CN112521149A - high-Q-value microwave dielectric ceramic powder, microwave dielectric ceramic, preparation method and application - Google Patents
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Abstract
The invention discloses a high Q value microwave dielectric ceramic and a preparation method and application thereof, wherein the microwave dielectric ceramic has a composition expression of Ba6‑3x(La1‑y‑zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratios respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075. The invention also discloses the high-Q-value microwave dielectric ceramic powder. The microwave dielectric ceramic does not contain Nd element, has low production cost and dielectric constant of about 90, can meet the use requirements of microwave components required by base station construction and the like, has near-zero temperature coefficient of resonant frequency, good temperature stability, higher quality factor (Qxf) and better comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of microwave dielectric ceramics, and particularly relates to high-Q-value microwave dielectric ceramic powder, microwave dielectric ceramics, a preparation method and application.
Background
With the development of the international and domestic mobile communication industry toward 5G, a large number of ceramic filters having a dielectric constant of 90 have been used in the construction of base stations for mobile communication. At present, the domestic microwave dielectric ceramic powder with the dielectric constant of 90 and the high Q multiplied by F value is almost monopolized by Japan at the present stage, and the raw material powder with the specification used in other countries needs to be imported from Japan and has expensive price and long delivery time. In addition, the microwave dielectric ceramic material having a dielectric constant of 90 generally contains Nd only2O3In case of (2), a high Q value can be obtained; however, Nd2O3Is a relatively expensive raw material in the rare earth group; this is because the amount of Nd element is not large in the world. In addition, the existing microwave dielectric ceramics with dielectric constant of about 90 cannot simultaneously obtain higher qualityThe factor and the temperature coefficient of the resonance frequency close to zero, namely the comprehensive performance is not ideal; therefore, it is required to develop a composition containing no Nd2O3The microwave dielectric ceramic powder and the microwave dielectric ceramic with high Q value, medium dielectric constant and near-zero temperature coefficient of resonance frequency.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide high-Q-value microwave dielectric ceramic powder, microwave dielectric ceramic, a preparation method and application. The microwave dielectric ceramic powder does not contain Nd2O3The microwave dielectric ceramic has the advantages of low production cost, good temperature stability, high quality factor, low dielectric loss and excellent comprehensive performance.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme: a high-Q microwave dielectric ceramic has Ba as its composition expression6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratios respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
Furthermore, the preparation raw materials of the high-Q-value microwave dielectric ceramic comprise barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide, and the mass ratio of the barium carbonate, the lanthanum oxide, the samarium oxide, the bismuth oxide and the titanium oxide is expressed according to a composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54The molar ratio of each element in (1) is calculated.
Preferably, in the composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein y is 0.7 and z is 0.06.
The invention also provides a preparation method of the high-Q microwave dielectric ceramic, which comprises the following steps:
(1) according to composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Molar ratio of each element in BaCO3Powder, La2O3Powder Sm2O3Powder of Bi2O3Powder, TiO2The powder is proportioned, ball-milled after being fully mixed, dried and sieved after ball-milling, and then the powder is put into a corundum crucible for roasting to obtain pre-sintered powder; wherein, the composition expression is Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratio respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
(2) Fully ball-milling the pre-sintered powder obtained in the step (1), and drying, granulating and sieving to obtain granulated powder;
(3) and (3) pressing and molding the granulated powder obtained in the step (2), and finally sintering to obtain the microwave dielectric ceramic with high Q value and low loss.
Further, the roasting temperature in the step (1) is 1100-1150 ℃, and the roasting time is 4-5 hours.
Further, the sintering temperature in the step (3) is 1200-1350 ℃, and the sintering time is 4-5 hours.
Further, the granulation process in the step (2) is to mix the pre-sintered powder material and the granulating agent and then prepare the mixture into micron-sized spherical particles; the granulation process adopts a centrifugal spray granulation process, and the granulating agent is added into the pre-sintering powder in a spray form; the granulating agent comprises deionized water, a dispersing agent, glue, a plasticizer and a release agent, wherein the mass ratio of the powder, the deionized water, the dispersing agent, the glue, the plasticizer and the release agent is 200:190:1:10: 2.
Further, in the step (3), the granulated powder is pressed into a cylinder with the diameter of 15mm and the height of 6 mm.
The invention further provides high-Q-value microwave dielectric ceramic powder for preparing the microwave dielectric ceramic, which comprises barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide, wherein the mass ratio of the barium carbonate, the lanthanum oxide, the samarium oxide, the bismuth oxide and the titanium oxide is expressed as Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54The molar ratio of each element in the composition expression Ba is calculated6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratio respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
The invention also provides application of the high-Q microwave dielectric ceramic to microwave components, wherein the microwave components comprise a resonator, a filter, a dielectric antenna, a dielectric guided wave loop and the like.
