CN111978080A - High-adjustable low-loss low-sintering ceramic material of barium strontium titanate composite copper gallate - Google Patents
High-adjustable low-loss low-sintering ceramic material of barium strontium titanate composite copper gallate Download PDFInfo
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- 238000005245 sintering Methods 0.000 title claims abstract description 34
- 229910052454 barium strontium titanate Inorganic materials 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 24
- 239000010949 copper Substances 0.000 title claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 22
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 239000011812 mixed powder Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 9
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910002113 barium titanate Inorganic materials 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229920001778 nylon Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000010304 firing Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910010252 TiO3 Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 229910015805 BaWO4 Inorganic materials 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Abstract
The low-sintering ceramic material of the barium strontium titanate composite copper gallate with high adjustability and low loss is characterized in that the general formula of the components of the low-sintering ceramic material of the barium strontium titanate-based composite copper gallate with high adjustability and low loss is as follows: (1-x) Ba0.4Sr0.6TiO3‑xCuGa2O4Wherein the value range of x is more than or equal to 5wt% and less than or equal to 90wt%, and BaTiO is selected3、SrTiO3CuO and Ga2O3The powder is used as a raw material, mixed powder is prepared by batching, ball milling, drying and high-temperature presintering, presintering is carried out at the temperature of 550-600 ℃ after tabletting, and then, firing is carried out at the temperature of 1000-1050 ℃. The low-sintering ceramic material of the barium strontium titanate composite copper gallate with high adjustability and low loss prepared by the invention can meet the co-sintering requirement of cheap copper electrodes and can work in a wide rangeThe performance is stable at the temperature range of (-55-60 ℃) and the comprehensive performance is high.
Description
Technical Field
The invention belongs to the technical field of electronic materials and devices, and particularly relates to a high-adjustable low-loss barium strontium titanate composite copper gallate low-sintering ceramic material and preparation thereof.
Background
The ferroelectric material barium strontium titanate is well known for its large dielectric nonlinearity. The BST-based composite material prepared by modification means such as ion doping, dielectric compounding and the like can be used as microwave devices such as a tunable phase shifter, a tunable capacitor, a filter and the like. However, three important performance parameters of a material, dielectric constant, tunability and Q value ((Q))1/tan) They are often restricted to each other. In reported research work, researchers discovered that the quality factor Q value can be significantly improved but the electrical tunability is deteriorated by modifying the performance of barium strontium titanate by doping rare earth ions; the scholars adopt dielectric BaWO4The composite barium strontium titanate shows that the electrical adjustability is obviously improved compared with that of the pure barium strontium titanate, but the Q value is deteriorated. However, the dielectric compounding method has a simple process and is beneficial to reducing the cost, so that the method is still a feasible means for adopting the dielectric to compound barium strontium titanate for modification, and the key point is to find a proper dielectric material which can simultaneously meet the key parameters of high electric adjustability, high Q value and low dielectric constant. Further, the miniaturization, high frequency, and integration of electronic components are progressing. Reducing the sintering temperature of BST-based ceramic materials to meet the requirements of LTCC technology is a hot spot today. In reported work, low melting point oxides, fluorides, glasses, and the like are generally added to lower the sintering temperature of BST, but controlling the dielectric constant at a lower level often requires excessive addition, which deteriorates dielectric tunability. Therefore, the dual purposes of low BST fever and reasonable modification are still difficult.
Disclosure of Invention
The invention aims to provide a high-adjustable low-loss low-sintering ceramic material of barium strontium titanate composite copper gallate, which has high comprehensive performance and simple preparation process, and the technical scheme is as follows:
the low-sintering ceramic material of the barium strontium titanate composite copper gallate with high adjustability and low loss is characterized by being a low-sintering ceramic material of the barium strontium titanate composite copper gallate with high adjustability and low lossThe chemical composition formula of (A) is: (1-x) Ba0.4Sr0.6TiO3-xCuGa2O4Wherein the value range of x is more than or equal to 5wt% and less than or equal to 90wt%, and the preparation method comprises the following steps:
(1) selecting BaTiO3Powder, SrTiO3Powder, CuO powder and Ga2O3The powder is used as main raw material according to (1-x) Ba0.4Sr0.6TiO3-xCuGa2O4Proportioning the Ba, Sr, Ti, Cu and Ga according to the stoichiometric ratio, putting the proportioned raw materials into a nylon ball milling tank, adding zirconia balls and ball milling media, carrying out ball milling, discharging, drying, presintering and grinding to obtain mixed powder 1; the temperature for pre-sintering is 1100-1200 ℃, and the sintering time is 4-6 hours.
(2) Adding the mixed powder 1 in the step (1) into zirconia balls and absolute ethyl alcohol or deionized water for ball milling for 24-48 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 7-10%, uniformly mixing, granulating, and pressing under the pressure of 10-100 MPa to prepare a ceramic green sheet;
(4) carrying out glue discharging treatment on the ceramic green sheet in the step (3) at the temperature of 550-600 ℃ for 4-10 hours; and after the binder is removed, sintering the mixture at the temperature of 1000-1050 ℃ for 4-6 hours to form ceramic, thus obtaining the low-sintering ceramic material of barium strontium titanate composite copper gallate with high adjustability and low loss.
