CN112745106A - Low-expansion-coefficient microwave dielectric ceramic material and preparation method thereof - Google Patents
Low-expansion-coefficient microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title description 12
- 239000000654 additive Substances 0.000 claims abstract description 35
- 230000000996 additive effect Effects 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 13
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 13
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 13
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000000919 ceramic Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims 2
- 238000010304 firing Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention is suitable for the technical field of dielectric ceramic production, and discloses a low-expansion-coefficient microwave dielectric ceramic material which comprises a main component and a modified additive, wherein the main component is xAl2O3‑yTiO2Wherein x is 0.88-0.92 and y is 0.06-0.09; the modifying additive is ZrO2，La2O3、Nd2O3、SiO2、CaCO3A combination of at least two of the above. Also provides a method for preparing the microwave dielectric ceramic material with the low expansion coefficient. The low-expansion-coefficient microwave dielectric ceramic material has the advantages of low expansion coefficient, adjustable dielectric constant, high quality factor and near-zero temperature coefficient of resonant frequency.
Description
Technical Field
The invention relates to the technical field of dielectric ceramic production, in particular to a low-expansion-coefficient microwave dielectric ceramic material and a preparation method thereof.
Background
The microwave dielectric material is ceramic which is used as a medium and can complete one or more functions in a microwave frequency band (300 MHz-300 GHz) circuit, and is mainly used for preparing microwave components such as a resonator, a filter, a dielectric antenna, a dielectric guided wave loop and the like. With the rapid deployment of a 5G network, the number of antennas is increased by 5G large-scale antenna technology, and the requirements of miniaturization, light weight, low cost and high performance of a filter for 5G communication are obvious, but a metal cavity filter adopted by the current 4G communication has the defects of large volume, heavy weight, more heat generation, higher price and difficulty in wide application in a high-integration antenna.
Microwave dielectric ceramic materials are often subjected to environmental temperature shock (thermal shock) during high-temperature service to generate cracks and even fail. Because the microwave dielectric ceramic has poor thermal shock performance and is related to the larger thermal expansion coefficient of the existing microwave dielectric ceramic, how to reduce the expansion coefficient of the ceramic material is a technical problem to be solved by the prior art.
Disclosure of Invention
In order to overcome the technical problems in the background art, the invention provides a microwave dielectric ceramic material with low expansion coefficient, adjustable dielectric constant, high quality factor and near-zero resonant frequency temperature coefficient and a preparation method thereof.
The invention is realized by the following technical scheme:
the microwave dielectric ceramic material with the low expansion coefficient comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.88-0.92 and y is 0.06-0.09; the modifying additive is ZrO2，La2O3、Nd2O3、SiO2、CaCO3A combination of at least two of the above.
Optionally, the modified additives respectively account for the following main components in percentage by mass: ZrO (ZrO)20-3.0% of La2O30-3.0% of Nd2O30-3% of SiO20 to 0.7 percent of CaCO3Is 0-2.0%.
The invention also provides a method for preparing the microwave dielectric ceramic material with the low expansion coefficient, which comprises the following steps:
1) mixing Al2O3、TiO2The xAl is prepared2O3-yTiO2Then, uniformly mixing the mixture with the modified additive to obtain a mixture;
2) putting the mixture obtained in the step 1) into a planetary ball mill for wet ball milling to obtain ball milling slurry;
3) drying the ball milling slurry obtained in the step 2) to obtain dry powder S1;
4) putting the dried powder S1 into a high-temperature furnace box type furnace for pre-burning to prepare a pre-burned block;
5) crushing the pre-sintered block obtained in the step 4), and then placing the crushed pre-sintered block in a ball mill for wet ball milling to prepare dry powder S2;
6) uniformly mixing the dry powder S2 with an adhesive, and then carrying out spray granulation to prepare granulated powder;
7) dry-pressing and molding the granulated powder obtained in the step 6) into a green body;
8) and 7) sintering the green body obtained in the step 7) in a high-temperature box type furnace according to a set temperature curve to obtain the microwave dielectric ceramic body.
Wherein the presintering temperature in the step 4) is 1170-1200 ℃, and the presintering time is 3-5 hours.
Wherein the ball milling time in the step 5) is 4-8 hours.
