CN108840666B - Low-temperature sintered microwave dielectric ceramic material and preparation method thereof - Google Patents
Low-temperature sintered microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- CN108840666B CN108840666B CN201810812107.4A CN201810812107A CN108840666B CN 108840666 B CN108840666 B CN 108840666B CN 201810812107 A CN201810812107 A CN 201810812107A CN 108840666 B CN108840666 B CN 108840666B
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention belongs to the field of functional ceramics, and particularly relates to a low-temperature sintered microwave dielectric ceramic material and a preparation method thereof. Chemical composition BiW0.5Te3O12The low-temperature sintered microwave dielectric ceramic material has the advantages of ultralow sintering temperature (480-530 ℃), low dielectric constant (26-30), high quality factor (6,754-13, 120GHz), and negative frequency temperature coefficient (-86-197 × 10)‑6/° c), can be used for MLCC compensation type substrate materials, has good commercial value, and can be used for MLCC compensation type substrate materials; the invention also provides a preparation method thereof, which has simple process, no pollution in the process, suitability for industrial production and wide application prospect.
Description
Technical Field
The invention belongs to the field of functional ceramics, and particularly relates to a low-temperature sintered microwave dielectric ceramic material and a preparation method thereof.
Background
With the further expansion of the operating frequency of the communication equipment to the high-frequency range, particularly after the communication equipment enters a millimeter wave band, the dielectric loss of the material is obviously increased, the signal transmission delay time is longer (the signal delay time is in direct proportion to the dielectric constant), and the signal attenuation problem is prominent (the dielectric loss is large, the Qf is low, and the signal attenuation is large). The development of microwave dielectric ceramics with low dielectric constant and high Qf value is of great significance. In addition, with the development of microwave devices with high frequency, miniaturization, multifunction, high reliability and low cost, LTCC technology is becoming the first choice for high frequency substrate and integrated device applications.
According to the structure, performance characteristics and use requirements of LTCC, microwave dielectric ceramics for LTCC are mainly divided into two categories of LTCC substrate/packaging materials and microwave component materials for LTCC. The LTCC substrate material should have low sintering temperature, low dielectric constant, low dielectric loss, high insulation resistance, etc. The research difficulty of the substrate material is large, the core technology of the material research of various foreign companies is confidential, the research of the substrate material at home is in the starting stage, and the research of the related material and the preparation technology has a gap compared with the foreign technology. The LTCC substrate materials currently used are mainly glass ceramics and glass ceramics, such as BaO-SiO of Murata2-Al2O36.1, Qf 1500 GHz; 951 (Al) by Dupont2O3+CaZrO3+ glass) at 7.8, Qf 900 GHz; NEC Co LtdMLS-25 (Al)2O3-B2O3-SiO2) It was 4.7 and Qf was 720 GHz. One limitation of these materials is the small Qf value and the large dielectric losses.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a low-temperature sintering microwave dielectric ceramic material which has the advantages of ultralow sintering temperature, high Qf value, low dielectric constant and negative frequency temperature coefficient and can be used for MLCC compensation type substrate materials; the invention also provides a preparation method thereof, which has simple process, no pollution in the process, suitability for industrial production and wide application prospect.
The low-temperature sintered microwave dielectric ceramic material has the chemical composition of BiW0.5Te3O12。
The preparation method of the low-temperature sintered microwave dielectric ceramic material comprises the following steps:
(1) the raw material Bi2O3、WO3、TeO2Respectively according to BiW0.5Te3O12Weighing and proportioning by a chemical formula;
(2) mixing all the raw materials, putting the mixture into a ball milling tank, carrying out ball milling, drying the ball-milled raw materials, and sieving;
(3) calcining the powder obtained in the step (2) at 400 +/-10 ℃;
(4) adding a PVA aqueous solution into the calcined powder in the step (3) for granulation, drying, sieving, and pressing into a cylindrical shape by using a powder tablet press;
(5) and (4) sintering the cylinder obtained in the step (4) at 480-530 ℃, and preserving heat to obtain the low-temperature sintered microwave dielectric ceramic material.
Wherein:
the purity of the used raw materials is more than 99.9 percent.