The barium strontium titanate composite copper gallate ceramic material with high adjustability and low loss has the following advantages:
(1) the Curie temperature of the composite ceramic is controlled in a proper range through the preferable Ba/Sr, and the composite ceramic is (1-x) Ba0.4Sr0.6TiO3-xCuGa2O4The performance is stable in a wide working temperature range (-55-60 ℃).
(2) The dielectric constant is adjusted in different suitable intervals by using different x mass ratios, so that the requirements of different devices under application can be met, and the application range of the material is widened;
(3) the dielectric constant is low, the Q value is high, the electric adjustability is high, and the comprehensive dielectric property under microwave is high;
(4) the traditional electronic ceramic preparation process is adopted, so that the process is simple; the material system belongs to green environment-friendly materials, and has no toxic or side effect. The material can be co-fired with a cheap copper electrode, has excellent performance and is suitable for components such as a microwave adjustable phase shifter, a capacitor, a microwave dielectric antenna and the like.
Detailed Description
Example 1
(1) According to 90wt% of Ba0.4Sr0.6TiO3+10 wt % CuGa2O4In the chemical ratio of BaTiO312.4g、SrTiO314.6g, CuO0.5g and Ga2O32.5g of powder, putting the prepared raw materials into a nylon ball milling tank, adding zirconia balls and ball milling media, carrying out ball milling, discharging, drying, pre-sintering and grinding to obtain mixed powder 1; the temperature for pre-sintering is 1100 ℃ and 1200 ℃ respectively, and the sintering time is 6 hours;
(2) adding zirconia balls and absolute ethyl alcohol or deionized water into the mixed powder 1 in the step (1) to perform ball milling for 24 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 10%, uniformly mixing and granulating, and then pressing under the pressure of 10MPa to prepare a ceramic green sheet;
(4) carrying out heat preservation on the ceramic green sheet in the step (3) at 550 ℃ for 10 hours to carry out glue discharging treatment; after the binder is removed, the ceramic is sintered for 4 hours at 1050 ℃ to obtain the low-sintering ceramic material of barium strontium titanate composite copper gallate with high adjustability and low loss.
BaTiO used for experiment3Purity of 99.5%, produced by Michelin Biochemical technology Ltd, SrTiO399.5% purity, produced by Michelin Biochemical technology Ltd, 99% purity of CuO, produced by Tianjin chemical reagent three factories, Ga2O3Michelin biochemical technology with purity of 99.99%Limited company production;
the prepared high-electric adjustable high-Q-value barium strontium titanate-based composite copper gallate ceramic has the following properties: curie temperature Tc (K) @10kHz of 214, dielectric constantr(room temperature 20 ℃ C.) 637 kHz and tan dielectric loss(room temperature 20 ℃) 0.0090 @10kHz, dielectric tunabilityT(30 kV/cm, 20 ℃) 9.8% at @10kHz, 1758% at the resonance frequency (MHz), and a dielectric constant at resonancer605 and a Q value of 173.
Example 2
(1) According to 70 wt% of Ba0.4Sr0.6TiO3+30 wt % CuGa2O4In the chemical ratio of BaTiO39.6g、SrTiO311.4g, CuO1.6g and Ga2O37.4g of powder, putting the prepared raw materials into a nylon ball milling tank, adding zirconia balls and a ball milling medium, carrying out ball milling, discharging, drying, pre-sintering and grinding to obtain mixed powder 1; the pre-sintering temperature is 1100 ℃ and 1200 ℃, and the sintering time is 5 hours;
(2) adding zirconia balls and absolute ethyl alcohol or deionized water into the mixed powder 1 in the step (1) to perform ball milling for 30 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 10%, uniformly mixing and granulating, and then pressing under the pressure of 10MPa to prepare a ceramic green sheet;
(4) carrying out heat preservation on the ceramic green sheet in the step (3) at 580 ℃ for 7 hours to carry out glue discharging treatment; after the binder is removed, the ceramic is sintered for 4 hours at 1030 ℃ to obtain the low-sintering ceramic material of barium strontium titanate composite copper gallate with high adjustability and low loss.
BaTiO used for experiment3Purity of 99.5%, produced by Michelin Biochemical technology Ltd, SrTiO399.5% purity, produced by Michelin Biochemical technology Ltd, 99% purity of CuO, produced by Tianjin chemical reagent three factories, Ga2O3The purity of 99.99% produced by McLin Biotechnology Ltd;
prepared byThe high adjustable low loss barium strontium titanate composite copper gallate ceramic has the following properties: curie temperature Tc (K) @10kHz of 219 and dielectric constantr(room temperature 20 ℃ C.) with a dielectric loss tan of 363 at 10kHzAt room temperature of 20 deg.C, 0.0117 at 10kHz and dielectric tunabilityT(30 kV/cm, 20 ℃) 12.01% at @10kHz, 2132 at the resonance frequency (MHz), and the dielectric constant at resonancer345, and a Q value of 225.
