CN102887702A - Low-temperature-sintered lithium-zinc-titanium microwave dielectric ceramic and preparation method thereof - Google Patents
Low-temperature-sintered lithium-zinc-titanium microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- CN102887702A CN102887702A CN2012103813090A CN201210381309A CN102887702A CN 102887702 A CN102887702 A CN 102887702A CN 2012103813090 A CN2012103813090 A CN 2012103813090A CN 201210381309 A CN201210381309 A CN 201210381309A CN 102887702 A CN102887702 A CN 102887702A
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Abstract
The invention discloses a low-temperature-sintered lithium-zinc-titanium microwave dielectric ceramic which is composed of Li2ZnTi3O8-m wt% MBS, wherein 0<=m<=5, and m is the mass percentage of an added sintering assistant; and the MBS is composed of 42 wt% of MgO, 45 wt% of B2O3 and 13 wt% of SiO2. The preparation method comprises the following steps: mixing Li2CO3, ZnO and TiO2 according to mol ratio, carrying out ball milling, drying, presintering at 900 DEG C, adding the sintering assistant to carry out secondary mixing, and finally, sintering at 860-940 DEG C to obtain the microwave dielectric ceramic. The invention successfully lowers the sintering temperature to 900 DEG C, and maintains the excellent microwave dielectric properties; and the invention has the advantages of simple preparation technique and no pollution, and can be used in the fields related to LTCC (low temperature co-fired ceramic).
Description
Technical field
The invention belongs to a kind of ceramic composition take composition as feature, particularly a kind of new type low temperature sintering lithium zinc titanium (Li of system
2ZnTi
3O
8) microwave dielectric ceramic materials and preparation method thereof.
Background technology
Along with communication equipment towards high frequency, small-sized, light weight, high integrated, multi-functional, high reliability and low-cost future development, the microwave circuit components and parts take microwave-medium ceramics as the basis need to possess better dielectric and processing performance to satisfy application requiring.Microwave-medium ceramics is as the critical material of making these devices, and its performance index have determined the performance of micro-wave communication device and system to a great extent.And LTCC Technology (LTCC) realize just microwave device to high frequency, at a high speed, the important channel of lightweight, the future development such as slim, the sintering temperature of LTCC technical requirements microwave dielectric ceramic materials is lower than 1000 ℃, and with the common burning of electrode materials Ag (961 ℃ of fusing points) chemical reaction does not occur.The sintering temperature of most of microwave dielectric ceramic materials of research can't be burnt with metal electrode material at low temperatures altogether all more than 1200 ℃ at present.Therefore, reduce the sintering temperature of microwave-medium ceramics and develop the microwave dielectric ceramic materials that intrinsic sintering temperature is low, dielectric properties are good and have great practical value.
The Li of spinel structure
2ZnTi
3O
8Be a kind of microwave dielectric material of development of novel, its sintering temperature is 1075 ℃, has excellent dielectric properties at microwave frequency band.The present invention adopts conventional solid-state method, under the condition of adding fusing assistant, prepares low sintering Li
2ZnTi
3O
8Microwave-medium ceramics.
Summary of the invention
The present invention seeks to, with Li
2CO
3, ZnO, TiO
2Be main raw material, add a small amount of MBS glass low melting point sintering aid, make lithium zinc sintering temperature of lithium-niobium-titanium serial Microwave Dielectric Ceramics (MWDC) successfully be reduced to 900 ℃, keep simultaneously its excellent microwave dielectric property.
The present invention is achieved by following technical solution.