And (3) in the step (2), the ball milling time is 4-6 hours, and the sieving is carried out by a sieve of 80 meshes.
The calcination time in the step (3) is 3 +/-0.1 hours.
The PVA aqueous solution in the step (4) is a PVA aqueous solution with the mass fraction of 5%.
The cylinder in the step (4) is a cylinder with phi 12mm multiplied by 6 mm.
And (4) the pressure of the powder tablet press in the step (4) is 8-12 MPa.
And (5) keeping the temperature for 2-4 hours.
And testing the prepared low-temperature sintered microwave dielectric ceramic material by using a tester, wherein the tester is a network analyzer.
As a most preferred technical scheme, the preparation method of the low-temperature sintering microwave dielectric ceramic material comprises the following steps:
(1) adding Bi2O3、WO3、TeO2Weighing the ingredients according to the mol ratio of 1:0.5:3 respectively, mixing, adding the raw materials into a nylon tank, and carrying out ball milling for 6 hours; placing the ball-milled raw materials in an infrared drying oven for drying and sieving;
(2) calcining the sieved raw materials at 400 ℃ for 3 hours;
(3) adding 5% PVA water solution by mass into the calcined powder for granulation, drying, sieving, and pressing into a cylinder with the diameter of 12mm multiplied by 6mm by a powder tablet press;
(4) sintering the cylinder in the step (3) at 520 ℃, and preserving heat for 4 hours to prepare ultralow-temperature sintered microwave dielectric ceramic;
(5) and (4) testing the microwave dielectric property of the microwave dielectric ceramic prepared in the step (4).
The microwave dielectric property is as follows: 29.1pC/N, Qf 13,120GHz,. tauf＝-197×10-6/℃。
Compared with the prior art, the invention has the following advantages:
(1) the low-temperature sintered microwave dielectric ceramic material is a microwave dielectric ceramic with high Qf value and low dielectric constant.
(2) The low-temperature sintering microwave dielectric ceramic material has the advantages of ultralow sintering temperature (480-530 ℃), low dielectric constant (26-30), high quality factor (6,754-13, 120GHz), and negative frequency temperature coefficient (-86-197 × 10)-6/° c) can be used for MLCC compensation type substrate materials, and has good commercial value.
(3) The low-temperature sintered microwave dielectric ceramic material has excellent microwave dielectric property and can meet the application of the microwave dielectric ceramic in the LTCC technology.
(4) The invention also provides a preparation method thereof, which has simple process, no pollution in the process, suitability for industrial production and wide application prospect.
Detailed Description
The present invention will be further described with reference to the following examples.
Examples 1 to 8
Chemical raw material Bi with purity of more than 99.9 percent is adopted2O3、WO3、TeO2Preparation BiW0.5Te3O12The microwave dielectric ceramic has the following specific embodiment:
(1) adding Bi2O3、WO3、TeO2Respectively weighing the ingredients according to the mol ratio of 1:0.5:3, and specifically weighing 3.9908 g of Bi2O31.9856 g WO39.0236 g TeO2After mixing, adding the raw materials into a nylon tank, and carrying out ball milling for 4-6 hours, wherein the specific ball milling time of the examples 1-8 is shown in Table 1; placing the ball-milled raw materials in an infrared drying oven for drying and sieving;
(2) calcining the sieved raw materials at 400 ℃ for 3 hours;
(3) adding 5% PVA water solution by mass into the calcined powder for granulation, drying, sieving, and pressing into a cylinder with the diameter of 12mm multiplied by 6mm by a powder tablet press;
(4) sintering the cylinder in the step (3) at 480-530 ℃, and preserving heat for 2-4 hours, wherein the specific sintering temperature and time of the embodiment 1-8 are shown in the table 1, so as to prepare the low-temperature sintering microwave dielectric ceramic;
(5) and (4) testing the microwave dielectric property of the low-temperature sintered microwave dielectric ceramic material prepared in the step (4).
The results of the measurements of the relevant process parameters and microwave dielectric properties for examples 1-8 are detailed in Table 1.
