequency temperature coefficient [tau]f is -41 to -55*10<-6>/DEG C.
Description
Technical field
The invention belongs to a kind of ceramic composition that composition is feature of take, relate in particular to a kind of employing method for annealing and improve MgTiO
3microwave-medium ceramics of quality factor q value and preparation method thereof.
Background technology
The development of nearly more than ten years short-wave communication tedhnology is developing rapidly of mobile communication and satellite communication technology particularly, traditional metal chamber resonator can not meet the demand of application, and market is day by day vigorous to being applied to the demand of microwave-medium ceramics of the novel microwave components and parts such as dielectric resonator, dielectric filter.The basic demand of microwave dielectric ceramic materials is: suitable specific inductivity, lower dielectric loss (higher quality factor q value) and less frequency-temperature coefficient.
Along with the development of stupalith, for meeting different application, the novel material of various excellent performances continues to bring out.MgTiO
3pottery series ceramic material is owing to having higher quality factor, and abundant raw material, with low cost, has been subject to paying close attention to widely.But in order to meet the requirement of microwave application, the method that research improves Q value of material has great importance and is worth.
Summary of the invention
Object of the present invention is in order to adapt to electronic information technology constantly to the needs of high frequency and digitizing future development, to provide a kind of with MgO and TiO
2for raw material, by simple solid phase method, prepare MgTiO
3microwave dielectric ceramic materials, and by the method for annealing, improve its quality factor q value.
The present invention is achieved by following technical solution.
Adopt method for annealing to prepare high quality factor magnesium titanate microwave-medium ceramics, target synthetics expression formula is MgTiO
3;
The preparation method of this high quality factor magnesium titanate microwave-medium ceramics, has following steps:
(1) by raw material MgO and TiO
2press stoichiometric equation MgTiO
3prepare burden; Powder is put into polyester tank, add after deionized water and zirconium ball, on planetary ball mill, ball milling is 4～24 hours; ;
(2) raw material after step (1) ball milling is put into loft drier, in 100～120 ℃ of oven dry, then cross 40 mesh sieves;
(3) powder after step (2) is dried, sieved is put into moderate oven, in 850～1000 ℃ of pre-burnings, is incubated 2～8 hours;
(4) paraffin that is 6%～10% using the additional mass percent of powder after step (3) pre-burning carries out granulation as tackiness agent, crosses 80 mesh sieves, with powder compressing machine, with the pressure of 4～8MPa, makes green compact;
(5) by the green compact of step (4) in 1250 ℃ of-1450 ℃ of sintering, be incubated 2～8 hours, make magnesium titanate microwave-medium ceramics;
(6) the magnesium titanate microwave-medium ceramics of step (5) is annealed at 1100 ℃～1250 ℃, be incubated 2～14h, make the magnesium titanate microwave-medium ceramics of high quality factor;
Described step (1) adopts planetary ball mill to carry out ball milling, and drum's speed of rotation is 400 revs/min.
The mass ratio of the powder of described step (1) and deionized water and zirconium ball is 1 ︰ 1 ︰ 1.
The green compact of described step (4) are the former plate shape of diameter 10mm thickness 5mm.
The sintering temperature of described step (5) is 1350 ℃.
The annealing temperature of described step (6) is 1200 ℃.
The present invention is with MgO and TiO
2for raw material, by simple solid phase method, prepared a kind of novel microwave dielectric ceramic materials MgTiO
3, then by the method for annealing, improve its quality factor q value.Its DIELECTRIC CONSTANT ε
rbe 17.3～17.9, quality factor q * f is 240000～270000GHz, temperature coefficient of resonance frequency τ
ffor-41～-55 * 10
-6/ ℃.This preparation method has greatly improved MgTiO
3the quality factor q value of microwave dielectric ceramic materials.
Embodiment
The present invention is with MgO (analytical pure) and TiO
2(analytical pure) is initial feed, by simple solid phase method, prepares microwave-medium ceramics.Specific embodiments is as follows:
1.MgO and TiO
2press MgTiO
3stoichiometric ratio is prepared burden, and proportioning raw materials is: 3.3530g MgO, 6.6470gTiO
2.The mixed powder of about 10g is put into polyester tank, add 200ml deionized water, add after the zirconium ball of 150g, on planetary ball mill, ball milling is 12 hours, and rotating speed is 400 revs/min;
2. the raw material after ball milling is placed in loft drier in 100～120 ℃ of oven dry, then crosses 40 mesh sieves;
3. the powder of drying after sieving is put into moderate oven, in 900 ℃ of pre-burnings, is incubated 4 hours;
4. to add quality percentage composition be that 8% paraffin wax binder is carried out granulation to the powder after pre-burning, crosses after 80 mesh sieves, and with powder compressing machine, powder being pressed into diameter under the pressure of 4MPa is 10mm, the green compact that thickness is about 5mm; Green compact, at 1350 ℃ of sintering, are incubated to 4 hours, make magnesium titanate microwave-medium ceramics.
5. the magnesium titanate microwave-medium ceramics after sintering is annealed at 1150 ℃～1200 ℃, be incubated 6～10h, make the magnesium titanate microwave-medium ceramics of high quality factor.
