CN112552034A - Low-loss low-dielectric-constant temperature-stable microwave dielectric ceramic and preparation method thereof - Google Patents
Low-loss low-dielectric-constant temperature-stable microwave dielectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-loss low-dielectric constant temperature stable microwave dielectric ceramic, the composition expression of which is aMg2SiO4‑bMg2TiO4‑cCaTiO3‑dLi2NdO3Wherein a, b, c and d independently represent mole percentages, and satisfy the following conditions: a is more than or equal to 50 mol% and less than or equal to 60 mol%, b is more than or equal to 20 mol% and less than or equal to 30 mol%, c is more than or equal to 10 mol% and less than or equal to 20 mol%, d is more than or equal to 10 mol% and less than or equal to 20 mol%, and a + b + c + d is equal to 100 mol%. The invention also discloses a preparation method of the temperature-stable microwave dielectric ceramic with low loss and low dielectric constant. The microwave dielectric ceramic has the advantages of low dielectric constant, high quality factor and high temperature stability; the preparation process is simple, the adopted raw materials are moderate in price, pollution is avoided, and the industrialization prospect is good.
Description
Technical Field
The invention belongs to the technical field of electronic ceramics and preparation thereof, and particularly relates to a temperature-stable microwave dielectric ceramic with low loss and low dielectric constant and a preparation method thereof.
Background
The microwave dielectric ceramic is used as a dielectric material in a microwave frequency band (300MHz-300GHz) circuit and can complete one or more functions, is widely used for producing components such as a resonator, a filter, a dielectric antenna, a dielectric waveguide loop and the like in modern communication, is a key basic material of modern communication technology, and is already applied to portable mobile phones, automobile phones and cordless electric appliancesThe system has very important application in the aspects of telephone, television satellite receiver, military radar and the like, and plays an increasingly important role in the miniaturization and integration processes of modern communication tools. The microwave dielectric ceramic with ultralow dielectric constant is mainly represented by Al2O3-TiO2、Y2BaCuO5、MgAl2O4 and Mg2SiO4The dielectric constant Er is less than or equal to 20, the quality factor Qxf is more than or equal to 5000GHz, and the temperature coefficient tf of the resonant frequency is less than or equal to 10 ppm/DEG C, so that the material is mainly used in the fields of microwave circuit substrates, radio frequency electronic tag (RFID) circuit substrates and electronic packaging; wherein, Mg2SiO4The loss and the temperature stability of the material cannot meet the application requirements of the existing material when Qf is 73760GHz, Er is 7.4 and tf is-60 ppm/DEG C.
At present, there has been a technique of utilizing MgTa2O6For Mg2SiO4Adjusting the performance; for example, the Chinese patent CN201711066157.4 obtains the chemical structural formula of xMg2SiO4-(1-x)MgTa2O6The microwave dielectric ceramic with + y wt% B has a frequency temperature coefficient close to zero and a high quality factor value, but has a high dielectric constant, namely the comprehensive performance of the microwave dielectric ceramic is still not ideal; and when the sintering aid B substance is not added, the microwave dielectric ceramic has poor temperature stability, and the resonant frequency temperature coefficient can be adjusted only after the sintering aid B substance is added. In addition, Ta for preparing the microwave dielectric ceramic2O5The raw material price is high, so that the production cost is increased, and the market application of the product is limited. Therefore, it is necessary to develop a microwave dielectric ceramic with low production cost, low dielectric constant, high quality factor and good temperature stability to meet the requirement of ultra-high frequency band application.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a temperature-stable low-dielectric-constant microwave dielectric ceramic and a preparation method thereof; the microwave dielectric ceramic has the advantages of lower dielectric constant, higher quality factor and better temperature stability; the preparation process is simple, the adopted raw materials are moderate in price, pollution is avoided, and the industrialization prospect is good.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a low-loss low-dielectric-constant temperature-stable microwave dielectric ceramic is characterized in that: its composition expression is aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3Wherein a, b, c and d independently represent mole percentages, and satisfy the following conditions: a is more than or equal to 50 mol% and less than or equal to 60 mol%, b is more than or equal to 20 mol% and less than or equal to 30 mol%, c is more than or equal to 10 mol% and less than or equal to 20 mol%, d is more than or equal to 10 mol% and less than or equal to 20 mol%, and a + b + c + d is equal to 100 mol%.
Furthermore, the dielectric constant of the microwave dielectric ceramic is 9 to 11, the Q x f value of the quality factor is 95000 to 150000GHz, and the temperature coefficient of the resonance frequency is-2 to 10 ppm/DEG C.