Example 3
(1) According to 50 wt% of Ba0.4Sr0.6TiO3+50 wt % CuGa2O4In the chemical ratio of BaTiO36.9g、SrTiO38.1g, CuO2.6g and Ga2O312.4g of powder, putting the prepared raw materials into a nylon ball milling tank, adding zirconia balls and ball milling media, carrying out ball milling, discharging, drying, pre-sintering and grinding to obtain mixed powder 1; the pre-sintering temperature is 1100 ℃ and 1200 ℃, and the sintering time is 4 hours;
(2) adding zirconia balls and absolute ethyl alcohol or deionized water into the mixed powder 1 in the step (1) to perform ball milling for 48 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 8%, uniformly mixing and granulating, and then pressing under the pressure of 30MPa to prepare a ceramic green sheet;
(4) carrying out heat preservation on the ceramic green sheet in the step (3) at the temperature of 600 ℃ for 4 hours to carry out glue discharging treatment; after the binder is removed, the ceramic is sintered at 1000 ℃ for 6 hours, and the low-sintering ceramic material of barium strontium titanate composite copper gallate with high adjustability and low loss is obtained.
BaTiO used for experiment3Purity of 99.5%, produced by Michelin Biochemical technology Ltd, SrTiO399.5% purity, produced by Michelin Biochemical technology Ltd, 99% purity of CuO, produced by Tianjin chemical reagent three factories, Ga2O3The purity of 99.99% produced by McLin Biotechnology Ltd;
the prepared high-electric adjustable high-Q-value barium strontium titanate-based composite copper gallate ceramic has the following properties: house with house bodyThe internal temperature Tc (K) @10kHz is 228, and the dielectric constantr(room temperature 20 ℃ C.) 0.10 kHz of 209 and a dielectric loss tan(room temperature 20 ℃) @10kHz 0.0161, dielectric tunabilityT15.5% at (30 kV/cm, 20 ℃) @10kHz, 2493% at the resonance frequency (MHz), and a dielectric constant at resonancer198 and Q values 446.
Claims (1)
1. The low-sintering ceramic material of the barium strontium titanate composite copper gallate with high adjustability and low loss is characterized in that the general formula of the low-sintering ceramic material of the barium strontium titanate composite copper gallate with high adjustability and low loss is as follows: (1-x) Ba0.4Sr0.6TiO3-xCuGa2O4Wherein the value range of x is more than or equal to 5wt% and less than or equal to 90wt%, and the preparation method comprises the following steps:
(1) selecting BaTiO3Powder, SrTiO3Powder, CuO powder and Ga2O3The powder is used as main raw material according to (1-x) Ba0.4Sr0.6TiO3-xCuGa2O4Proportioning the Ba, Sr, Ti, Cu and Ga according to the stoichiometric ratio, putting the proportioned raw materials into a nylon ball milling tank, adding zirconia balls and ball milling media, carrying out ball milling, discharging, drying, presintering and grinding to obtain mixed powder 1; the temperature for pre-sintering is 1100-1200 ℃, and the sintering time is 4-6 hours;
(2) adding the mixed powder 1 in the step (1) into zirconia balls and absolute ethyl alcohol or deionized water for ball milling for 24-48 hours, discharging, drying and sieving to obtain mixed powder 2;
(3) adding the mixed powder 2 in the step (2) into a polyvinyl alcohol aqueous solution with the mass ratio of 7-10%, uniformly mixing, granulating, and pressing under the pressure of 10-100 MPa to prepare a ceramic green sheet;
(4) carrying out glue discharging treatment on the ceramic green sheet in the step (3) at the temperature of 550-600 ℃ for 4-10 hours; and after the binder is removed, sintering the mixture at the temperature of 1000-1050 ℃ for 4-6 hours to form ceramic, thus obtaining the low-sintering ceramic material of barium strontium titanate composite copper gallate with high adjustability and low loss.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110386815A (en) * | 2019-07-23 | 2019-10-29 | 山东理工大学 | A kind of compound zinc aluminate ceramic material of barium strontium titanate that can be practical with higher adjustable rate low-loss |
| CN110386816A (en) * | 2019-07-23 | 2019-10-29 | 山东理工大学 | A kind of high adjustable compound gallic acid zinc ceramic material of rate low-loss barium strontium titanate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110386815A (en) * | 2019-07-23 | 2019-10-29 | 山东理工大学 | A kind of compound zinc aluminate ceramic material of barium strontium titanate that can be practical with higher adjustable rate low-loss |
| CN110386816A (en) * | 2019-07-23 | 2019-10-29 | 山东理工大学 | A kind of high adjustable compound gallic acid zinc ceramic material of rate low-loss barium strontium titanate |
Non-Patent Citations (1)
| Title |
|---|
| WEI WANG等: "Enhanced dielectric properties in median-temperature sintered Ba0.4Sr0.6TiO3-CuGa2O4 composite ceramics", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 837, pages 1 - 7 * |
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