CN1769243A - BMT nanometer powder preparation, multi-phase microwave dielectric ceramic and its preparation method - Google Patents
BMT nanometer powder preparation, multi-phase microwave dielectric ceramic and its preparation method Download PDFInfo
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- CN1769243A CN1769243A CN 200410072627 CN200410072627A CN1769243A CN 1769243 A CN1769243 A CN 1769243A CN 200410072627 CN200410072627 CN 200410072627 CN 200410072627 A CN200410072627 A CN 200410072627A CN 1769243 A CN1769243 A CN 1769243A
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Abstract
The invention belongs to the art of electrical functional material. The invention discloses a barium tantalum-magnesium acid nano multiple-phase pottery, and designs a wet-chemical technique route with low cost, high effect and convenience for synthesis of powdery barium tantalum-magnesium acid, which is used to prepare barium tantalum-magnesium acid nano multiple-phase pottery as an additive (6-12wt %) by traditional art for electrical pottery. This material can be sintered tightly at 1500Deg. C, and the microwave dielectric property is that: the permittivity is 24.8, quality factor below 10GHz is 14500, and the temperature coefficient of capacity is -32ppm/ Deg. C. In the invention, not only the sintering temperature of barium tantalum-magnesium acid system is decreased, but also the quality factor of the prepared material is dramatically improved compared with normal barium tantalum-magnesium acid material.
Description
Technical field
The present invention relates to a kind of stupalith and manufacture method thereof that is applied to electronic devices and components, more particularly, is a kind of ceramic material and manufacture method thereof that is applied to microwave device.
Background technology
Along with the development of microwave integrated circuit and the trend of microwave communication circuit microminiaturization in recent years, have middle high-k, the microwave-medium ceramics of low-dielectric loss and low resonant frequency temperature factor has become a development class novel medium material rapidly.Wherein, the BMT (Ba (Mg that has complex perovskite structure
1/3Ta
2/3) O
3Be abbreviated as BMT) pottery is at present at the highest a kind of material of X-band Q value, it hangs down ε in being
rClassic typical case's representative of class microwave dielectric ceramic materials also is the used main medium ceramic materials in microwave high-frequency field such as present satellite communication.Yet, pure BMT material is easy-sintering not, but often need sintering temperature and the above soaking time of 16h more than 1600 ℃ just can reach the sintered density of practicability and get rid of the by product phase that is unfavorable for microwave dielectric property, thereby seriously restricted the scale operation and the chip type device application of this material; Though doping vario-property and interpolation sintering aid can improve its sintering character, being introduced in of impurity phase reduced its quality factor to a certain extent.The BMT nano-powder that makes with technologies such as sol-gel and hydrolysis of alkoxide has been used for synthetic at a lower temperature single-phase BMT pottery in recent years, but complex process, cost costliness, and the quality factor of the BMT pottery that makes far below the conditional electronic ceramic process of the quality factor of material.Therefore the BMT material is improved microwave dielectric property, reduce production costs, particularly reduce sintering temperature and just seem very necessary with the research that reduces soaking time.
Summary of the invention
The object of the present invention is to provide a kind of novel B MT medium ceramic material that has good sintering character and excellent microwave dielectric property simultaneously and preparation method thereof.Technical problem to be solved by this invention is at present BMT material preparation and the problem in using, design the wet chemical technology route that a kind of cost is lower, high-efficient simple ground synthesizes the BMT nano-powder, and prepare the BMT nano heterogeneous ceramic as additive by the ordinary electronic ceramic process with synthetic BMT nano-powder.This invention has not only significantly reduced the sintering temperature of BMT system, and the quality factor of gained material compare to common BMT material and also are significantly improved.
Ba (Mg
1/3Ta
2/3) O
3The preparation method of nano-powder comprises the steps:
(1) Ta
2O
5Carry out frit reaction with excessive caustic soda, the product dissolved dilution is after hydrolysis, filtration, washing make Ta
2O
5NH
2The O nano colloidal particles;
(2) according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, with Ta
2O
5NH
2The O nano colloidal particles is scattered in the mixing solutions of magnesium citrate, barium citrate, by stir and by force ultrasonic (insert ultra-sonic dispersion, 1500 watts of power) disperse to make it to form steady suspension, the spray-dried presoma that makes the BMT powder of suspension;
(3) presoma is heat-treated make the BMT nano-powder.
Ba (Mg
1/3Ta
2/3) O
3The nano-powder multi-phase microwave dielectric ceramic, BMT nano-powder proportion is 6～12wt%, the common powder proportion of BMT is 88～94wt%.