Optionally, the adhesive in the step 6) is a polyvinyl alcohol solution with the weight percent of 7%, and the mass percentage of the adhesive is 1% -2%.
Wherein the glue discharging temperature zone of the step 8) is 400-600 ℃, the heat preservation time is 2-4 hours, the high-temperature sintering temperature zone is 1250-1400 ℃, and the sintering time is 4-6 hours.
The low-expansion-coefficient microwave dielectric ceramic material prepared by the invention has the advantages of low thermal expansion coefficient, excellent microwave performance, low dielectric constant, high quality factor, small dielectric constant temperature coefficient and the like, and can be used for manufacturing microwave devices such as resonators, antennas, filters and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clear and complete, some embodiments of the present invention will be described below. The examples are for illustrative purposes only and do not limit the scope of the present invention in any way. Unless otherwise indicated, the materials used in the examples are conventional or commercially available materials, and the materials and reagents are used in addition in a manner conventional in the art. The meanings stated are all customary in the art, for example 10% NaOH solution means mass fraction and 55% ethanol solution means volume fraction.
Example 1 microwave dielectric ceramic material with low expansion coefficient
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.918 and y is 0.078; the modifying additive is ZrO2And La2O3Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: ZrO (ZrO)20-3.0% of La2O3Is 0-3.0%.
The preparation method of the microwave dielectric ceramic material with the low expansion coefficient comprises the following steps:
1) mixing Al2O3、TiO2The xAl is prepared2O3-yTiO2Then, uniformly mixing the mixture with the modified additive to obtain a mixture;
2) putting the mixture obtained in the step 1) into a planetary ball mill for wet ball milling to obtain ball milling slurry;
3) drying the ball milling slurry obtained in the step 2) to obtain dry powder S1;
4) putting the dried powder S1 into a high-temperature furnace box type furnace for pre-burning to prepare a pre-burned block;
5) crushing the pre-sintered block obtained in the step 4), and then placing the crushed pre-sintered block in a ball mill for wet ball milling to prepare dry powder S2;
6) uniformly mixing the dry powder S2 with an adhesive, and then carrying out spray granulation to prepare granulated powder;
7) dry-pressing and molding the granulated powder obtained in the step 6) into a green body;
8) and 7) sintering the green body obtained in the step 7) in a high-temperature box type furnace according to a set temperature curve to obtain the microwave dielectric ceramic body.
Wherein the presintering temperature in the step 4) is 1170-1200 ℃, and the presintering time is 3-5 hours.
The ball milling time in the step 5) is 4-8 hours.
The adhesive in the step 6) is a polyvinyl alcohol solution with the weight percent of 7%, and the mass percentage of the adhesive is 1% -2%.
The glue discharging temperature zone of the step 8) is 400-600 ℃, the heat preservation time is 2-4 hours, the high-temperature sintering temperature zone is 1250-1400 ℃, and the sintering time is 4-6 hours.
Example 2 microwave dielectric ceramic Material with Low coefficient of expansion
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.914 and y is 0.072; the modifying additive is ZrO2And Nd2O3Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: ZrO (ZrO)20-3.0% of Nd2O3Is 0-3%.
The preparation method comprises the following steps: the same as in example 1.
EXAMPLE 3 Low expansion coefficient microwave dielectric ceramic Material
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.902 and y is 0.075; the modifying additive is ZrO2And SiO2Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: ZrO (ZrO)20-3.0% of SiO2Is 0-0.7%.
The preparation method comprises the following steps: the same as in example 1.
EXAMPLE 4 Low expansion coefficient microwave dielectric ceramic Material
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.914 and y is 0.074; the modifying additive is ZrO2、La2O3、Nd2O3Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: ZrO (ZrO)20-3.0% of La2O30-3.0% of Nd2O3Is 0-3%.
The preparation method comprises the following steps: the same as in example 1.
EXAMPLE 5 Low expansion coefficient microwave dielectric ceramic Material
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.89 and y is 0.075; the modified additive is Nd2O3、SiO2、CaCO3Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: nd (neodymium)2O30-3% of SiO20 to 0.7 percent of CaCO3Is 0-2.0%.
The preparation method comprises the following steps: the same as in example 1.
