CN116606142A - Microwave dielectric ceramic and preparation method and application thereof - Google Patents
Microwave dielectric ceramic and preparation method and application thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 50
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 10
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims abstract description 10
- 238000004891 communication Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- 229920002994 synthetic fiber Polymers 0.000 claims description 5
- 235000015895 biscuits Nutrition 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
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- 230000001070 adhesive effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
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- 238000000748 compression moulding Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/20—Frequency-selective devices, e.g. filters
- H01P1/2002—Dielectric waveguide filters
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Abstract
The invention belongs to the technical field of ceramic materials, and provides a microwave dielectric ceramic, a preparation method and application thereof, wherein the microwave dielectric ceramic comprises a main material and auxiliary materials, and the main material comprises (1-x-y) MgNb 2 O 6 ‑xMgTiO 3 ‑yCa 1‑n Sm 2n/3 O 3 The auxiliary material comprises MnCO 3 And/or Al 2 O 3 Wherein x=0.01-0.1, y=0.01-0.2, n=0.1-1. The microwave dielectric ceramic provided by the invention has high quality factor and good temperature stability, realizes adjustable dielectric constant in a wider range (25-35), and can meet the manufacturing requirements of resonators and filters for high-frequency communication.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a microwave dielectric ceramic, a preparation method and application thereof.
Background
With the development of microwave communication technology to high frequency (millimeter wave), for example, the 5G communication frequency is 2-30GHz, the requirements of higher quality factors (Qf) are put forward for ceramic resonators and filters applied to the microwave communication technology, and meanwhile, the microwave communication technology has good temperature stability (the temperature coefficient of resonant frequency τf of near zero is less than +/-10 ppm/DEGC). And in order to meet the miniaturization of devices and the design requirements of different device sizes, ceramics are also required to have a high dielectric constant (K) and to be tunable over a wide range.
The traditional method for adjusting the temperature stability is to compound two materials with positive temperature coefficient and negative temperature coefficient. However, after the two materials are compounded, the dielectric constant is difficult to be adjusted within a wider range, so that the requirements of different designs (such as typical MgTiO with good temperature stability can not be met 3 -CaTiO 3 The dielectric constant of the system is only slightly adjustable between 19 and 21). Therefore, development of a microwave dielectric ceramic material having a high quality factor, temperature stability and a dielectric constant adjustable in a wide range is needed.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a microwave dielectric ceramic, and a preparation method and application thereof. The microwave dielectric ceramic provided by the invention not only has a high quality factor (Qf is not lower than 84600 and even can reach 104500), and has good temperature stability (τf is less than +/-9 ppm/DEG C), but also has an adjustable dielectric constant within a wider range of 25-35.
A first aspect of the present invention provides a microwave dielectric ceramic.
Specifically, the microwave dielectric ceramic comprises a main material and auxiliary materials, wherein the main material comprises (1-x-y) MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 The auxiliary material comprises MnCO 3 And/or Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.01-0.1, y=0.01-0.2, n=0.1-1.
The invention leads MgNb with negative temperature coefficient and ultra-high quality factor to be adopted 2 O 6 、MgTiO 3 And Ca having a positive temperature coefficient 1-n Sm 2n/3 O 3 The mixed system of the three is used as the main material of the microwave dielectric ceramic, and the three different microwave dielectric properties are utilized by the component compounding technology: the microwave dielectric ceramic with stable temperature, medium dielectric constant and high quality factor can be obtained by the mixing rule of dielectric constants, the parallel model of quality factors and the superposition effect of resonant frequency, and the dielectric constant can be adjusted in a wider range (25-35), so that the manufacturing requirements of resonators and filters for high-frequency communication can be met.
Preferably, x=0.03-0.06, y=0.05-0.15, n=0.3-0.5. x, y and n are all molar ratios.
Further preferably, the x=0.03-0.06, y=0.05-0.15, n=0.35-0.45.
Preferably, the auxiliary material comprises MnCO accounting for 0.1-1wt% of the total mass of the main material 3 And 0.05 to 0.5wt% Al 2 O 3 。
Further preferably, the auxiliary material comprises MnCO accounting for 0.2 to 0.5 weight percent of the total mass of the main material 3 And 0.05 to 0.2wt% Al 2 O 3 。
Preferably, the main material comprises the following raw materials: mgNb 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/3 O 3 。
The second aspect of the invention provides a method for preparing the microwave dielectric ceramic.
A preparation method of microwave dielectric ceramic comprises the following steps:
mixing the main materials and the auxiliary materials, granulating, pressing and forming to obtain a ceramic biscuit, discharging glue, and sintering to obtain the microwave dielectric ceramic.
Preferably, the main material and the auxiliary material are mixed and then ground.
Preferably, the granulating is carried out by mixing the main material and the auxiliary material, adding the adhesive and granulating.
Preferably, the binder is polyvinyl alcohol (PVA).
Preferably, the pressure of the compression molding is 160-300MPa.
Preferably, the sintering temperature is 1400-1500 ℃, and the sintering time is 3-8 hours.
