CN113773080B - Ultralow-loss temperature-stable microwave dielectric ceramic material, and preparation method and application thereof - Google Patents
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Abstract
The invention discloses an ultra-low loss temperature stable microwave dielectric ceramic material, a preparation method and application thereof, wherein the preparation method of the ceramic material comprises the following steps: s1: mixing MgO and Li2CO3And Nb2O5Mixing with agate ball and absolute alcohol, ball milling for 8-10 hr, drying and pre-sintering to obtain Li3Mg2(NbO6) Pre-burning powder; s2: mixing carbonate with TiO2Fully mixing the powder with agate balls and absolute ethyl alcohol, ball-milling for 8-10h, and drying and pre-sintering to prepare titanate pre-sintered powder; s3: mixing Li in S13Mg2(NbO6) Fully mixing and ball-milling the pre-sintered powder, the titanate pre-sintered powder in S2, LiF, agate balls and absolute ethyl alcohol for 8-10h, drying, granulating, sieving, pressing into a cylindrical green compact by a powder tablet press, and sintering the green compact to obtain the ultralow-loss temperature-stable microwave dielectric ceramic material. The invention obviously improves the temperature stability of the ceramic material, has lower loss and enriches the requirements of the current high-frequency communication electronic circuit technology on the low-dielectric-constant material with good temperature stability of the working environment and higher Q value.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to an ultralow-loss temperature-stable microwave dielectric ceramic material, a preparation method and application thereof.
Background
At present, in order to improve the temperature stability of the ceramic material, a compound which has an opposite resonant frequency temperature coefficient and does not chemically react with the base material is mainly added to form the composite ceramic material, but the method can increase the dielectric loss of the ceramic material to a certain extent, remarkably reduce the Q value of the material and influence the application range of the ceramic material. Therefore, it is a technical problem to be solved by the present application to develop a new ceramic material with high Q value and high temperature stability.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the ultralow-loss temperature-stable microwave dielectric ceramic material, the preparation method and the application, so that the temperature stability of the ceramic material is remarkably improved, the dielectric loss is reduced relative to a base material, and the requirements of the current high-frequency communication electronic circuit technology on a low-dielectric-constant material with good working environment temperature stability and higher Q value are enriched.
The invention provides an ultra-low loss temperature stable microwave dielectric ceramic material, which comprises the following components:
Li3Mg2(NbO6) 80.2-94.8wt%,
the balance being niobate;
wherein the quality factor of the microwave dielectric ceramic material is larger than that of the Li3Mg2(NbO6) The figure of merit of (1).
Preferably, the niobate is Ca (NbO)3)。
Preferably, the ceramic material has dielectric loss of 0.000082-0.000084, quality factor of 83420-84970GHz, dielectric constant of 15.6-15.9 and temperature coefficient of resonance frequency of-12.5-10.7 ppm/DEG C.
The invention provides a preparation method of an ultra-low loss temperature stable microwave dielectric ceramic material, which comprises the following steps:
S1:Li3Mg2(NbO6) Preparation of pre-fired powder
Mixing MgO and Li2CO3And Nb2O5Mixing with agate ball and absolute alcohol, ball milling for 8-10 hr, drying and pre-sintering to obtain Li3Mg2(NbO6) Pre-burning powder;
s2: preparation of titanate pre-sintering powder
Mixing carbonate with TiO2Fully mixing the powder with agate balls and absolute ethyl alcohol, ball-milling for 8-10h, and drying and pre-sintering to prepare titanate pre-sintered powder;
s3: preparation of ceramic materials
Mixing Li in S13Mg2(NbO6) Fully mixing and ball-milling the pre-sintered powder, the titanate pre-sintered powder in S2, LiF, agate balls and absolute ethyl alcohol for 8-10h, drying, granulating, sieving, pressing into a cylindrical green compact by a powder tablet press, and sintering the green compact to obtain the ultralow-loss temperature-stable microwave dielectric ceramic material.
Preferably, the carbonate in S2 is CaCO3The titanate pre-sintering powder isCaTiO3Pre-sintering the powder.
Preferably, the drying conditions in S1 are: the temperature is 80-100 ℃, and the time is 10-12 h; the conditions of the pre-burning are as follows: the temperature is 1000 ℃ and 1200 ℃, and the time is 2-6 h.