The invention has the beneficial effects that:
the microwave dielectric ceramic powder does not contain Nd2O3The method adopts mixed powder containing barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide, and the design principle of the mixture ratio of each component in the mixed powder is as follows: according to composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein x, y and z represent the molar ratio respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075. The microwave dielectric ceramic powder does not contain Nd2O3The production cost of the microwave dielectric ceramic is reduced, and Ba can be obtained6-3x(La1-y-zSmyBiz)8+2xTi18O54Structural microwave dielectric ceramics; the microwave dielectric ceramic with the structure does not contain Nd element, has low production cost and dielectric constant of about 90, can meet the use requirements of microwave components required by base station construction and the like, has near-zero temperature coefficient of resonant frequency, good temperature stability, higher quality factor (Qf) and better comprehensive performance.
The microwave dielectric ceramic is applied to microwave components, can improve the electrical property of the microwave components such as a cavity filter, particularly reduce the insertion loss of the filter, and obtain a more stable temperature coefficient so as to reduce the influence of the filter on the filter due to the use environment factors in the actual use.
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 Q value microwave dielectric ceramic, the composition expression of which is Ba6-3x(La1-y-zSmyBiz)8+ 2xTi18O54Wherein x, y and z represent molar ratios respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075. Preferably, in the composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein y is 0.7 and z is 0.06.
The preparation raw materials of the high-Q-value microwave dielectric ceramic comprise barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide, and the mass ratio of the barium carbonate, the lanthanum oxide, the samarium oxide, the bismuth oxide and the titanium oxide is expressed according to a composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54The molar ratio of each element in (1) is calculated.
The invention also provides a preparation method of the high-Q microwave dielectric ceramic, which comprises the following steps:
(1) according to composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Molar ratio of each element in BaCO3Powder, La2O3Powder Sm2O3Powder of Bi2O3Powder, TiO2The method comprises the following steps of (1) mixing powder, fully mixing all oxide powder, carrying out ball milling, drying and screening after ball milling, and then putting the mixture into a corundum crucible for roasting to obtain pre-sintered powder; wherein, the composition expression is Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratio respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
(2) Fully ball-milling the pre-sintered powder obtained in the step (1), and drying, granulating and sieving to obtain granulated powder;
(3) and (3) pressing and molding the granulated powder obtained in the step (2), and finally sintering to obtain the microwave dielectric ceramic with high Q value and low loss.
Wherein the roasting temperature in the step (1) is 1100-1150 ℃, and the roasting time is 4-5 h.
Wherein the sintering temperature in the step (3) is 1200-1350 ℃, and the sintering time is 4-5 h.
Wherein, the granulation process in the step (2) is to mix the pre-sintering powder and the granulating agent and then prepare micron-sized spherical particles; the granulation process adopts a centrifugal spray granulation process, and the granulating agent is added into the pre-sintering powder in a spray form; the granulating agent comprises deionized water, a dispersing agent, glue, a plasticizer and a release agent, wherein the mass ratio of the powder, the deionized water, the dispersing agent, the glue, the plasticizer and the release agent is 200:190:1:10: 2.
Wherein, in the step (3), the granulating powder is pressed into a cylinder with the diameter of 15mm and the height of 6 mm.
The invention further provides high-Q-value microwave dielectric ceramic powder for preparing the microwave dielectric ceramic, which comprises barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide, wherein the mass ratio of the barium carbonate, the lanthanum oxide, the samarium oxide, the bismuth oxide and the titanium oxide is expressed as Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54The molar ratio of each element in the composition expression Ba is calculated6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratio respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
The invention also provides application of the high-Q microwave dielectric ceramic to microwave components, wherein the microwave components comprise a resonator, a filter, a dielectric antenna, a dielectric guided wave loop and the like.
The following examples and comparative examples are provided to illustrate the microwave dielectric ceramics of the present invention; composition expression Ba of microwave dielectric ceramic6-3x(La1-y-zSmyBiz)8+2xTi18O54The values of y and z and the properties of the microwave dielectric ceramics are shown in Table 1.
TABLE 1 values of y and z and microwave dielectric ceramic Properties
As can be seen from the comparison between examples 1-6 and comparative examples 1-12, the dielectric constant of the microwave dielectric ceramic of the present invention is about 90, and the microwave dielectric ceramic has a near-zero temperature coefficient (Tcf) of resonant frequency, good temperature stability, a higher quality factor, and better microwave comprehensive performance. Among them, the microwave dielectric ceramic of example 3 is the most excellent in overall performance. The composition expression of the microwave dielectric ceramic of the embodiment 3 is Ba4(La0.24Sm0.7Bi0.06)8+4/3Ti18O54Obtaining the proportion of the microwave dielectric ceramic powder, namely BaCO according to the molar ratio of each element in the composition expression3Powder, La2O3Powder Sm2O3Powder of Bi2O3Powder, TiO2The powder has a mass ratio of 21 Kg: 10 Kg: 30 Kg: 2 Kg: 37 Kg.
