CN113896524A - High-temperature stable low-dielectric constant microwave dielectric ceramic and preparation method thereof - Google Patents
High-temperature stable low-dielectric constant microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims description 44
- 239000000843 powder Substances 0.000 claims description 40
- 238000000498 ball milling Methods 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 24
- 238000007873 sieving Methods 0.000 claims description 24
- 238000004321 preservation Methods 0.000 claims description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- 239000011812 mixed powder Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 239000012798 spherical particle Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 11
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 11
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 235000010981 methylcellulose Nutrition 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
- 238000005469 granulation Methods 0.000 description 11
- 230000003179 granulation Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 238000011056 performance test Methods 0.000 description 7
- 238000004891 communication Methods 0.000 description 6
- 239000003989 dielectric material Substances 0.000 description 4
- SXSVTGQIXJXKJR-UHFFFAOYSA-N [Mg].[Ti] Chemical compound [Mg].[Ti] SXSVTGQIXJXKJR-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
- 229910017676 MgTiO3 Inorganic materials 0.000 description 1
- 229910003122 ZnTiO3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052634 enstatite Inorganic materials 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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Abstract
The invention discloses a high-temperature stable low-dielectric constant microwave dielectric ceramic, the composition expression of which is aMgSiO3‑bMgTiO3‑cZnTiO3‑dLiNdTi2O6‑eCaTiO3Wherein a, b, c, d and e independently represent mole percentages, and satisfy the following conditions: a is more than or equal to 10 mol% and less than or equal to 20 mol%, b is more than or equal to 65 mol% and less than or equal to 75 mol%, c is more than or equal to 2 mol% and less than or equal to 10 mol%, d is more than or equal to 2 mol% and less than or equal to 10 mol%, e is more than or equal to 5 mol% and less than or equal to 10 mol%, and a + b + c + d + e is equal to 100 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, near-zero adjustable frequency temperature coefficient, good temperature stability, nontoxic preparation raw materials, low price 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 the development of recent decades, microwave dielectric ceramics have become a new type of functional ceramic material, which can perform one or more functions as a dielectric material in microwave frequency circuit. The dielectric property of microwave is a determining factor of microwave dielectric ceramic application, and the relative dielectric constant epsilonrQuality factor Qxf and resonant frequency temperature coefficient taufAre three main parameters of microwave dielectric performance.
With the rapid development of the 5G mobile communication system industry, microwave components, in particular, filters and resonators, have received much attention from researchers as important components in communication equipment. In order to further improve the performance of microwave components and adapt to higher and higher communication frequencies in the communication field, the requirements on the microwave dielectric material mainly include the following points: (1) low dielectric constant epsilonr(ii) a (2) A quality factor Qxf as high as possible; (3) near zero temperature coefficient of resonance frequencyf(ii) a (4) The selected material is cheap, non-toxic and environment-friendly. In view of the current requirements in the 5G-6G communication field, the most suitable microwave dielectric ceramic with low dielectric constant is generally a microwave dielectric material with a dielectric constant of 20 + -1.
At present, in a low-dielectric-constant microwave dielectric material system with a dielectric constant of 20 +/-1, a magnesium-titanium system is researched more, but a product with a very good temperature coefficient and a high Q value cannot be obtained all the time due to the fact that a pure magnesium-titanium system has a large negative temperature coefficient.
Therefore, how to improve the microwave dielectric property and obtain the microwave dielectric ceramic with both high Q value and near-zero adjustable frequency temperature coefficient is a technical problem to be mainly solved.
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, near-zero adjustable frequency temperature coefficient, good temperature stability, nontoxic preparation raw materials, low price and simple preparation process.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a high-temperature stable low-dielectric constant microwave dielectric ceramic with the composition expression of aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3Wherein a, b, c, d ande independently represents the mole percentage and satisfies the following conditions: a is more than or equal to 10 mol% and less than or equal to 20 mol%, b is more than or equal to 65 mol% and less than or equal to 75 mol%, c is more than or equal to 2 mol% and less than or equal to 10 mol%, d is more than or equal to 2 mol% and less than or equal to 10 mol%, e is more than or equal to 5 mol% and less than or equal to 10 mol%, and a + b + c + d + e is equal to 100 mol%.
In a preferred embodiment of the present invention, in the formula, a is 15 mol%, b is 70 mol%, c is 5 mol%, d is 5 mol%, and e is 5 mol%.