Preferably, the drying conditions in S2 are: the temperature is 80-100 ℃, and the time is 10-12 h; the conditions of the pre-burning are as follows: the temperature is 1000 ℃ and 1100 ℃ and the time is 2-6 h.
Preferably, Li in said S33Mg2(NbO6) The mass ratio of the pre-sintered powder to the titanate pre-sintered powder to LiF is (96-x) x:4, wherein x is more than or equal to 2.6 and less than or equal to 4.5.
Preferably, the conditions for green body sintering in S3 are: the temperature is 1025 ℃ and 1100 ℃ and the time is 4-8 h.
The invention provides an application of the ultra-low loss temperature stable microwave dielectric ceramic material in microwave devices.
Mechanism of action
The invention is achieved by mixing Li3Mg2(NbO6) And titanate, and controlling its proportioning and regulating later-stage sintering process to promote titanate and small portion of Li3Mg2(NbO6) The temperature stability of the microwave dielectric ceramic material is obviously improved by the oxidation-reduction reaction in which the niobium ions in the generated niobate are reduced from high valence to low valence; in addition, Li is contained in the matrix ceramic material3Mg2(NbO6) When the component with positive temperature stability is added to improve the temperature stability of the microwave dielectric ceramic material, the quality factor of the ceramic material is inevitably reduced, and the ceramic material prepared by the method not only improves the temperature stability of the microwave dielectric ceramic material, but also has the quality factor (83420-84970GHz) relative to Li3Mg2(NbO6) The quality factor (79600GHz) is increased to a certain extent, which shows that the microwave dielectric ceramic material prepared by the method improves the temperature stability and reduces the dielectric loss.
Advantageous technical effects
The temperature-stable niobate microwave dielectric ceramic material prepared by the invention has good dielectric loss, quality factor, dielectric constant, resonant frequency temperature coefficient and other properties, overcomes the defects of high sintering temperature and large resonant frequency temperature coefficient of the ceramic material, reduces the dielectric loss while ensuring the temperature stability of the material, enriches the requirements of the current high-frequency communication electronic circuit technology on low-dielectric-constant materials with good working environment temperature stability and higher Q value, and can be widely applied to the manufacturing of microwave devices.
Drawings
FIG. 1 is an X-ray powder diffraction pattern of the ultra-low loss temperature stable microwave dielectric ceramic material prepared in examples 1-8 of the present invention.
Detailed Description
Example 1
(1) Preparation of Li3Mg2(NbO6) Pre-sintered powder
According to Li3Mg2(NbO6) 3.12g of MgO having a purity of 99.99% and 4.291g of Li having a purity of 99.99% were weighed in the stoichiometric ratio of (1)2CO3And 5.145g of Nb with a purity of 99.99%2O5To obtain a raw material 1; putting the raw material 1, agate balls and absolute ethyl alcohol into a nylon ball mill according to the mass ratio of 1:2:2, fully mixing and ball milling for 8 hours, drying for 12 hours at 90 ℃, presintering for 4 hours at 1100 ℃ to prepare Li3Mg2(NbO6) Pre-sintering the powder.
(2) Preparation of CaTiO3Pre-sintered powder
According to CaTiO37.399g of CaCO having a purity of 99.95% were weighed out in the stoichiometric ratio of3And 5.876g of 99.99% pure TiO2To obtain a raw material 2; putting the raw material 2, agate balls and absolute ethyl alcohol into a nylon ball milling tank according to the mass ratio of 1:2:2, fully mixing and ball milling for 8 hours, drying for 12 hours at 90 ℃, presintering for 4 hours at 1000 ℃ to prepare CaTiO3Pre-sintering the powder.
(3) Preparation of niobate microwave dielectric ceramic material
Weighing 9.591gLi3Mg2(NbO6) Pre-sintered powder, 0.409g CaTiO3Pre-sintering powder and 0.417g LiF powder with the purity of 99.99 percent to obtain a raw material 3; will be originalThe material 3, agate balls and absolute ethyl alcohol are filled into a nylon ball mill tank according to the mass ratio of 1:2:2, fully mixed and ball milled for 8 hours, dried at 90 ℃ for 12 hours, added with a polyvinyl alcohol aqueous solution with the mass percent of 3 percent of that of the raw material being 5 percent, granulated, sieved by a 120-mesh sieve, pressed into cylindrical green bodies with the diameter of 11.5mm and the thickness of 6mm by a powder tablet machine under the pressure of 200MPa, and sintered at 1050 ℃ for 6 hours to prepare the niobate microwave dielectric ceramic material.