Preferably, the main material comprises the following raw materials: mgO, nb 2 O 5 、TiO 2 、CaCO 3 And Sm 2 O 3 。
Preferably, the preparation method of the main material comprises the following steps:
(1) Taking MgO and Nb 2 O 5 、TiO 2 、CaCO 3 And Sm 2 O 3 Raw materials respectively according to MgNb 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/3 O 3 Is prepared by mixing, grinding, drying and calcining the above materials according to the chemical formula to obtain MgNb respectively 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/3 O 3 Three synthetic materials;
(2) The three synthetic materials prepared in the step (1) are mixed according to (1-x-y) MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 (wherein x=0.03-0.06 and y=0.05-0.15 are molar ratios) to obtain the main material.
Preferably, in step (1), the milling time is 12-24 hours.
Preferably, in the step (1), mgNb is obtained by calcining at 1200-1300 ℃ for 3-7 hours 2 O 6 The method comprises the steps of carrying out a first treatment on the surface of the Calcining at 1100-1200 deg.c for 2-6 hr to obtain MgTiO 3 The method comprises the steps of carrying out a first treatment on the surface of the Calcining at 1150-1250 deg.c for 2-6 hr to obtain Ca 1-n Sm 2n/3 O 3 。
The third aspect of the invention provides an application of the microwave dielectric ceramic.
An application of microwave dielectric ceramics in the field of microwave communication.
Compared with the prior art, the invention has the following beneficial effects:
the microwave dielectric ceramic provided by the invention comprises a main material and auxiliary materials, wherein the main material comprises (1-x-y) MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 The auxiliary material comprises MnCO 3 And/or Al 2 O 3 Wherein x=0.01-0.1, y=0.01-0.2, n=0.1-1. The main material adopted by the invention is MgNb 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/3 O 3 (n=0.35-0.45) and adopting MnCO at the same time 3 And/or Al 2 O 3 As auxiliary materials, the microwave dielectric ceramic provided by the invention has high quality factor (Qf is not lower than 84600 and even can reach 104500), and has good temperature stability (τf<(+ -9 ppm/. Degree.C.) in a broader rangeThe dielectric constant (dielectric constant is 25-35) is adjustable in the range. The microwave dielectric ceramic provided by the invention can meet the manufacturing requirements of resonators and filters for high-frequency communication.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
Example 1
A microwave dielectric ceramic comprises main materials and auxiliary materials, wherein the main materials comprise (1-x-y) MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 The auxiliary material comprises MnCO accounting for 0.25 weight percent of the total mass of the main material 3 And 0.2wt% of Al based on the total mass of the main material 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Where x=0.03, y=0.05, n=0.3.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) MgO, nb is selected 2 O 5 、TiO 2 、CaCO 3 And Sm 2 O 3 As raw materials, respectively according to MgNb 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/ 3 O 3 (wherein n=0.35-0.45) and then placing the mixture in a ball mill for grinding for 12-24 hours, and uniformly mixing;
(2) Drying MgO, nb 2 O 5 Calcining the two raw materials at 1200 ℃ for 6 hours to obtain MgNb 2 O 6 The method comprises the steps of carrying out a first treatment on the surface of the MgO, tiO 2 Calcining the two raw materials at 1150 ℃ for 4 hours to obtain MgTiO 3 The method comprises the steps of carrying out a first treatment on the surface of the CaCO is put into 3 And Sm 2 O 3 Calcining the two raw materials at 1200 ℃ for 3 hours to obtain Ca 1-n Sm 2n/3 O 3 ；
(3) To MgNb 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/3 O 3 Three synthetic materials, namely (1-x-y) MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 Is mixed according to the chemical proportion, and MnCO is added 3 And Al 2 O 3 Grinding and mixing again in a ball mill to obtain powder;
(4) Adding PVA accounting for 2% of the total mass of the powder into the powder, granulating, and then pressing and forming under 260MPa to obtain a ceramic biscuit;
(5) And (3) discharging the adhesive from the ceramic biscuit, and sintering at 1480 ℃ for 4 hours to obtain the microwave dielectric ceramic.
Examples 2 to 6
Examples 2-6 provide microwave dielectric ceramics, differing from example 1 in x, y, n, mnCO 3 Content of (2) and Al 2 O 3 Is different in content. See in particular table 1.
Comparative example 1
This comparative example provides a microwave dielectric ceramic, which is different from example 1 in that Sm 2 O 3 Bi is changed into 2 O 3 。
Product effect test
The microwave dielectric ceramics provided in the above examples were subjected to performance testing by using the test method of complex dielectric constant of solid dielectric microwave of GBT 5597-1999, and the test results are shown in the following table.
Table 1 parameters and performance test results for each example
As is clear from the above table, the dielectric constant (K) of the microwave dielectric ceramics prepared in examples 1-6 of the invention is adjustable between 25-35, the resonance frequency temperature is about zero (τf <.+ -. 10 ppm/. Degree.C), and the microwave dielectric ceramics have high quality factor (Qf > 80000). In contrast, the dielectric constant k=41.2, the quality factor qf= 34400, and the temperature coefficient of resonance frequency of +18ppm/°c of comparative example 1 cannot meet the application requirements of the high-frequency microwave communication device.
