CN113896524B - High-temperature stable low-dielectric-constant microwave dielectric ceramic and preparation method thereof - Google Patents
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- 239000000843 powder Substances 0.000 claims description 39
- 238000000498 ball milling Methods 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 27
- 239000000758 substrate Substances 0.000 claims description 27
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- 239000011230 binding agent Substances 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
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- 239000001923 methylcellulose Substances 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
- 230000003000 nontoxic effect Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 14
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- SXSVTGQIXJXKJR-UHFFFAOYSA-N [Mg].[Ti] Chemical compound [Mg].[Ti] SXSVTGQIXJXKJR-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a high-temperature stable low-dielectric constant microwave dielectric ceramic, the composition expression of which is aMgSiO 3 ‑bMgTiO 3 ‑cZnTiO 3 ‑dLiNdTi 2 O 6 ‑eCaTiO 3 Wherein a, b, c, d and e each independently represent a mole percent and satisfy the following conditions: a is more than or equal to 10% and less than or equal to 20% by mol, b is more than or equal to 65% and less than or equal to 75% by mol, c is more than or equal to 2% and less than or equal to 10% by mol, d is more than or equal to 2% and less than or equal to 10% by mol, e is more than or equal to 5% and less than or equal to 10% by mol, and a+b+c+d+e=100% by mol. The invention also discloses a preparation method of the high-temperature stable low-dielectric constant microwave dielectric ceramic. The microwave dielectric ceramic has excellent microwave dielectric property, low sintering temperature, high Q value, zero adjustable frequency temperature coefficient, good temperature stability, nontoxic raw materials, low cost and simple preparation process.
Description
Technical Field
The invention belongs to the technical field of electronic ceramics and preparation thereof, and particularly relates to a high-temperature stable low-dielectric-constant microwave dielectric ceramic and a preparation method thereof.
Background
With recent decades of development, microwave dielectric ceramics have become a new type of functional ceramic material that performs one or more functions as a dielectric material in microwave frequency band circuits. Microwave dielectric properties are determining factors for microwave dielectric ceramic applications, while the relative dielectric constant ε r Quality factor Q x f and resonant frequency temperature coefficient tau f Is three main parameters of microwave dielectric properties.
With the rapid development of the 5G mobile communication system industry, microwave components, particularly filters and resonators, are receiving a great deal of attention from researchers as important devices in communication equipment. In order to further improve the performance of microwave components and adapt to higher and higher communication frequency in the communication field, the requirements on microwave dielectric materials mainly comprise the following points: (1) Low dielectric constant epsilon r The method comprises the steps of carrying out a first treatment on the surface of the (2) a quality factor Q x f as high as possible; (3) Near zero resonant frequency temperature coefficient τ f The method comprises the steps of carrying out a first treatment on the surface of the And (4) the selected materials are low in price, nontoxic and environment-friendly. From now on 5G-In view of the requirements in the 6G communication field, the low-dielectric-constant microwave dielectric ceramic most suitable for the requirements generally refers to a microwave dielectric material with a dielectric constant of 20±1.
At present, in a microwave dielectric material system with a low dielectric constant of 20+/-1, a magnesium-titanium system is studied more, but due to the fact that the pure magnesium-titanium system has a large negative temperature coefficient, a product with a very good temperature coefficient and a high Q value cannot be obtained all the time.
Therefore, how to improve the microwave dielectric performance and obtain the microwave dielectric ceramics with high Q value and near zero adjustable frequency temperature coefficient is a technical problem to be solved in an important way.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a high-temperature stable low-dielectric-constant microwave dielectric ceramic and a preparation method thereof; the microwave dielectric ceramic has excellent microwave dielectric property, low sintering temperature, high Q value, zero adjustable frequency temperature coefficient, good temperature stability, nontoxic raw materials, low cost and simple preparation process.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
a high-temperature stable low-dielectric constant microwave dielectric ceramic has the composition expression of aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 Wherein a, b, c, d and e each independently represent a mole percent and satisfy the following conditions: a is more than or equal to 10% and less than or equal to 20% by mol, b is more than or equal to 65% and less than or equal to 75% by mol, c is more than or equal to 2% and less than or equal to 10% by mol, d is more than or equal to 2% and less than or equal to 10% by mol, e is more than or equal to 5% and less than or equal to 10% by mol, and a+b+c+d+e=100% by mol.
As a preferred embodiment of the present invention, in the composition expression, a=15 mol%, b=70 mol%, c=5 mol%, d=5 mol%, and e=5 mol%.
Further, the relative dielectric constant of the microwave dielectric ceramic is 19-21, the Q multiplied by f value is more than 60000GHz, and the temperature coefficient of resonance frequency is within +/-3 ppm/DEG C.