EXAMPLE 6 Low expansion coefficient microwave dielectric ceramic Material
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.89 and y is 0.075; the modified additive is Nd2O3、SiO2、CaCO3Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: nd (neodymium)2O30-3% of SiO20 to 0.7 percent of CaCO3Is 0-2.0%.
The preparation method comprises the following steps: the same as in example 1.
Example 7 microwave dielectric ceramic Material with Low coefficient of expansion
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.884 and y is 0.08; the modifying additive is ZrO2，La2O3、Nd2O3Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: ZrO (ZrO)20-3.0% of La2O30-3.0% of Nd2O3Is 0-3%.
The preparation method comprises the following steps: the same as in example 1.
EXAMPLE 8 Low expansion coefficient microwave dielectric ceramic Material
Comprises a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.88 and y is 0.085; the modifying additive is ZrO2，La2O3、SiO2Combinations of (a) and (b).
Wherein the modified additives respectively account for the main components in the following mass ratio: ZrO (ZrO)20-3.0% of La2O30-3.0% of SiO2Is 0-0.7%.
The preparation method comprises the following steps: the same as in example 1.
Tables 1-2 show chemical feedstock formulations and sample testing data for examples 1-8 of the present invention.
Table 1:
table 2:
the low-expansion-coefficient microwave dielectric ceramic material prepared by the invention has the dielectric constant of 11-13, the quality factor Qxf value of 95000-11800 GHz and the temperature coefficient (tau) of resonance frequencyf) Is-10 to +10 ppm/DEG C, and has a thermal expansion coefficient of 2.5 to 8.6 ppm/DEG C; the microwave dielectric constant adjustable microwave dielectric constant can be applied to microwave devices such as filters, GPS antennas and resonators for 5G communication base stations, and has the advantages of low expansion coefficient, adjustable dielectric constant, high quality factor and near-zero resonant frequency temperature coefficient.
The above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present application.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The microwave dielectric ceramic material with the low expansion coefficient is characterized by comprising a main component and a modified additive, wherein the main component is xAl2O3-yTiO2Wherein x is 0.88-0.92 and y is 0.06-0.09; the modifying additive is ZrO2，La2O3、Nd2O3、SiO2、CaCO3A combination of at least two of the above.
2. The microwave dielectric ceramic material with the low expansion coefficient as claimed in claim 1, wherein the mass ratio of the modifying additive to the main component is: ZrO (ZrO)20-3.0% of La2O30-3.0% of Nd2O30-3% of SiO20 to 0.7 percent of CaCO3Is 0-2.0%.
3. A method for preparing the low-expansion-coefficient microwave dielectric ceramic material as claimed in any one of claims 1 to 2, which is characterized by comprising the following steps:
1) mixing Al2O3、TiO2The xAl is prepared2O3-yTiO2Then, uniformly mixing the mixture with the modified additive to obtain a mixture;
2) putting the mixture obtained in the step 1) into a planetary ball mill for wet ball milling to obtain ball milling slurry;
3) drying the ball milling slurry obtained in the step 2) to obtain dry powder S1;
4) putting the dried powder S1 into a high-temperature furnace box type furnace for pre-burning to prepare a pre-burned block;
5) crushing the pre-sintered block obtained in the step 4), and then placing the crushed pre-sintered block in a ball mill for wet ball milling to prepare dry powder S2;
6) uniformly mixing the dry powder S2 with an adhesive, and then carrying out spray granulation to prepare granulated powder;
7) dry-pressing and molding the granulated powder obtained in the step 6) into a green body;
8) and 7) sintering the green body obtained in the step 7) in a high-temperature box type furnace according to a set temperature curve to obtain the microwave dielectric ceramic body.
4. The method of claim 3, wherein the pre-firing temperature of step 4) is 1170-1200 ℃ and the pre-firing time is 3-5 hours.
5. The method as claimed in claim 3, wherein the ball milling time in the step 5) is 4 to 8 hours.
6. The method as claimed in claim 3, wherein the binder in the step 6) is 7 wt% of polyvinyl alcohol solution, and the mass ratio of the binder is 1-2%.
7. The method as claimed in claim 3, wherein the gel-removing temperature zone of step 8) is 400-600 ℃, the temperature is maintained for 2-4 hours, the high-temperature sintering temperature zone is 1250-1400 ℃, and the sintering time is 4-6 hours.
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