The invention further provides a preparation method of the temperature-stable microwave dielectric ceramic with low loss and low dielectric constant, which comprises the following steps:
(1) unsaturated ceramic phase Li2NdO3Synthesis of (2)
Mixing Li2CO3Powder and Nd2O3The powder is according to the chemical formula Li2NdO3Mixing the corresponding elements in the mixture according to the molar ratio of the Li2CO3And Nd2O3Mixing, ball milling, stoving, sieving, roasting in corundum crucible to obtain Li2NdO3A composition;
(2) with Mg2SiO4Powder material, Mg2TiO4Powder material, CaTiO3Powder material, Li2NdO3The powder is taken as a raw material and is expressed by a composition expression aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3The molar percentages of the respective compositions in (1) are measured for Mg2SiO4Powder material, Mg2TiO4Powder material, CaTiO3Powder material, Li2NdO3Powder material, fully mixing the weighed materialsBall milling, drying, granulating, sieving, pressing and molding the sieved granules, and finally sintering to obtain the temperature-stable microwave dielectric ceramic with low loss and low dielectric constant; wherein, in composition expression aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3Wherein a, b, c and d each independently represent a mole percentage, and satisfy the following condition: a is more than or equal to 50 mol% and less than or equal to 60 mol%, b is more than or equal to 20 mol% and less than or equal to 30 mol%, c is more than or equal to 10 mol% and less than or equal to 20 mol%, d is more than or equal to 10 mol% and less than or equal to 20 mol%, and a + b + c + d is equal to 100 mol%.
Further, Mg therein2SiO4The powder is MgO and SiO2Synthesizing raw materials; mg (magnesium)2TiO4The powder is MgO and TiO2Synthesized as raw material, CaTiO3The powder material is CaO and TiO2Is synthesized by raw materials.
Further, the roasting process in the step (1) is roasting and heat preservation for 3-5 hours at the temperature of 1000-1200 ℃.
Further, the sintering process in the step (2) is sintering at 1300-1380 ℃ for 3-8 h.
Further, the granulation in the step (2) is to mix the dried powder with a binder and then prepare micron-sized spherical particles.
Still further, 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 (2), the granules are pressed into cylinders with the diameter of 10mm and the height of 6 mm.
Compared with the prior art, the invention has the following beneficial effects: the invention adopts positive temperature coefficient CaTiO3Phase and negative temperature coefficient Mg2SiO4、Mg2TiO4The phases are compositely compensated, and unsaturated ceramic phase Li is introduced2NdO3Doping is carried out, the ceramic phase Li2NdO3High Q value of (2) compensates for CaTiO3Low Q value of ceramic phase, and Li ceramic phase2NdO3And a strongly complementary temperature coefficient, in the presence of Mg2SiO4And CaTiO3On the premise of phase, the ceramic has excellent adjustment effect on the temperature coefficient of the finally synthesized ceramic, so that the final ceramic has a near-zero temperature coefficient of resonant frequency, and the low dielectric constant of the final ceramic is reduced, so that the dielectric constant requirement of ultrahigh frequency band application is met. The invention relates to a method for preparing a titanium dioxide coating by using CaTiO3Phase, Mg2SiO4Phase, Mg2TiO4Phase, Li2NdO3The matching and complementation of the microwave dielectric ceramic and the ceramic are realized, and the microwave dielectric ceramic with lower dielectric constant, higher quality factor and better temperature stability is finally obtained; in addition, the preparation process is simple, the price of the adopted raw materials is moderate, no pollution is caused, and the industrialization prospect is good.
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 low-loss low-dielectric constant temperature stable microwave dielectric ceramic, and the composition expression is aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3Wherein a, b, c and d independently represent mole percentages, and satisfy the following conditions: a is more than or equal to 50 mol% and less than or equal to 60 mol%, b is more than or equal to 20 mol% and less than or equal to 30 mol%, c is more than or equal to 10 mol% and less than or equal to 20 mol%, d is more than or equal to 10 mol% and less than or equal to 20 mol%, and a + b + c + d is equal to 100 mol%. The dielectric constant of the microwave dielectric ceramic is 9-11, the Q x f value of the quality factor is 95000-150000 GHz, and the temperature coefficient of the resonance frequency is-2-10 ppm/DEG C.