Example 2
In the step (3) of example 1, the green body was sintered at 1050 ℃ for 4 hours, and other steps were the same as in example 1 to prepare a niobate microwave dielectric ceramic material.
Example 3
In the step (3) of example 1, the green body is sintered at 1050 ℃ for 8 hours, and other steps are the same as in example 1 to prepare a niobate microwave dielectric ceramic material.
Example 4
In the step (3) of example 1, the green body is sintered for 6 hours at 1025 ℃, and other steps are the same as in example 1, so that the niobate microwave dielectric ceramic material is prepared.
Example 5
In the step (3) of example 1, the green body was sintered at 1075 ℃ for 6 hours, and other steps were the same as in example 1 to prepare a niobate microwave dielectric ceramic material.
Example 6
In the step (3) of example 1, the green body was sintered at 1100 ℃ for 6 hours, and other steps were the same as in example 1 to prepare a niobate microwave dielectric ceramic material.
Example 7
In step (3) of example 1, 9.370g of Li were weighed3Mg2(NbO6) Pre-sintered powder, 0.270g CaTiO3The pre-sintered powder and 0.417g LiF powder with the purity of 99.99 percent are prepared into the niobate microwave dielectric ceramic material by the same steps as the embodiment 1.
Example 8
In step (3) of example 1, 9.534g of Li were weighed3Mg2(NbO6) Pre-sintered powder, 0.466g CaTiO3The pre-sintered powder and 0.417g LiF powder with the purity of 99.99 percent are prepared into the niobate microwave dielectric ceramic material by the same steps as the example 1.
The niobate microwave dielectric ceramic materials obtained in the above examples 1 to 8 were characterized by using a Smartlab type X-ray diffractometer, and the results are shown in FIG. 1, and the ceramic materials prepared by using the niobate microwave dielectric ceramic materials were made of Li3Mg2(NbO6) Phase and Ca (NbO)3) The compositions of the phases are shown in the table 1. Due to Ti elementAnd Nb elementHas similar atomic radii, and Ti element may replace Nb element to enter Li during sintering process3Mg2(NbO6) The crystal lattice of the compound, therefore, the compound containing Ti element is not detected during the X-ray detection.
TABLE 1 phase composition of microwave dielectric ceramic materials prepared in examples 1-8
The ceramic materials prepared in examples 1 to 8 were ground and polished, and then processed into a cylinder having a diameter of 11.5mm and a height of 5.5 to 6.5mm, and the ceramic materials were subjected to microwave dielectric property test by using a closed cavity resonance method using an ZVB20 vector network analyzer (manufactured by rodder & schwarz, germany) in combination with a high and low temperature chamber, and the results are shown in table 2.
TABLE 2 microwave dielectric Properties of microwave dielectric ceramic materials prepared in examples 1-8
As can be seen from table 2, the dielectric loss of the niobate microwave dielectric ceramic material prepared in embodiments 1 to 8 of the present invention is 0.000082 to 0.000084, the quality factor is 83420-84970GHz, the dielectric constant is 15.6 to 15.9, and the temperature coefficient of the resonant frequency is-12.5 to 10.7 ppm/deg.c, which illustrates that the niobate microwave dielectric ceramic material prepared in embodiments 1 to 8 improves the temperature stability of the ceramic material and simultaneously reduces the dielectric loss, enriches the requirements of the current high-frequency communication electronic circuit technology for low-dielectric-constant materials with good temperature stability of the working environment and higher Q value, and can be widely applied to the manufacture of microwave devices.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The ultra-low loss temperature stable microwave dielectric ceramic material is characterized by comprising the following components:
Li3Mg2(NbO6)80.2-94.8wt%,
the balance being niobate;
wherein the quality factor of the microwave dielectric ceramic material is larger than that of the Li3Mg2(NbO6) The quality factor of (2);
the preparation method of the ultralow-loss temperature-stable microwave dielectric ceramic material comprises the following steps:
S1:Li3Mg2(NbO6) Preparation of pre-fired powder
Mixing MgO and Li2CO3And Nb2O5Fully mixing the powder with agate balls and absolute ethyl alcohol, ball-milling the mixture for 8 to 10 hours, and drying and presintering the mixture to obtain Li3Mg2(NbO6) Pre-burning powder;
s2: preparation of titanate pre-sintered powder
Mixing carbonate with TiO2Mixing with agate ball and absolute alcohol, ball milling for 8-10 hr, drying and pre-sintering to obtain TiAcid salt pre-sintering powder;
s3: preparation of ceramic materials
Mixing Li in S13Mg2(NbO6) Fully mixing and ball-milling the pre-sintered powder, the titanate pre-sintered powder in S2, LiF, agate balls and absolute ethyl alcohol for 8-10h, drying, granulating, sieving, pressing into a cylindrical green compact by using a powder tablet press, and sintering the green compact to obtain the ultralow-loss temperature-stable microwave dielectric ceramic material;
the carbonate in S2 is CaCO3The titanate pre-sintered powder is CaTiO3Pre-burning powder;
li in said S33Mg2(NbO6) The mass ratio of the pre-sintered powder to the titanate pre-sintered powder to LiF is (96-x) x:4, wherein x is more than or equal to 2.6 and less than or equal to 4.5;
the sintering conditions of the green body in the S3 are as follows: the temperature is 1025 ℃ and 1100 ℃ and the time is 4-8 h.