Claims (10)
1. The microwave dielectric ceramic is characterized by comprising a main material and auxiliary materials, wherein the main material comprises (1-x-y) MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 The auxiliary material comprises MnCO 3 And/or Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.01-0.1, y=0.01-0.2, n=0.1-1.
2. The microwave dielectric ceramic of claim 1, wherein x = 0.03-0.06, y = 0.05-0.15, and n = 0.3-0.5.
3. The microwave dielectric ceramic according to claim 1, wherein the auxiliary material comprises MnCO accounting for 0.1-1wt% of the total mass of the main material 3 And 0.05 to 0.5wt% Al 2 O 3 。
4. A method for preparing a microwave dielectric ceramic according to any one of claims 1 to 3, comprising the steps of:
mixing the main materials and the auxiliary materials, granulating, pressing and forming to obtain a ceramic biscuit, discharging glue, and sintering to obtain the microwave dielectric ceramic.
5. The method according to claim 4, wherein the pressure of the press molding is 160 to 300MPa.
6. The method according to claim 4, wherein the sintering temperature is 1400-1500 ℃ and the sintering time is 3-8 hours.
7. The preparation method according to claim 4, wherein the main materials comprise the following components: mgO, nb 2 O 5 、TiO 2 、CaCO 3 And Sm 2 O 3 。
8. The preparation method according to claim 7, wherein the preparation method of the main material comprises the steps of:
(1) Taking MgO and Nb 2 O 5 、TiO 2 、CaCO 3 And Sm 2 O 3 According to MgNb respectively 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/3 O 3 Is prepared by mixing, grinding, drying and calcining the above materials according to the chemical formula to obtain MgNb respectively 2 O 6 、MgTiO 3 And Ca 1-n Sm 2n/3 O 3 Three synthetic materials;
(2) The three synthetic materials prepared in the step (1) are mixed according to (1-x-y) MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 Is mixed according to the chemical formula to obtain the main material.
9. The process according to claim 8, wherein in the step (1), mgNb is obtained by calcining at 1200 to 1300℃for 3 to 7 hours 2 O 6 The method comprises the steps of carrying out a first treatment on the surface of the Calcining at 1100-1200 deg.c for 2-6 hr to obtain MgTiO 3 The method comprises the steps of carrying out a first treatment on the surface of the Calcining at 1150-1250 deg.c for 2-6 hr to obtain Ca 1-n Sm 2n/3 O 3 。
10. Use of a microwave dielectric ceramic according to any one of claims 1-3 in the field of microwave communications.
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Citations (7)
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| JP2002326865A (en) * | 2001-04-27 | 2002-11-12 | Matsushita Electric Ind Co Ltd | Dielectric porcelain composition and dielectric device |
| US20030132820A1 (en) * | 2002-01-17 | 2003-07-17 | Khosro Shamsaifar | Electronically tunable combline filter with asymmetric response |
| WO2009070047A1 (en) * | 2007-11-26 | 2009-06-04 | Elizaveta Arkadievna Nenasheva | Low dielectric loss ceramic ferroelectric composite material |
| CN102044730A (en) * | 2010-12-06 | 2011-05-04 | 武汉凡谷电子技术股份有限公司 | Transverse magnetic (TM) mode dielectric filter |
| CN110668795A (en) * | 2019-11-15 | 2020-01-10 | 山东国瓷功能材料股份有限公司 | Microwave dielectric ceramic material, preparation method and application thereof, microwave dielectric ceramic body, preparation method and application thereof, and microwave device |
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| JPS61251563A (en) * | 1985-04-30 | 1986-11-08 | マルコン電子株式会社 | High permittivity ceramic composition |
| CN1189480A (en) * | 1997-01-23 | 1998-08-05 | 阿莫同有限公司 | Dielectric ceramic compositions |
| JP2002326865A (en) * | 2001-04-27 | 2002-11-12 | Matsushita Electric Ind Co Ltd | Dielectric porcelain composition and dielectric device |
| US20030132820A1 (en) * | 2002-01-17 | 2003-07-17 | Khosro Shamsaifar | Electronically tunable combline filter with asymmetric response |
| WO2009070047A1 (en) * | 2007-11-26 | 2009-06-04 | Elizaveta Arkadievna Nenasheva | Low dielectric loss ceramic ferroelectric composite material |
| CN102044730A (en) * | 2010-12-06 | 2011-05-04 | 武汉凡谷电子技术股份有限公司 | Transverse magnetic (TM) mode dielectric filter |
| CN110668795A (en) * | 2019-11-15 | 2020-01-10 | 山东国瓷功能材料股份有限公司 | Microwave dielectric ceramic material, preparation method and application thereof, microwave dielectric ceramic body, preparation method and application thereof, and microwave device |
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