The preparation method of the temperature-stable microwave dielectric ceramic with low loss and low dielectric constant comprises the following steps:
(1) unsaturated ceramic phase Li2NdO3Synthesis of (2)
Mixing Li2CO3Powder and Nd2O3The powder is according to the chemical formula Li2NdO3Mixing the corresponding elements in the mixture according to the molar ratio of the Li2CO3And Nd2O3Mixing, fully ball-milling, drying and sieving after ball-milling, and then placing the mixture into a corundum crucible to roast and preserve heat for 3-5 hours at the temperature of 1000-1200 ℃ to obtain Li2NdO3A composition;
(2) with Mg2SiO4Powder material, Mg2TiO4Powder material, CaTiO3Powder material, Li2NdO3The powder is taken as a raw material and is expressed by a composition expression aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3The molar percentages of the respective compositions in (1) are measured for Mg2SiO4Powder material, Mg2TiO4Powder material, CaTiO3Powder material, Li2NdO3Powder, the weighed materials are fully mixed and then are subjected to ball milling, drying, granulation and sieving are carried out after the ball milling, the sieved granules are pressed and formed, and finally, the mixture is sintered for 3-8 hours at the temperature of 1300-1380 ℃ to obtain the temperature stable type microwave dielectric ceramic with low loss and low dielectric constant; wherein, in composition expression aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3Wherein a, b, c and d each independently represent a mole percentage, and satisfy the following condition: a is more than or equal to 50 mol% and less than or equal to 60 mol%, b is more than or equal to 20 mol% and less than or equal to 30 mol%, c is more than or equal to 10 mol% and less than or equal to 20 mol%, d is more than or equal to 10 mol% and less than or equal to 20 mol%, and a + b + c + d is equal to 100 mol%.
Mg in step (2)2SiO4Powder material, Mg2TiO4And CaTiO3The powder is a known raw material, wherein Mg2SiO4The powder is MgO and SiO2The raw materials are synthesized by roasting at 1000-1200 ℃; mg (magnesium)2TiO4The powder is MgO and TiO2The raw materials are synthesized by roasting at 1000-1200 ℃; CaTiO3The powder material is CaO and TiO2The material is synthesized by roasting at 1000-1200 ℃.
And (2) the granulation is to mix the dried powder with a binder and then prepare micron-sized spherical particles. The binder is selected from at least one of polyvinyl alcohol solution, polyvinyl butyral solution, acrylic solution or methyl cellulose.
In the molding in the step (2), the pellet was pressed into a cylinder having a diameter of 10mm and a height of 6 mm.
6 embodiments are designed according to the method of the present invention, the values of a, b, c and d in the composition expression of the microwave dielectric ceramic of the 6 embodiments, the sintering temperature in the step (2) and the microwave dielectric property obtained by testing the microwave dielectric ceramic by using a microwave network analyzer are shown in table 1; further, in the production methods of the respective examples, Mg2SiO4Powder material, Mg2TiO4And CaTiO3The roasting synthesis temperature of the powder is 1000 ℃, and the roasting time is 4 hours.
TABLE 1 values of the parameters of examples 1 to 6 and the microwave dielectric properties of the microwave dielectric ceramics
The invention is further illustrated by comparison with comparative examples below, and the composition expression aMg is specific to microwave dielectric ceramics2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3The values of a, b, c and d and the sintering temperature after granulation and molding in the preparation methods of the microwave dielectric ceramics of comparative example 1, comparative example 2 and comparative example 3 are shown in table 2, and the rest of the preparation processes are the same as the examples of the present invention. The microwave dielectric properties obtained by testing the comparative microwave dielectric ceramics by using a microwave network analyzer are shown in table 2.
TABLE 2 values of the parameters of comparative examples 1 to 3 and the microwave dielectric properties of the microwave dielectric ceramics
As can be seen from tables 1 and 2, compared with the microwave dielectric ceramics of comparative examples 1 to 3, the microwave dielectric ceramics of examples 1 to 6 of the present invention have a lower dielectric constant, a higher quality factor, and a near-zero temperature coefficient of resonant frequency, and have better temperature stability and excellent microwave dielectric comprehensive properties, and can meet the requirement of ultra-high frequency band application.
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 (9)
1. A low-loss low-dielectric-constant temperature-stable microwave dielectric ceramic is characterized in that: its composition expression is aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3Wherein a, b, c and d independently represent mole percentages, and satisfy the following conditions: a is more than or equal to 50 mol% and less than or equal to 60 mol%, b is more than or equal to 20 mol% and less than or equal to 30 mol%, c is more than or equal to 10 mol% and less than or equal to 20 mol%, d is more than or equal to 10 mol% and less than or equal to 20 mol%, and a + b + c + d is equal to 100 mol%.