A kind of low temperature sintering lithium zinc titanium series microwave dielectric ceramic is by Li
2ZnTi
3O
8-m wt%MBS forms, wherein, 0＜m＜5, m is the mass percent that adds sintering aid;
Described MBS is 42wt%MgO-45wt%B
2O
3-13wt%SiO
2
The preparation method of low temperature sintering lithium zinc titanium series microwave dielectric ceramic has following steps:
⑴ according to Li
2ZnTi
3O
8, with raw material Li
2CO
3, ZnO, TiO
2Li in molar ratio
2CO
3: ZnO:TiO
2=1:1:3 weigh batching;
⑵ put into ball grinder with the powder of step ⑴ preparation, adds zirconia ball and deionized water, material, and water, the mass ratio of ball are 1:7:7, ball milling 4～6 hours; Place infrared drying oven to dry the raw material behind the ball milling, cross 40 mesh sieves after the oven dry, obtain evengranular powder;
⑶ the powder that handle step ⑵ well is 900 ℃ of lower pre-burnings 3 hours, and insulation 4 hours under this temperature, synthetic principal crystalline phase; Again preburning powdered material is pulverized, pressed Li
2ZnTi
3O
8The ratio of-mwt%MBS is to wherein adding mwt%MBS, wherein, 0＜m＜5, m is the mass percent that adds sintering aid;
Described MBS is 42wt%MgO-45wt%B
2O
3-13wt%SiO
2
⑷ put into ball grinder with step ⑶ products therefrom, adds deionized water in powder, and ball milling 6～12 hours adds mass percent and be 6～10% paraffin as the tackiness agent granulation after the oven dry, cross 80 mesh sieves after, use the powder compressing machine pressure forming;
⑸ the green compact after with step ⑷ moulding are incubated 2～6 hours in 860～940 ℃ of sintering, make microwave-medium ceramics;
⑹ the microwave dielectric property of test microwave-medium ceramics.
The operating pressure of described step ⑷ tabletting machine is 4～6MPa, and the green compact specification is the right cylinder of Φ 10mm * 5mm.
The ball milling of described step ⑵ and step ⑷ adopts planetary ball mill, and rotating speed is 1000 rev/mins.
Described step ⑸ is the microwave dielectric property by network analyzer test microwave-medium ceramics.
The preferred sintering temperature of described step ⑸ is 880-900 ℃, is incubated 4 hours.
The preferred Ball-milling Time of described step ⑵ is 6 hours.
The preferred MBS addition of described step ⑶ is 2.0wt%.
The present invention is with Li
2ZnTi
3O
8Microwave-medium ceramics is the basis, add the MBS sintering aid, successfully its sintering temperature is reduced to 900 ℃, having prepared specific inductivity is 23～25, quality factor 27000～56200GHz, temperature coefficient of resonance frequency be-9.4～-microwave-medium ceramics of 12.9ppm/ ℃.In addition, this preparation technology is simple, and process is pollution-free, has improved its temperature coefficient of resonance frequency, is a kind of desirable LTCC material, is with a wide range of applications.
Embodiment
The present invention adopts purity greater than 99.9% analytical pure raw material Li
2CO
3, ZnO, TiO
2Preparation Li
2ZnTi
3O
8Microwave-medium ceramics.
At first, according to Li
2ZnTi
3O
8, with Li
2CO
3, ZnO, TiO
2Li in molar ratio
2CO
3: ZnO:TiO
2=1:1:3 weigh batching.Mixed powder is put into the polyester tank, add deionized water and zirconia ball, material, water, the mass ratio of ball is 1:7:7, and ball milling is 4～6 hours hours on planetary ball mill, and rotating speed is 1000 rev/mins.Again the raw material behind the ball milling is dried in the 1500W infrared drying oven, after the oven dry raw material crossed 40 mesh sieves.Powder after sieving is 900 ℃ of lower pre-burnings 3 hours, and insulation 4 hours under this temperature, synthetic principal crystalline phase.Again preburning powdered material is pulverized, pressed Li
2ZnTi
3O
8The ratio of-m wt%MBS is to wherein adding m wt%MBS, and wherein, MBS is 42wt%MgO-45wt%B
2O
3-13wt%SiO
2, 0＜m＜5, m is the mass percent that adds sintering aid; After being made into powder, add deionized water in the powder, ball milling 6～12 hours hours adds mass percent and is 6～10% paraffin as the tackiness agent granulation after the oven dry, cross 80 mesh sieves after, depress to the cylinder of Φ 10mm * 5mm at 6MPa pressure with powder compressing machine.Again with green compact in 860～940 ℃ of sintering, be incubated 2～6 hours hours, make lithium zinc titanium series microwave dielectric ceramic.Pass through at last the microwave dielectric property of network analyzer test article.