Furthermore, the relative dielectric constant of the microwave dielectric ceramic is 19-21, the Qxf value is more than 60000GHz, and the temperature coefficient of the 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 aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3MgO and SiO are respectively weighed according to the mol percentage of each element2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible for heat preservation and presintering to obtain a powder base material;
wherein, the composition expression is aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3Wherein a, b, c, d and e each independently represent a mole percentage, and satisfy the following condition: a is more than or equal to 10 mol% and less than or equal to 20 mol%, b is more than or equal to 65 mol% and less than or equal to 75 mol%, c is more than or equal to 2 mol% and less than or equal to 10 mol%, d is more than or equal to 2 mol% and less than or equal to 10 mol%, e is more than or equal to 5 mol% and less than or equal to 10 mol%, and a + b + c + d + e is equal to 100 mol%;
(2) fully ball-milling the powder base material obtained in the step (1), and drying, granulating and sieving the ball-milled powder base material;
(3) and (3) pressing and forming the mixed powder treated 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, the composition expression of aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 15 mol%, b is 70 mol%, c is 5 mol%, d is 5 mol%, and e is 5 mol%.
Further, the heat-preservation pre-sintering process in the step (1) is roasting for 3-5 hours at 1000-1200 ℃.
Further, the sintering process in the step (3) is sintering 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 solution, or methyl cellulose.
Further, in the step (3), the mixed powder is pressed into a cylinder with 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 MgTiO3As a base phase material and CaTiO3、MgSiO3、ZnTiO3、LiNdTi2O6The four auxiliary phase materials act simultaneously to achieve the temperature coefficient modulation effect, and the ZnTiO material has the advantages of high temperature coefficient modulation effect3And LiNdti2O6The phases are low-temperature sintering phases, so that a higher Q value can be obtained while the sintering temperature is effectively reduced, particularly the resonance frequency temperature coefficient of an adjustable material is realized, the Q multiplied by f value of the obtained microwave dielectric ceramic reaches more than 60000GHz, and the resonance frequency temperature coefficient is within +/-3 ppm/DEG C. The microwave dielectric ceramic has excellent microwave dielectric property, has higher Q value and near-zero adjustable frequency temperature coefficient while ensuring lower sintering temperature, has good temperature stability, nontoxic preparation raw materials, low price and simple preparation process, and has wide application prospect in the field of 5G communication and future 6G communication.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a high-temperature stable low-dielectric constant microwave dielectric ceramic, the composition expression of which is aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3Wherein a, b, c, d and e independently represent mole percentages, and satisfy the following conditions: a is more than or equal to 10 mol% and less than or equal to 20 mol%, b is more than or equal to 65 mol% and less than or equal to 75 mol%, c is more than or equal to 2 mol% and less than or equal to 10 mol%, d is more than or equal to 2 mol% and less than or equal to 10 mol%, e is more than or equal to 5 mol% and less than or equal to 10 mol%, and a + b + c + d + e is equal to 100 mol%.
In the above-mentioned composition expression, it is preferable that a be 15 mol%, b be 70 mol%, c be 5 mol%, d be 5 mol%, and e be 5 mol%.
The microwave dielectric ceramic has a relative dielectric constant of 19-21, a Qxf value of more than 60000GHz, and a temperature coefficient of resonance frequency 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 aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3MgO and SiO are respectively weighed according to the mol percentage of each element2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible for heat preservation and presintering to obtain a powder base material;
wherein, the composition expression is aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3Wherein a, b, c, d and e each independently represent a mole percentage, and satisfy the following condition: a is more than or equal to 10 mol% and less than or equal to 20 mol%, b is more than or equal to 65 mol% and less than or equal to 75 mol%, c is more than or equal to 2 mol% and less than or equal to 10 mol%, d is more than or equal to 2 mol% and less than or equal to 10 mol%,5mol％≤e≤10mol％，a+b+c+d+e＝100mol％；
(2) fully ball-milling the powder base material obtained in the step (1), and drying, granulating and sieving the ball-milled powder base material;
(3) and (3) pressing and forming the mixed powder treated in the step (2), and finally sintering to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
In the composition formula of the above method, it is preferable that a is 15 mol%, b is 70 mol%, c is 5 mol%, d is 5 mol%, and e is 5 mol%.
Wherein, the heat preservation and pre-sintering process in the step (1) is roasting for 3-5 hours at 1000-1200 ℃.
Wherein, the sintering process in the step (3) is sintering at 1300-1360 ℃ for 3-5 h.
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 solution, or methyl cellulose.
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 further illustrate the invention but are not intended to limit the invention thereto.
Example 1
The composition of the high temperature stable low dielectric constant microwave dielectric ceramic of example 1 is represented by the formula aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 10 mol%, b is 75 mol%, c is 5 mol%, d is 5 mol%, and e is 5 mol%.
The preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic of embodiment 1 includes the following steps:
(1) MgO and SiO are respectively weighed according to the mol percentage of each element in the composition expression2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Mixing the weighed materials, ball millingGrinding, drying, sieving, and placing into a corundum crucible for heat preservation and presintering at 1100 deg.C for 3h to obtain powder base material;
(2) fully ball-milling the powder base material 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 sintering for 4 hours at the temperature of 1300 ℃ to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 1 was subjected to a microwave dielectric property test using a microwave network analyzer, and the results of the property test are shown in table 1.
Example 2
The composition of the high temperature stable low dielectric constant microwave dielectric ceramic of example 2 is represented by the formula aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 10 mol%, b is 75 mol%, c is 2 mol%, d is 3 mol%, and e is 10 mol%.
The preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic of embodiment 2 includes the following steps:
(1) MgO and SiO are respectively weighed according to the mol percentage of each element in the composition expression2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible to perform heat preservation and presintering for 3 hours at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering at the temperature of 1320 ℃ for 4h to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 2 was subjected to a microwave dielectric property test using a microwave network analyzer, and the results of the property test are shown in table 1.
Example 3
The composition of the high temperature stable low dielectric constant microwave dielectric ceramic of example 3 is represented by the formula aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 15 mol%, b is 70 mol%, c is 5 mol%, d is 5 mol%, and e is 5 mol%.
The preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic of embodiment 3 includes the following steps:
(1) MgO and SiO are respectively weighed according to the mol percentage of each element in the composition expression2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible to perform heat preservation and presintering for 3 hours at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 3 was subjected to a microwave dielectric property test using a microwave network analyzer, and the results of the property test are shown in table 1.
Example 4
The composition of the high temperature stable low dielectric constant microwave dielectric ceramic of example 4 is represented by the formula aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 15 mol%, b is 70 mol%, c is 2 mol%, d is 3 mol%, and e is 10 mol%.
The preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic of embodiment 4 includes the following steps:
(1) MgO and SiO are respectively weighed according to the mol percentage of each element in the composition expression2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible to perform heat preservation and presintering for 3 hours at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering at the temperature of 1320 ℃ for 4h to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 4 was subjected to a microwave dielectric property test using a microwave network analyzer, and the results of the property test are shown in table 1.
Example 5
The composition of the high temperature stable low dielectric constant microwave dielectric ceramic of example 5 is represented by the formula aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 20 mol%, b is 65 mol%, c is 2 mol%, d is 3 mol%, and e is 10 mol%.
The preparation method of the high-temperature stable low-dielectric-constant microwave dielectric ceramic of embodiment 5 includes the following steps:
(1) MgO and SiO are respectively weighed according to the mol percentage of each element in the composition expression2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Mixing the weighed materials sufficiently and then ballingGrinding, drying after ball milling, sieving, and then putting into a corundum crucible for heat preservation and presintering for 3h at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering for 4 hours at the temperature of 1300 ℃ to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in example 5 was subjected to a microwave dielectric property test using a microwave network analyzer, and the results of the property test are shown in table 1.
4 comparative examples are designed below for comparison with examples 1-5 of the present invention.
Comparative example 1
In the composition expression aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 0 mol%, b is 70 mol%, c is 10 mol%, d is 10 mol%, and e is 10 mol%.
The preparation method of the microwave dielectric ceramic of comparative example 1 comprises the following steps:
(1) MgO and CaCO are respectively weighed according to the mol percentage of each element in the composition expression3、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible to perform heat preservation and presintering for 3 hours at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in the comparative example 1 is subjected to microwave dielectric performance test by using a microwave network analyzer, and the performance test results are shown in table 1.
Comparative example 2
In the composition expression aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 10 mol%, b is 70 mol%, c is 0 mol%, d is 10 mol%, and e is 10 mol%.
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 mol percentage of each element in the composition expression2、CaCO3、Li2CO3、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible to perform heat preservation and presintering for 3 hours at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in the comparative example 2 is subjected to microwave dielectric performance test by using a microwave network analyzer, and the performance test results are shown in table 1.
Comparative example 3
In the composition expression aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 10 mol%, b is 70 mol%, c is 10 mol%, d is 0 mol%, and e is 10 mol%.
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 mol percentage of each element in the composition expression2、CaCO3、ZnO、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible to perform heat preservation and presintering for 3 hours at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in the comparative example 3 is tested for microwave dielectric performance by a microwave network analyzer, and the performance test results are shown in table 1.
Comparative example 4
In the composition expression aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 10 mol%, b is 70 mol%, c is 10 mol%, d is 10 mol%, and e is 0 mol%.