6. by the microwave property of network analyzer and dependence test fixture test resulting product.
Related process parameter and the microwave dielectric property of the specific embodiment of the invention refer to table 1.
Table 1
Claims (6)
1. adopt method for annealing to prepare high quality factor magnesium titanate microwave-medium ceramics, target synthetics expression formula is MgTiO
3;
The preparation method of this high quality factor magnesium titanate microwave-medium ceramics, has following steps:
(1) by raw material MgO and TiO
2press stoichiometric equation MgTiO
3prepare burden; Powder is put into polyester tank, add after deionized water and zirconium ball, on planetary ball mill, ball milling is 4～24 hours; ;
(2) raw material after step (1) ball milling is put into loft drier, in 100～120 ℃ of oven dry, then cross 40 mesh sieves;
(3) powder after step (2) is dried, sieved is put into moderate oven, in 850～1000 ℃ of pre-burnings, is incubated 2～8 hours;
(4) paraffin that is 6%～10% using the additional mass percent of powder after step (3) pre-burning carries out granulation as tackiness agent, crosses 80 mesh sieves, with powder compressing machine, with the pressure of 4～8MPa, makes green compact;
(5) by the green compact of step (4) in 1250 ℃ of-1450 ℃ of sintering, be incubated 2～8 hours, make magnesium titanate microwave-medium ceramics;
(6) the magnesium titanate microwave-medium ceramics of step (5) is annealed at 1100 ℃～1250 ℃, be incubated 2～14h, make the magnesium titanate microwave-medium ceramics of high quality factor.
2. employing method for annealing according to claim 1 is prepared high quality factor magnesium titanate microwave-medium ceramics, it is characterized in that, described step (1) adopts planetary ball mill to carry out ball milling, and drum's speed of rotation is 400 revs/min.
3. employing method for annealing according to claim 1 is prepared high quality factor magnesium titanate microwave-medium ceramics, it is characterized in that, the mass ratio of the powder of described step (1) and deionized water and zirconium ball is 1 ︰ 1 ︰ 1.
4. employing method for annealing according to claim 1 is prepared high quality factor magnesium titanate microwave-medium ceramics, it is characterized in that, the green compact of described step (4) are the former plate shape of diameter 10mm thickness 5mm.
5. employing method for annealing according to claim 1 is prepared high quality factor magnesium titanate microwave-medium ceramics, it is characterized in that, the sintering temperature of described step (5) is 1350 ℃.
6. employing method for annealing according to claim 1 is prepared high quality factor magnesium titanate microwave-medium ceramics, it is characterized in that, the annealing temperature of described step (6) is 1200 ℃.
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| CN201410175153.XA CN103979952A (en) | 2014-04-28 | 2014-04-28 | Method for preparing high-quality-factor magnesium titanate microwave dielectric ceramics by adopting annealing method |
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| CN201410175153.XA CN103979952A (en) | 2014-04-28 | 2014-04-28 | Method for preparing high-quality-factor magnesium titanate microwave dielectric ceramics by adopting annealing method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206134A (en) * | 2018-10-24 | 2019-01-15 | 天津大学 | A kind of preparation method of high quality factor magnesium titanate base microwave medium ceramics |
| CN110577401A (en) * | 2019-08-14 | 2019-12-17 | 天津大学 | preparation method of titanium dioxide-based dielectric material |
| CN113880573A (en) * | 2021-09-10 | 2022-01-04 | 天津大学 | Temperature-stable low-dielectric-loss microwave dielectric ceramic material and preparation method thereof |
| CN113968732A (en) * | 2021-11-29 | 2022-01-25 | 湖南纳金新材料技术有限公司 | Preparation method of high-stability low-loss microwave dielectric ceramic material and microwave dielectric ceramic material prepared by applying same |
-
2014
- 2014-04-28 CN CN201410175153.XA patent/CN103979952A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| HONG ZHU ET AL.: "Annealing Effects on Conductivity and Microwave Dielectric Loss of MgTiO3 Ceramics", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 * |
| SANTHOSH KUMAR THATIKONDA ET AL.: "Effects of CeO2 nanoparticles and annealing temperature on the microwave dielectric properties of MgTiO3 ceramics", 《CERAMICS INTERNATIONAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206134A (en) * | 2018-10-24 | 2019-01-15 | 天津大学 | A kind of preparation method of high quality factor magnesium titanate base microwave medium ceramics |
| CN110577401A (en) * | 2019-08-14 | 2019-12-17 | 天津大学 | preparation method of titanium dioxide-based dielectric material |
| CN113880573A (en) * | 2021-09-10 | 2022-01-04 | 天津大学 | Temperature-stable low-dielectric-loss microwave dielectric ceramic material and preparation method thereof |
| CN113968732A (en) * | 2021-11-29 | 2022-01-25 | 湖南纳金新材料技术有限公司 | Preparation method of high-stability low-loss microwave dielectric ceramic material and microwave dielectric ceramic material prepared by applying same |
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Application publication date: 20140813 |