2. The low loss, low dielectric constant temperature stable microwave dielectric ceramic of claim 1 further comprising: the dielectric constant of the microwave dielectric ceramic is 9-11, the Q x f value of the quality factor is 95000-150000 GHz, and the temperature coefficient of the resonance frequency is-2-10 ppm/DEG C.
3. A method for preparing the low-loss low-dielectric-constant temperature-stable microwave dielectric ceramic according to claim 1 or 2, comprising the steps of:
(1) unsaturated ceramic phase Li2NdO3Synthesis of (2)
Mixing Li2CO3Powder and Nd2O3The powder is according to the chemical formula Li2NdO3Mixing the corresponding elements in the mixture according to the molar ratio of the Li2CO3And Nd2O3After mixing, fillBall milling, drying, sieving, calcining in corundum crucible to obtain Li2NdO3A composition;
(2) with Mg2SiO4Powder material, Mg2TiO4Powder material, CaTiO3Powder material, Li2NdO3The powder is taken as a raw material and is expressed by a composition expression aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3The molar percentages of the respective compositions in (1) are measured for Mg2SiO4Powder material, Mg2TiO4Powder material, CaTiO3Powder material, Li2NdO3Powder, the weighed materials are fully mixed and then ball-milled, the ball-milled materials are dried, granulated and sieved, the sieved granules are pressed and formed, and finally the temperature stable type microwave dielectric ceramic with low loss and low dielectric constant is obtained by sintering; wherein, in composition expression aMg2SiO4-bMg2TiO4-cCaTiO3-dLi2NdO3Wherein a, b, c and d each independently represent a mole percentage, and satisfy the following condition: a is more than or equal to 50 mol% and less than or equal to 60 mol%, b is more than or equal to 20 mol% and less than or equal to 30 mol%, c is more than or equal to 10 mol% and less than or equal to 20 mol%, d is more than or equal to 10 mol% and less than or equal to 20 mol%, and a + b + c + d is equal to 100 mol%.
4. The method of claim 3, wherein Mg is added to the microwave dielectric ceramic to form a low-loss, low-dielectric-constant temperature-stable microwave dielectric ceramic2SiO4The powder is MgO and SiO2Synthesizing raw materials; mg (magnesium)2TiO4The powder is MgO and TiO2Synthesized as raw material, CaTiO3The powder material is CaO and TiO2Is synthesized by raw materials.
5. The method for preparing the temperature stable microwave dielectric ceramic with low loss and low dielectric constant as claimed in claim 3, wherein the firing process in step (1) is firing at 1000-1200 ℃ for 3-5 h.
6. The method for preparing a temperature stable microwave dielectric ceramic with low loss and low dielectric constant as claimed in claim 3, wherein the sintering process in step (2) is sintering at 1300-1380 ℃ for 3-8 h.
7. The method according to claim 3, wherein the step (2) of granulating comprises mixing the dried powder with a binder, and then making micron-sized spherical particles.
8. The method of claim 7, wherein the binder is selected from at least one of a polyvinyl alcohol solution, a polyvinyl butyral solution, an acrylic solution, and methyl cellulose.
9. The method of claim 3, wherein in step (2), the particles are pressed into a cylinder with a diameter of 10mm and a height of 6 mm.
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Cited By (5)
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| CN113105231A (en) * | 2021-04-12 | 2021-07-13 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material and preparation method thereof |
| CN113896524A (en) * | 2021-11-18 | 2022-01-07 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | High-temperature stable low-dielectric constant microwave dielectric ceramic and preparation method thereof |
| CN113896531A (en) * | 2021-11-09 | 2022-01-07 | 济南大学 | Low-loss composite microwave dielectric ceramic with stable temperature and preparation method thereof |
| CN114180949A (en) * | 2021-12-16 | 2022-03-15 | 大富科技(安徽)股份有限公司 | Ceramic material and preparation method thereof, and ceramic sintered body and preparation method thereof |
| CN116102347A (en) * | 2022-12-23 | 2023-05-12 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | High-dielectric-constant microwave dielectric ceramic for MLCC (multi-layer ceramic) and preparation method thereof |
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| CN113105231A (en) * | 2021-04-12 | 2021-07-13 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material and preparation method thereof |
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| CN113896524A (en) * | 2021-11-18 | 2022-01-07 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | High-temperature stable low-dielectric constant microwave dielectric ceramic and preparation method thereof |
| CN114180949A (en) * | 2021-12-16 | 2022-03-15 | 大富科技(安徽)股份有限公司 | Ceramic material and preparation method thereof, and ceramic sintered body and preparation method thereof |
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