Ba (Mg
1/3Ta
2/3) O
3The preparation method of nano-powder multi-phase microwave dielectric ceramic comprises the steps:
(1) will be 6～12wt% by BMT nano-powder proportion according to above-mentioned BMT nano-powder that makes and the common powder of BMT, the common powder proportion of BMT is 88～94wt% mixed, make it to mix by wet ball grinding, obtain the BMT composite nano-powder;
(2) the BMT composite nano-powder sieves after adding tackiness agent, after the compression moulding in air atmosphere sintering, described sintering temperature is 1500 ℃, is incubated 4 hours, makes BMT nanometer multi-phase microwave dielectric ceramic.
Being prepared as of the common powder of BMT: according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing high-purity Ta
2O
5, BaCO
3With MgO, wet ball grinding mixes the back oven dry, makes the common powder of BMT in 4 hours 1200 ℃ of calcinings.
Pure BMT material is easy-sintering not, but often need sintering temperature and the above soaking time of 16h more than 1600 ℃ just can reach the sintered density of practicability and get rid of the by product phase that is unfavorable for microwave dielectric property, the preparation method of diphase ceramic material of the present invention, not only effectively reduce sintering temperature (1500 ℃), and significantly shortened soaking time (4h).BMT material of the present invention extremely preparation method has not only improved microwave dielectric property, has simplified processing method, has reduced production cost, particularly reduces sintering temperature and reduces soaking time.
Embodiment
BMT nanometer multi-phase microwave dielectric ceramic of the present invention, the according to the form below Recipe is prepared.
| Sequence number | The BMT nano-powder | The common powder of BMT | Sintering process |
| 1 | 0 gram | 30 grams | 1500 ℃ are incubated 4 hours |
| 2 | 0.9 gram | 29.1 gram | 1500 ℃ are incubated 4 hours |
| 3 | 1.8 gram | 28.2 gram | 1500 ℃ are incubated 4 hours |
| 4 | 2.7 gram | 27.3 gram | 1500 ℃ are incubated 4 hours |
| 5 | 3.6 gram | 26.4 gram | 1500 ℃ are incubated 4 hours |
| 6 | 4.5 gram | 25.5 gram | 1500 ℃ are incubated 4 hours |
The prepared BMT nanometer of above-mentioned Recipe multi-phase microwave dielectric ceramic is carried out density measurement and microwave dielectric property test, and concrete data see the following form.
| Sequence number | Relative density | ε r | Q×f | α c |
| 1 | 89.87 | 19.1 | -- | -110ppm/℃ |
| 2 | 92.94 | 22.8 | 4800 | -46ppm/℃ |
| 3 | 94.14 | 24.1 | 100700 | -39ppm/℃ |
| 4 | 95.98 | 24.8 | 145000 | -32ppm/℃ |
| 5 | 94.85 | 24.3 | 124000 | -30ppm/℃ |
| 6 | 93.80 | 23.9 | 8600 | -42ppm/℃ |
Preparation method to BMT nanometer multi-phase microwave dielectric ceramic is described further below in conjunction with specific embodiment.
Embodiment 1:
(1) takes by weighing high-purity Ta
2O
510 grams and analytical pure caustic soda 30 gram carry out frit reaction after mixing, the water-soluble after-filtration of product is about 7 to make Ta with filtrate with Glacial acetic acid titration to pH value
2O
5NH
2The O nano colloidal particles is separated out.Nano colloidal particles is standby after washing, filtration, takes out a small amount of micelle and heat-treats the water content of determining wherein.
(2) according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing 7.9 gram Ta
2O
5NH
2O nano colloidal particles, 10.6 gram magnesium citrates and 41.2 gram barium citrates.To mix Ta after the dissolving of magnesium citrate and barium citrate
2O
5NH
2The O nano colloidal particles joins in this mixing solutions, by stirring and strong ultra-sonic dispersion is the insert ultra-sonic dispersion, and 1500 watts of power make it to form steady suspension, the spray-dried presoma that makes the BMT powder of suspension, presoma obtained the BMT nano-powder in 2 hours 800 ℃ of calcinings.
(3) according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing the high-purity Ta of 29.2 grams
2O
5, 39.4 the gram BaCO
3With 2.6 gram MgO, wet ball grinding mixes oven dry after 12 hours, makes the common powder of BMT in 4 hours 1200 ℃ of calcinings.