Specific embodiment of the invention preparation technology's relevant technologies parameter sees table 1 for details.
Table 1
Testing method of the present invention and test set are as follows:
1. the diameter of sample and thickness use milscale to measure.
2. by Agilent 8720ES network analyzer, adopt open type chamber parallel plate method to measure the specific inductivity of prepared cylindrical ceramic, test fixture is put into the high low temperature circulation warm of ESPEC MC-710F type case carry out the measurement of temperature coefficient of resonance frequency, temperature range is 25-85 ℃.
3. adopt enclosed chamber method to measure the quality factor of prepared cylindrical ceramic sample, the survey frequency scope is in the 7-8GHz scope.
The microwave dielectric property test result of the specific embodiment of the invention sees table 2 for details.
Table 2
| № | ε r | Q×f(GHz) | τ f(ppm/℃) |
| Embodiment 1 | 24.2 | 41300 | -11.5 |
| Embodiment 2 | 24.1 | 36000 | -12.5 |
| Embodiment 3 | 24.8 | 45700 | -11.7 |
| Embodiment 4 | 24.7 | 52300 | -9.6 |
| Embodiment 5 | 24.3 | 49700 | -10.9 |
| Embodiment 6 | 24.1 | 51300 | -11.5 |
| Embodiment 7 | 23.8 | 26800 | -12.1 |
| Embodiment 8 | 23.5 | 35400 | -10.7 |
| Embodiment 9 | 24.5 | 45000 | -12.9 |
| Embodiment 10 | 24.7 | 55000 | -10.4 |
| Embodiment 11 | 25.0 | 56200 | -9.9 |
| Embodiment 12 | 24.1 | 41300 | -9.4 |
Claims (8)
1. low temperature sintering lithium zinc titanium series microwave dielectric ceramic is by Li
2ZnTi
3O
8-mwt%MBS forms, wherein, 0＜m＜5, m is the mass percent that adds sintering aid.
Described MBS is 42wt%MgO-45wt%B
2O
3-13wt%SiO
2
2. the preparation method of the low temperature sintering lithium zinc titanium series microwave dielectric ceramic of claim 1 has following steps.
⑴ according to Li
2ZnTi
3O
8, with raw material Li
2CO
3, ZnO, TiO
2Li in molar ratio
2CO
3: ZnO:TiO
2=1:1:3 weigh batching;
⑵ put into ball grinder with the powder of step ⑴ preparation, adds zirconia ball and deionized water, material, and water, the mass ratio of ball are 1:7:7, ball milling 4～6 hours; Place infrared drying oven to dry the raw material behind the ball milling, cross 40 mesh sieves after the oven dry, obtain evengranular powder;
⑶ the powder that handle step ⑵ well is 900 ℃ of lower pre-burnings 3 hours, and insulation 4 hours under this temperature, synthetic principal crystalline phase; Again preburning powdered material is pulverized, pressed Li
2ZnTi
3O
8The ratio of-mwt%MBS is to wherein adding mwt%MBS, wherein, 0＜m＜5, m is the mass percent that adds sintering aid;
Described MBS is 42wt%MgO-45wt%B
2O
3-13wt%SiO
2
⑷ put into ball grinder with step ⑶ products therefrom, adds deionized water in powder, and ball milling 6～12 hours adds mass percent and be 6～10% paraffin as the tackiness agent granulation after the oven dry, cross 80 mesh sieves after, use the powder compressing machine pressure forming;
⑸ the green compact after with step ⑷ moulding are incubated 2～6 hours in 860～940 ℃ of sintering, make microwave-medium ceramics;
⑹ the microwave dielectric property of test microwave-medium ceramics.
3. according to claim 2 the preparation method of low temperature sintering lithium zinc titanium series microwave dielectric ceramic is characterized in that the operating pressure of described step ⑷ tabletting machine is 4～6MPa, and the green compact specification is the right cylinder of Φ 10mm * 5mm.