The invention further provides a preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic, which comprises the following steps:
(1) According to the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 The mol percent of each element is respectively weighed MgO and SiO 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for heat preservation and presintering to obtain a powder substrate;
wherein, in the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 Wherein a, b, c, d and e each independently represent a mole percent and satisfy the following conditions: a is more than or equal to 10mol% and less than or equal to 20mol%, b is more than or equal to 65mol% and less than or equal to 75mol%, c is more than or equal to 2mol% and less than or equal to 10mol%, d is more than or equal to 2mol% and less than or equal to 10mol%, e is more than or equal to 5mol% and less than or equal to 10mol%, and a+b+c+d+e=100 mol%;
(2) Fully ball-milling the powder substrate obtained in the step (1), and drying, granulating and sieving the ball-milled powder substrate;
(3) And (3) pressing and forming the mixed powder processed in the step (2), and finally sintering to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
As a preferred technical scheme of the preparation method of the invention, the method has the following formula aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=15 mol%, b=70 mol%, c=5 mol%, d=5 mol%, e=5 mol%.
Further, the heat preservation presintering process in the step (1) is to bake for 3-5 hours at 1000-1200 ℃.
Further, the sintering process in the step (3) is to sinter at 1300-1360 ℃ for 3-5 h.
Further, the granulation in the step (2) is to mix the dried powder with a binder and then prepare micron-sized spherical particles.
Further preferably, the binder is selected from at least one of a polyvinyl alcohol solution, a polyvinyl butyral solution, an acrylic acid solution, or methylcellulose.
Further, in the step (3), the mixed powder was pressed into a cylinder having a diameter of 10mm and a height of 6 mm.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts MgTiO 3 As the base phase material, caTiO is used 3 、MgSiO 3 、ZnTiO 3 、LiNdTi 2 O 6 The four auxiliary materials act simultaneously to play a role in temperature coefficient modulation and as ZnTiO 3 And LiNdTi 2 O 6 The phases are low-temperature firing phases, the sintering temperature can be effectively reduced, and meanwhile, a higher Q value can be obtained, particularly, the temperature coefficient of the resonant frequency of an adjustable material is realized, the Q multiplied by f value of the obtained microwave dielectric ceramic reaches more than 60000GHz, and the temperature coefficient of the resonant frequency is within +/-3 ppm/DEG C. The microwave dielectric ceramic has excellent microwave dielectric property, ensures lower sintering temperature, has higher Q value and near-zero adjustable frequency temperature coefficient, has good temperature stability, is nontoxic in preparation raw materials, low in price and simple in preparation process, and has wide application prospect in the fields of 5G communication and future 6G communication.
Detailed Description
The following description of the embodiments of the present invention will be made more apparent and fully by reference to the accompanying drawings, in which it is shown, by way of illustration, only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a high-temperature stable low-dielectric constant microwave dielectric ceramic, the composition expression of which is aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 Wherein a, b, c, d and e each independently represent a mole percentage and satisfy the followingConditions are as follows: a is more than or equal to 10% and less than or equal to 20% by mol, b is more than or equal to 65% and less than or equal to 75% by mol, c is more than or equal to 2% and less than or equal to 10% by mol, d is more than or equal to 2% and less than or equal to 10% by mol, e is more than or equal to 5% and less than or equal to 10% by mol, and a+b+c+d+e=100% by mol.
In the above composition expression, a=15 mol%, b=70 mol%, c=5 mol%, d=5 mol%, and e=5 mol% are preferable.
The relative dielectric constant of the microwave dielectric ceramic is 19-21, the Q multiplied by f value is more than 60000GHz, and the temperature coefficient of resonance frequency is within +/-3 ppm/DEG C.
The invention further provides a preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic, which comprises the following steps:
(1) According to the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 The mol percent of each element is respectively weighed MgO and SiO 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for heat preservation and presintering to obtain a powder substrate;
wherein, in the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 Wherein a, b, c, d and e each independently represent a mole percent and satisfy the following conditions: a is more than or equal to 10mol% and less than or equal to 20mol%, b is more than or equal to 65mol% and less than or equal to 75mol%, c is more than or equal to 2mol% and less than or equal to 10mol%, d is more than or equal to 2mol% and less than or equal to 10mol%, e is more than or equal to 5mol% and less than or equal to 10mol%, and a+b+c+d+e=100 mol%;
(2) Fully ball-milling the powder substrate obtained in the step (1), and drying, granulating and sieving the ball-milled powder substrate;
(3) And (3) pressing and forming the mixed powder processed in the step (2), and finally sintering to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
In the composition expression of the above method, a=15 mol%, b=70 mol%, c=5 mol%, d=5 mol%, e=5 mol% are preferable.