(4) take by weighing BMT nano-powder 1.8 grams, common powder 28.2 grams of BMT, wet ball grinding mixes oven dry after 10 hours, crosses 80 mesh sieves behind the adding adhesive polyethylene alcohol, is pressed into diameter 15mm, the cylindrical biscuit of high 8mm.
(5) the cylindrical biscuit that will make carries out the aerobic sintering in common retort furnace, adopts micro-chip to control furnace temperature automatically.Calcining system is as follows: in 180 minutes temperature is risen to 550 ℃ by room temperature, be incubated 1 hour then under this temperature, again temperature constant speed in 180 minutes is risen to 1500 ℃, and be incubated 4 hours under this temperature, then cooling naturally.
Embodiment 2:
(1) takes by weighing high-purity Ta
2O
510 grams and analytical pure caustic soda 30 gram carry out frit reaction after mixing, the water-soluble after-filtration of product is about 7 to make Ta with filtrate with Glacial acetic acid titration to pH value
2O
5NH
2The O nano colloidal particles is separated out.Nano colloidal particles is standby after washing, filtration, takes out a small amount of micelle and heat-treats the water content of determining wherein.
(2) according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing 7.9 gram Ta
2O
5NH
2O nano colloidal particles, 10.6 gram magnesium citrates and 41.2 gram barium citrates.To mix Ta after the dissolving of magnesium citrate and barium citrate
2O
5NH
2The O nano colloidal particles joins in this mixing solutions, by stirring and strong ultra-sonic dispersion is the insert ultra-sonic dispersion, and 1500 watts of power make it to form steady suspension, the spray-dried presoma that makes the BMT powder of suspension, presoma obtained the BMT nano-powder in 2 hours 800 ℃ of calcinings.
(3) according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing the high-purity Ta of 29.2 grams
2O
5, 39.4 the gram BaCO
3With 2.6 gram MgO, wet ball grinding mixes oven dry after 12 hours, makes the common powder of BMT in 4 hours 1200 ℃ of calcinings.
(4) take by weighing BMT nano-powder 2.7 grams, common powder 27.3 grams of BMT, wet ball grinding mixes oven dry after 10 hours, crosses 80 mesh sieves behind the adding tackiness agent paraffin, is pressed into diameter 15mm, the cylindrical biscuit of high 8mm.
(5) the cylindrical biscuit that will make carries out the aerobic sintering in common retort furnace, adopts micro-chip to control furnace temperature automatically.Calcining system is as follows: in 180 minutes temperature is risen to 550 ℃ by room temperature, be incubated 1 hour then under this temperature, again temperature constant speed in 180 minutes is risen to 1500 ℃, and be incubated 4 hours under this temperature, then cooling naturally.
Embodiment 3:
(1) takes by weighing high-purity Ta
2O
510 grams and analytical pure caustic soda 30 gram carry out frit reaction after mixing, the water-soluble after-filtration of product is about 7 to make Ta with filtrate with Glacial acetic acid titration to pH value
2O
5NH
2The O nano colloidal particles is separated out.Nano colloidal particles is standby after washing, filtration, takes out a small amount of micelle and heat-treats the water content of determining wherein.
(2) according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing 7.9 gram Ta
2O
5NH
2O nano colloidal particles, 10.6 gram magnesium citrates and 41.2 gram barium citrates.To mix Ta after the dissolving of magnesium citrate and barium citrate
2O
5NH
2The O nano colloidal particles joins in this mixing solutions, by stirring and strong ultra-sonic dispersion is the insert ultra-sonic dispersion, and 1500 watts of power make it to form steady suspension, the spray-dried presoma that makes the BMT powder of suspension, presoma obtained the BMT nano-powder in 2 hours 800 ℃ of calcinings.
(3) according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing the high-purity Ta of 29.2 grams
2O
5, 39.4 the gram BaCO
3With 2.6 gram MgO, wet ball grinding mixes oven dry after 12 hours, makes the common powder of BMT in 4 hours 1200 ℃ of calcinings.
(4) take by weighing BMT nano-powder 3.6 grams, common powder 26.4 grams of BMT, wet ball grinding mixes oven dry after 10 hours, crosses 80 mesh sieves behind the adding tackiness agent paraffin, is pressed into diameter 15mm, the cylindrical biscuit of high 8mm.
The cylindrical biscuit that makes is carried out the aerobic sintering in common retort furnace, adopt micro-chip to control furnace temperature automatically.Calcining system is as follows: in 180 minutes temperature is risen to 550 ℃ by room temperature, be incubated 1 hour then under this temperature, again temperature constant speed in 180 minutes is risen to 1500 ℃, and be incubated 4 hours under this temperature, then cooling naturally.