2. The ultra-low loss temperature stable microwave dielectric ceramic material of claim 1 wherein the niobate is Ca (NbO)3)。
3. The ultra-low loss temperature stable microwave dielectric ceramic material as claimed in claim 2, wherein the dielectric loss of the ceramic material is 0.000082-0.000084, the quality factor is 83420-84970GHz, the dielectric constant is 15.6-15.9, and the temperature coefficient of the resonant frequency is-12.5-10.7 ppm/° C.
4. The method for preparing an ultra-low loss temperature stable microwave dielectric ceramic material as claimed in any one of claims 1 to 3, wherein the method comprises the following steps:
S1:Li3Mg2(NbO6) Preparation of pre-fired powder
Mixing MgO and Li2CO3And Nb2O5Mixing with agate ball and absolute alcohol, ball milling for 8-10 hr, drying and pre-sintering to obtain Li3Mg2(NbO6) Pre-burning powder;
s2: preparation of titanate pre-sintering powder
Mixing carbonate with TiO2Fully mixing the powder with agate balls and absolute ethyl alcohol, ball-milling for 8-10h, and drying and pre-sintering to prepare titanate pre-sintered powder;
s3: preparation of ceramic materials
Mixing Li in S13Mg2(NbO6) Fully mixing and ball-milling the pre-sintered powder, the titanate pre-sintered powder in S2, LiF, agate balls and absolute ethyl alcohol for 8-10h, drying, granulating, sieving, pressing into a cylindrical green compact by a powder tablet press, and sintering the green compact to obtain the ultralow-loss temperature-stable microwave dielectric ceramic material.
5. The method for preparing an ultra-low loss temperature stable microwave dielectric ceramic material as claimed in claim 4, wherein the carbonate in S2 is CaCO3The titanate pre-sintered powder is CaTiO3Pre-sintering the powder.
6. The method for preparing an ultra-low loss temperature stable microwave dielectric ceramic material according to claim 4, wherein the drying conditions in S1 are as follows: the temperature is 80-100 ℃, and the time is 10-12 h; the conditions of the pre-burning are as follows: the temperature is 1000 ℃ and 1200 ℃, and the time is 2-6 h.
7. The method for preparing an ultra-low loss temperature stable microwave dielectric ceramic material according to claim 4, wherein the drying conditions in S2 are as follows: the temperature is 80-100 ℃, and the time is 10-12 h; the conditions of the pre-burning are as follows: the temperature is 1000-1100 ℃, and the time is 2-6 h.
8. The method for preparing an ultra-low loss temperature stable microwave dielectric ceramic material as claimed in claim 4, wherein Li in S33Mg2(NbO6) The mass ratio of the pre-sintered powder to the titanate pre-sintered powder to LiF is (96-x) x:4, wherein x is more than or equal to 2.6 and less than or equal to 4.5.
9. The method of claim 4, wherein the green body sintering conditions in S3 are as follows: the temperature is 1025 ℃ and 1100 ℃ and the time is 4-8 h.
10. Use of the ultra-low loss temperature stable microwave dielectric ceramic material according to any of claims 1-3 in microwave devices.
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Li-Mg-Nb系微波介质陶瓷改性研究;王文文;《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》;20200715(第07期);第42-49页 * |
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