Wherein, the heat preservation presintering process in the step (1) is roasting for 3-5 h at 1000-1200 ℃.
Wherein the sintering process in the step (3) is to sinter for 3-5 hours at 1300-1360 ℃.
Wherein, the granulation in the step (2) is to mix the dried powder with a binder and then prepare micron-sized spherical particles; the binder is preferably at least one of a polyvinyl alcohol solution, a polyvinyl butyral solution, an acrylic acid solution, or methylcellulose.
Wherein in the step (3), the mixed powder is pressed into a cylinder with the diameter of 10mm and the height of 6 mm.
The following examples will illustrate the invention further, but are not intended to limit it.
Example 1
The high temperature stable low dielectric constant microwave dielectric ceramic of example 1 has the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=10mol%, b=75mol%, c=5mol%, d=5mol%, and e=5mol%.
The preparation method of the high-temperature stable low-dielectric constant microwave dielectric ceramic of the embodiment 1 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1300 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 1 was tested for its microwave dielectric properties by a microwave network analyzer, and the results of the performance tests are shown in table 1.
Example 2
The high temperature stable low dielectric constant microwave dielectric ceramic of example 2 has the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=10mol%, b=75mol%, c=2mol%, d=3mol%, and e=10mol%.
The preparation method of the high-temperature stable low-dielectric constant microwave dielectric ceramic in the embodiment 2 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1320 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 2 was tested for its microwave dielectric properties by a microwave network analyzer, and the results of the performance tests are shown in table 1.
Example 3
The high temperature stable low dielectric constant microwave dielectric ceramic of example 3 has the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In which a=15 mol%, b=70 mol%, c=5 mol%,d＝5mol％，e＝5mol％。
the preparation method of the high-temperature stable low-dielectric constant microwave dielectric ceramic in the embodiment 3 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 3 was tested for its microwave dielectric properties by a microwave network analyzer, and the results of the performance tests are shown in table 1.
Example 4
The high temperature stable low dielectric constant microwave dielectric ceramic of example 4 has the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=15 mol%, b=70 mol%, c=2 mol%, d=3 mol%, e=10 mol%.
The preparation method of the high-temperature stable low-dielectric constant microwave dielectric ceramic in the embodiment 4 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Mixing the materials, ball milling, oven drying, sieving, and placing into corundum crucible at 1100deg.CPreserving heat and presintering for 3 hours to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1320 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 4 was tested for its microwave dielectric properties by a microwave network analyzer, and the results of the performance tests are shown in table 1.
Example 5
The high temperature stable low dielectric constant microwave dielectric ceramic of example 5 has the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=20 mol%, b=65 mol%, c=2 mol%, d=3 mol%, and e=10 mol%.
The preparation method of the high-temperature stable low-dielectric constant microwave dielectric ceramic in the embodiment 5 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1300 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 5 was tested for its microwave dielectric properties by a microwave network analyzer, and the results of the performance tests are shown in table 1.
The following 4 comparative examples were designed to compare with examples 1-5 of the present invention.
Comparative example 1
In the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=0 mol%, b=70 mol%, c=10 mol%, d=10 mol%, and e=10 mol%.
The preparation method of the microwave dielectric ceramic of the comparative example 1 comprises the following steps:
(1) MgO and CaCO are respectively weighed according to the mole percentage of each element in the composition expression 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in comparative example 1 was tested for microwave dielectric properties by using a microwave network analyzer, and the results of the performance tests are shown in table 1.
Comparative example 2
In the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=10mol%, b=70mol%, c=0mol%, d=10mol%, and e=10mol%.
The preparation method of the microwave dielectric ceramic of the comparative example 2 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、CaCO 3 、Li 2 CO 3 、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in comparative example 2 was tested for microwave dielectric properties by using a microwave network analyzer, and the results of the performance tests are shown in table 1.
Comparative example 3
In the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=10mol%, b=70mol%, c=10mol%, d=0mol%, and e=10mol%.
The preparation method of the microwave dielectric ceramic of the comparative example 3 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、CaCO 3 、ZnO、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in comparative example 3 was tested for microwave dielectric properties by using a microwave network analyzer, and the results of the performance tests are shown in table 1.
Comparative example 4
In the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=10mol%, b=70mol%, c=10mol%, d=10mol%, and e=0mol%.