Claims (4)
1. the preparation method of a BMT nanometer powder is characterized in that, comprises the steps:
(1) Ta
2O
5Carry out frit reaction with excessive caustic soda, the product dissolved dilution is after hydrolysis, filtration, washing make Ta
2O
5NH
2The O nano colloidal particles;
(2) according to the stoichiometric ratio (Ba: Mg: Ta=3: 1: 2) of the BMT structure of matter with Ta
2O
5NH
2The O nano colloidal particles is scattered in the mixing solutions of magnesium citrate, barium citrate, by stir and by force ultrasonic (insert ultra-sonic dispersion, 1500 watts of power) disperse to make it to form steady suspension, the spray-dried presoma that makes the BMT powder of suspension;
(3) presoma is heat-treated make the BMT nano-powder.
2. a BMT nanometer powder multi-phase microwave dielectric ceramic is characterized in that, BMT nano-powder proportion is 6～12wt%, and the common powder proportion of BMT is 88～94wt%.
3. the preparation method of a BMT nanometer powder multi-phase microwave dielectric ceramic is characterized in that, comprises the steps:
(1) will make it to mix by wet ball grinding according to the described BMT nano-powder that makes of claim 1 and the common powder of BMT by the described mixed of claim 2, obtain the BMT composite nano-powder;
(2) the BMT composite nano-powder sieves after adding tackiness agent, after the compression moulding in air atmosphere sintering, described sintering temperature is 1500 ℃, is incubated 4 hours, makes BMT nanometer multi-phase microwave dielectric ceramic.
4. preparation method according to claim 3 is characterized in that, being prepared as of the common powder of described BMT: according to the stoichiometric ratio Ba of the BMT structure of matter: Mg: Ta=3: 1: 2, take by weighing high-purity Ta
2O
5, BaCO
3With MgO, wet ball grinding mixes the back oven dry, makes the common powder of BMT in 4 hours 1200 ℃ of calcinings.
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|---|---|---|---|
| CNB2004100726274A CN100344580C (en) | 2004-11-04 | 2004-11-04 | BMT nanometer powder preparation, multi-phase microwave dielectric ceramic and its preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100726274A CN100344580C (en) | 2004-11-04 | 2004-11-04 | BMT nanometer powder preparation, multi-phase microwave dielectric ceramic and its preparation method |
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|---|---|
| CN1769243A true CN1769243A (en) | 2006-05-10 |
| CN100344580C CN100344580C (en) | 2007-10-24 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844204A (en) * | 2015-04-15 | 2015-08-19 | 厦门万明电子有限公司 | High-dielectric microwave ceramic dielectric material, and preparation method and use thereof |
| CN109437899A (en) * | 2018-12-20 | 2019-03-08 | 中国科学院上海硅酸盐研究所 | A kind of microwave medium ceramic material with ultrahigh Q-value and preparation method thereof |
| US11201013B2 (en) | 2019-03-26 | 2021-12-14 | Tdk Corporation | Dielectric film and electronic component |
| US11257620B2 (en) | 2019-03-26 | 2022-02-22 | Tdk Corporation | Dielectric film and electronic component |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143836C (en) * | 2001-01-22 | 2004-03-31 | 兰招武 | High-frequency high-permittivity microwave medium ceramics and its production method |
| KR100487204B1 (en) * | 2001-08-30 | 2005-05-03 | (주)에어링크테크놀로지 | Microwave dielectric ceramic composition and method for manufacturing the same |
-
2004
- 2004-11-04 CN CNB2004100726274A patent/CN100344580C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844204A (en) * | 2015-04-15 | 2015-08-19 | 厦门万明电子有限公司 | High-dielectric microwave ceramic dielectric material, and preparation method and use thereof |
| CN104844204B (en) * | 2015-04-15 | 2017-07-04 | 厦门万明电子有限公司 | A kind of high dielectric microwave ceramic medium material, Preparation method and use |
| CN109437899A (en) * | 2018-12-20 | 2019-03-08 | 中国科学院上海硅酸盐研究所 | A kind of microwave medium ceramic material with ultrahigh Q-value and preparation method thereof |
| US11201013B2 (en) | 2019-03-26 | 2021-12-14 | Tdk Corporation | Dielectric film and electronic component |
| US11257620B2 (en) | 2019-03-26 | 2022-02-22 | Tdk Corporation | Dielectric film and electronic component |
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| CN100344580C (en) | 2007-10-24 |
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