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 mol percentage of each element in the composition expression2、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible to perform heat preservation and presintering for 3 hours at 1100 ℃ to obtain a powder base material;
(2) fully ball-milling the powder base material 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 sintering for 4 hours at the temperature of 1340 ℃ to obtain the high-temperature stable type low-dielectric-constant microwave dielectric ceramic.
The microwave dielectric ceramic obtained in the comparative example 4 is subjected to microwave dielectric performance test by using a microwave network analyzer, and the performance test results are shown in table 1.
TABLE 1
As can be seen from table 1, compared with the microwave dielectric ceramics of comparative examples 1 to 4, the microwave dielectric ceramics of examples 1 to 5 of the present invention have a higher Q value and an adjustable frequency temperature coefficient close to zero while ensuring a lower sintering temperature, and have better temperature stability. Among these, the microwave dielectric ceramic of example 3 has relatively best overall microwave dielectric properties.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents made by the contents of the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
1. A high-temperature stable low-dielectric constant microwave dielectric ceramic is characterized in that: the composition expression is aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3Wherein a, b, c, d and e independently represent mole percentages, and satisfy the following conditions: a is more than or equal to 10 mol% and less than or equal to 20 mol%, b is more than or equal to 65 mol% and less than or equal to 75 mol%, c is more than or equal to 2 mol% and less than or equal to 10 mol%, d is more than or equal to 2 mol% and less than or equal to 10 mol%, e is more than or equal to 5 mol% and less than or equal to 10 mol%, and a + b + c + d + e is equal to 100 mol%.
2. A high temperature stable low dielectric constant microwave dielectric ceramic as claimed in claim 1, wherein: in the composition formula, a is 15 mol%, b is 70 mol%, c is 5 mol%, d is 5 mol%, and e is 5 mol%.
3. A high temperature stable low dielectric constant microwave dielectric ceramic as claimed in claim 1, wherein: the microwave dielectric ceramic has a relative dielectric constant of 19-21, a Qxf value of more than 60000GHz, and a temperature coefficient of resonance frequency within +/-3 ppm/DEG C.
4. A preparation method of high-temperature stable low-dielectric-constant microwave dielectric ceramic is characterized by comprising the following steps:
(1) according to the composition expression aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3MgO and SiO are respectively weighed according to the mol percentage of each element2、CaCO3、Li2CO3、ZnO、Nd2O3、TiO2Fully mixing the weighed materials, performing ball milling, drying and sieving after ball milling, and then putting the mixture into a corundum crucible for heat preservation and presintering to obtain a powder base material;
wherein, the composition expression is aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3Wherein a, b, c, d and e each independently represent a mole percentage, and satisfy the following condition: a is more than or equal to 10 mol% and less than or equal to 20 mol%, b is more than or equal to 65 mol% and less than or equal to 75 mol%, c is more than or equal to 2 mol% and less than or equal to 10 mol%, d is more than or equal to 2 mol% and less than or equal to 10 mol%, e is more than or equal to 5 mol% and less than or equal to 10 mol%, and a + b + c + d + e is equal to 100 mol%;
(2) fully ball-milling the powder base material obtained in the step (1), and drying, granulating and sieving the ball-milled powder base material;
(3) and (3) pressing and forming the mixed powder treated in the step (2), and finally sintering to obtain the high-temperature stable low-dielectric-constant microwave dielectric ceramic.
5. The method according to claim 4, wherein the ceramic is a high temperature stable low dielectric constant microwave dielectric ceramic,
in the composition expression aMgSiO3-bMgTiO3-cZnTiO3-dLiNdTi2O6-eCaTiO3In the above formula, a is 15 mol%, b is 70 mol%, c is 5 mol%, d is 5 mol%, and e is 5 mol%.
6. The method for preparing a high temperature stable low dielectric constant microwave dielectric ceramic according to claim 4, wherein the heat-preserving pre-sintering process in step (1) is performed at 1000-1200 ℃ for 3-5 h.
7. The method as claimed in claim 4, wherein the sintering process in step (3) is carried out at 1300-1360 ℃ for 3-5 h.
8. The method as claimed in claim 4, wherein the granulating in step (2) is performed by mixing the dried powder with a binder and then forming micron-sized spherical particles.
9. The method as claimed in claim 8, wherein the binder is selected from at least one of polyvinyl alcohol solution, polyvinyl butyral solution, acrylic solution and methyl cellulose.
10. The method as claimed in claim 4, wherein in the step (3), the mixture powder is pressed into a cylinder with a diameter of 10mm and a height of 6 mm.
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