4. according to claim 2 the preparation method of low temperature sintering lithium zinc titanium series microwave dielectric ceramic is characterized in that the ball milling of described step ⑵ and step ⑷ adopts planetary ball mill, and rotating speed is 1000 rev/mins.
5. according to claim 2 the preparation method of low temperature sintering lithium zinc titanium series microwave dielectric ceramic is characterized in that described step ⑸ is the microwave dielectric property by network analyzer test microwave-medium ceramics.
6. according to claim 2 the preparation method of low temperature sintering lithium zinc titanium series microwave dielectric ceramic is characterized in that the preferred sintering temperature of described step ⑸ is 880-900 ℃, is incubated 4 hours.
7. according to claim 2 the preparation method of low temperature sintering lithium zinc titanium series microwave dielectric ceramic is characterized in that the preferred Ball-milling Time of described step ⑵ is 6 hours.
8. according to claim 2 the preparation method of low temperature sintering lithium zinc titanium series microwave dielectric ceramic is characterized in that the preferred MBS addition of described step ⑶ is 2.0wt%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193324A (en) * | 2014-08-14 | 2014-12-10 | 电子科技大学 | ZnO-MgO-TiO2 serial LTCC (low temperature co-fired ceramic) material |
| CN104692793A (en) * | 2015-02-05 | 2015-06-10 | 桂林理工大学 | Temperature-stable low-dielectric constant microwave dielectric ceramic Li2ZnTi5O12 and preparation method thereof |
| CN108793994A (en) * | 2018-08-15 | 2018-11-13 | 天津大学 | A kind of donor doping microwave dielectric ceramic with medium dielectric constant and preparation method thereof |
| CN108975906A (en) * | 2018-08-15 | 2018-12-11 | 天津大学 | A kind of medium dielectric constant microwave medium high stable type microwave-medium ceramics and preparation method thereof |
| CN112608144A (en) * | 2020-12-17 | 2021-04-06 | 洛阳中超新材料股份有限公司 | Lithium-based microwave dielectric ceramic material, preparation method thereof and lithium-based microwave dielectric ceramic |
| CN113242844A (en) * | 2019-02-27 | 2021-08-10 | 费罗公司 | LTCC dielectric compositions and devices with high Q |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193324A (en) * | 2014-08-14 | 2014-12-10 | 电子科技大学 | ZnO-MgO-TiO2 serial LTCC (low temperature co-fired ceramic) material |
| CN104692793A (en) * | 2015-02-05 | 2015-06-10 | 桂林理工大学 | Temperature-stable low-dielectric constant microwave dielectric ceramic Li2ZnTi5O12 and preparation method thereof |
| CN108793994A (en) * | 2018-08-15 | 2018-11-13 | 天津大学 | A kind of donor doping microwave dielectric ceramic with medium dielectric constant and preparation method thereof |
| CN108975906A (en) * | 2018-08-15 | 2018-12-11 | 天津大学 | A kind of medium dielectric constant microwave medium high stable type microwave-medium ceramics and preparation method thereof |
| CN113242844A (en) * | 2019-02-27 | 2021-08-10 | 费罗公司 | LTCC dielectric compositions and devices with high Q |
| JP2022521774A (en) * | 2019-02-27 | 2022-04-12 | フエロ コーポレーション | LTCC dielectric compositions and appliances with high Q value |
| JP7220299B2 (en) | 2019-02-27 | 2023-02-09 | フエロ コーポレーション | LTCC dielectric compositions and devices with high Q values |
| CN113242844B (en) * | 2019-02-27 | 2023-08-08 | 费罗公司 | LTCC dielectric compositions and devices having high Q values |
| CN112608144A (en) * | 2020-12-17 | 2021-04-06 | 洛阳中超新材料股份有限公司 | Lithium-based microwave dielectric ceramic material, preparation method thereof and lithium-based microwave dielectric ceramic |
| CN112608144B (en) * | 2020-12-17 | 2022-01-28 | 洛阳中超新材料股份有限公司 | Lithium-based microwave dielectric ceramic material, preparation method thereof and lithium-based microwave dielectric ceramic |
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Application publication date: 20130123 |