The detection method of embodiments 1 to 8 of the present invention is as follows:
1. the dielectric constant of the low-temperature sintering microwave dielectric ceramic material prepared in the embodiment 1-8 is measured by an open cavity parallel plate method by means of an Agilent 8720ES network analyzer, a test fixture is placed in a high-low temperature box to measure the temperature coefficient of the resonant frequency, the temperature range is 25-85 ℃, and the test frequency is within the range of 6.8-7.6 GHz.
2. The quality factor of the low-temperature sintering microwave dielectric ceramic material prepared in the examples 1-8 is measured by a closed cavity method, and the test frequency is in the range of 7.3-8.6 GHz.
TABLE 1
Claims (7)
1. A low-temperature sintered microwave dielectric ceramic material is characterized in that: chemical composition BiW0.5Te3O12;
The preparation method of the low-temperature sintered microwave dielectric ceramic material comprises the following steps:
(1) the raw material Bi2O3、WO3、TeO2Respectively according to BiW0.5Te3O12Weighing and proportioning by a chemical formula;
(2) mixing all the raw materials, putting the mixture into a ball milling tank, carrying out ball milling, drying the ball-milled raw materials, and sieving;
(3) calcining the powder obtained in the step (2) at 400 +/-10 ℃;
(4) adding a PVA aqueous solution into the calcined powder in the step (3) for granulation, drying, sieving, and pressing into a cylindrical shape by using a powder tablet press;
(5) and (4) sintering the cylinder obtained in the step (4) at 480-530 ℃, and preserving heat to obtain the low-temperature sintered microwave dielectric ceramic material.
2. The method for preparing the low-temperature sintering microwave dielectric ceramic material as claimed in claim 1, wherein the method comprises the following steps: and (3) in the step (2), the ball milling time is 4-6 hours, and the sieving is carried out by a sieve of 80 meshes.
3. The method for preparing the low-temperature sintering microwave dielectric ceramic material as claimed in claim 2, wherein: the calcination time in the step (3) is 3 +/-0.1 hours.
4. The method for preparing the low-temperature sintering microwave dielectric ceramic material as claimed in claim 2, wherein: the PVA aqueous solution in the step (4) is a PVA aqueous solution with the mass fraction of 5%.
5. The method for preparing the low-temperature sintering microwave dielectric ceramic material as claimed in claim 2, wherein: the cylinder in the step (4) is a cylinder with phi 12mm multiplied by 6 mm.
6. The method for preparing the low-temperature sintering microwave dielectric ceramic material as claimed in claim 2, wherein: and (4) the pressure of the powder tablet press in the step (4) is 8-12 MPa.
7. The method for preparing the low-temperature sintering microwave dielectric ceramic material as claimed in claim 2, wherein: and (5) keeping the temperature for 2-4 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747059A (en) * | 2009-12-22 | 2010-06-23 | 上海大学 | Method for preparing low temperature co-fired microwave dielectric ceramic material |
| CN103496981A (en) * | 2013-09-26 | 2014-01-08 | 桂林理工大学 | Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof |
| CN104671782A (en) * | 2015-02-04 | 2015-06-03 | 桂林理工大学 | Low-loss ultralow dielectric constant microwave dielectric ceramic Bi2WO6 |
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- 2018-07-23 CN CN201810812107.4A patent/CN108840666B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747059A (en) * | 2009-12-22 | 2010-06-23 | 上海大学 | Method for preparing low temperature co-fired microwave dielectric ceramic material |
| CN103496981A (en) * | 2013-09-26 | 2014-01-08 | 桂林理工大学 | Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof |
| CN104671782A (en) * | 2015-02-04 | 2015-06-03 | 桂林理工大学 | Low-loss ultralow dielectric constant microwave dielectric ceramic Bi2WO6 |
Non-Patent Citations (2)
| Title |
|---|
| Bi2O3-TeO2系微波介质陶瓷烧结及其性能研究;姜善涛;《兵器材料科学与工程》;20150930;第38卷(第5期);第26-28页 * |
| 超低温烧结微波介质陶瓷研究进展;张高群等;《硅酸盐学报》;20170930;第45卷(第9期);第1256-1264页 * |
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