The preparation method of the microwave dielectric ceramic of the comparative example 4 comprises the following steps:
(1) MgO and SiO are respectively weighed according to the mole percentage of each element in the composition expression 2 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for presintering for 3 hours at 1100 ℃ to obtain a powder substrate;
(2) Fully ball-milling the powder substrate obtained in the step (1), and then drying, granulating and sieving; wherein, the granulation is to mix the dried powder with polyvinyl alcohol solution and then prepare micron-sized spherical particles;
(3) And (3) pressing the mixed powder processed in the step (2) into a cylinder with the diameter of 10mm and the height of 6mm, and finally, carrying out heat preservation and sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in comparative example 4 was tested for microwave dielectric properties by using a microwave network analyzer, and the results of the performance tests are shown in table 1.
TABLE 1
As can be seen from Table 1, the microwave dielectric ceramics of examples 1 to 5 of the present invention have both a higher Q value and a near-zero tunable frequency temperature coefficient while ensuring a lower sintering temperature, and have better temperature stability, compared with the microwave dielectric ceramics of comparative examples 1 to 4. Among them, the microwave dielectric composite properties of the microwave dielectric ceramic of example 3 were relatively optimal.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all modifications or equivalent arrangements using the teachings of this invention, or direct or indirect application in other related arts, are included within the scope of this invention.
Claims (10)
1. A high temperature stable low dielectric constant microwave dielectric ceramic is characterized in that: the composition expression is aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 Wherein a, b, c, d and e each independently represent a mole percent and satisfy the following conditions: a is more than or equal to 10% and less than or equal to 20% by mol, b is more than or equal to 65% and less than or equal to 75% by mol, c is more than or equal to 2% and less than or equal to 10% by mol, d is more than or equal to 2% and less than or equal to 10% by mol, e is more than or equal to 5% and less than or equal to 10% by mol, and a+b+c+d+e=100% by mol.
2. The high temperature stable low dielectric constant microwave dielectric ceramic of claim 1, wherein: in this composition expression, a=15 mol%, b=70 mol%, c=5 mol%, d=5 mol%, e=5 mol%.
3. The high temperature stable low dielectric constant microwave dielectric ceramic of claim 1, wherein: the relative dielectric constant of the microwave dielectric ceramic is 19-21, the Q multiplied by f value is more than 60000GHz, and the temperature coefficient of resonance frequency is within +/-3 ppm/DEG C.
4. The preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic is characterized by comprising the following steps of:
(1) According to groupAdult expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 The mol percent of each element is respectively weighed MgO and SiO 2 、CaCO 3 、Li 2 CO 3 、ZnO、Nd 2 O 3 、TiO 2 Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then placing the materials into a corundum crucible for heat preservation and presintering to obtain a powder substrate;
wherein, in the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 Wherein a, b, c, d and e each independently represent a mole percent and satisfy the following conditions: a is more than or equal to 10mol% and less than or equal to 20mol%, b is more than or equal to 65mol% and less than or equal to 75mol%, c is more than or equal to 2mol% and less than or equal to 10mol%, d is more than or equal to 2mol% and less than or equal to 10mol%, e is more than or equal to 5mol% and less than or equal to 10mol%, and a+b+c+d+e=100 mol%;
(2) Fully ball-milling the powder substrate obtained in the step (1), and drying, granulating and sieving the ball-milled powder substrate;
(3) And (3) pressing and forming the mixed powder processed in the step (2), and finally sintering to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
5. The method for preparing a high temperature stable low dielectric constant microwave dielectric ceramic according to claim 4, wherein,
in the composition expression aMgSiO 3 -bMgTiO 3 -cZnTiO 3 -dLiNdTi 2 O 6 -eCaTiO 3 In a=15 mol%, b=70 mol%, c=5 mol%, d=5 mol%, e=5 mol%.
6. The method for preparing a high temperature stable low dielectric constant microwave dielectric ceramic according to claim 4, wherein the heat preservation presintering process in the step (1) is roasting for 3-5 hours at 1000-1200 ℃.
7. The method of preparing a high temperature stable low dielectric constant microwave dielectric ceramic according to claim 4, wherein the sintering process in step (3) is sintering at 1300-1360 ℃ for 3-5 h.
8. The method of preparing a high temperature stable low dielectric constant microwave dielectric ceramic according to claim 4, wherein the granulating in step (2) is to mix the dried powder with a binder and then prepare micron-sized spherical particles.
9. The method for preparing a high temperature stable low dielectric constant microwave dielectric ceramic according to claim 8, wherein the binder is at least one selected from the group consisting of polyvinyl alcohol solution, polyvinyl butyral solution, acrylic acid solution and methylcellulose.
10. The method of producing a high temperature stable low dielectric constant microwave dielectric ceramic according to claim 4, wherein in the step (3), the mixed powder is pressed into a cylinder having a diameter of 10mm and a height of 6 mm.
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