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 of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A high Q value microwave dielectric ceramic is characterized in that: the composition expression is Ba6-3x(La1-y-zSmyBiz)8+ 2xTi18O54Wherein x, y and z represent molar ratios respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
2. A high Q microwave dielectric ceramic according to claim 1 wherein: the microwave dielectric ceramic is prepared from barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide according to the mass ratioAccording to composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54The molar ratio of each element in (1) is calculated.
3. A high Q microwave dielectric ceramic according to claim 1 wherein: y is 0.7 and z is 0.06.
4. A preparation method of a high-Q microwave dielectric ceramic is characterized by comprising the following steps:
(1) according to composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54Molar ratio of each element in BaCO3Powder, La2O3Powder Sm2O3Powder of Bi2O3Powder, TiO2The powder is proportioned, ball-milled after being fully mixed, dried and sieved after ball-milling, and then the powder is put into a corundum crucible for roasting to obtain pre-sintered powder; wherein, the composition expression is Ba6-3x(La1-y- zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratio respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
(2) Fully ball-milling the pre-sintered powder obtained in the step (1), and drying, granulating and sieving to obtain granulated powder;
(3) and (3) pressing and molding the granulated powder obtained in the step (2), and finally sintering to obtain the microwave dielectric ceramic with high Q value and low loss.
5. The preparation method of the high-Q microwave dielectric ceramic according to claim 4, characterized in that the roasting temperature in the step (1) is 1100-1150 ℃, and the roasting time is 4-5 h.
6. The method for preparing microwave dielectric ceramic with high Q value according to claim 4, wherein the sintering temperature in step (3) is 1200-1350 ℃ and the sintering time is 4-5 h.
7. The method for preparing microwave dielectric ceramic with high Q value as claimed in claim 4, wherein the granulating process in step (2) is mixing the pre-sintered powder and the granulating agent, and then making into micron-sized spherical particles; the granulation process adopts a centrifugal spray granulation process, and the granulating agent is added into the pre-sintering powder in a spray form; the granulating agent comprises deionized water, a dispersing agent, glue, a plasticizer and a release agent, wherein the mass ratio of the powder, the deionized water, the dispersing agent, the glue, the plasticizer and the release agent is 200:190:1:10: 2.
8. The method for preparing microwave dielectric ceramic with high Q value as claimed in claim 4, wherein in step (3), the granulated powder is pressed into a cylinder with diameter of 15mm and height of 6 mm.
9. A high Q value microwave dielectric ceramic powder used for preparing the microwave dielectric ceramic of any one of claims 1 to 3, characterized by comprising barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide, wherein the mass ratio of barium carbonate, lanthanum oxide, samarium oxide, bismuth oxide and titanium oxide is according to the composition expression Ba6-3x(La1-y-zSmyBiz)8+2xTi18O54The molar ratio of each element in the composition expression Ba is calculated6-3x(La1-y-zSmyBiz)8+2xTi18O54Wherein x, y and z represent molar ratio respectively, and x is 2/3, y is 0.7 and z is 0.05-0.075.
10. Use of the high-Q microwave dielectric ceramic of any one of claims 1 to 3 in microwave components.
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| CN114180956A (en) * | 2021-12-20 | 2022-03-15 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Microwave dielectric ceramic for high-dielectric-constant 5G waveguide and preparation method and application thereof |
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| CN109320245A (en) * | 2018-11-29 | 2019-02-12 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | A kind of microwave-medium ceramics and preparation method thereof |
| CN110423117A (en) * | 2019-07-15 | 2019-11-08 | 深圳顺络电子股份有限公司 | A kind of high q-factor microwave dielectric ceramic materials and preparation method thereof |
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| CN109320245A (en) * | 2018-11-29 | 2019-02-12 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | A kind of microwave-medium ceramics and preparation method thereof |
| CN110423117A (en) * | 2019-07-15 | 2019-11-08 | 深圳顺络电子股份有限公司 | A kind of high q-factor microwave dielectric ceramic materials and preparation method thereof |
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| N. QIN, X.M. CHEN: "Effects of Sm/Bi co-substitution on microstructures and microwave dielectric characteristics of Ba6−3xLa8+2xTi18O54 (x = 2/3) solid solution", 《MATERIALS SCIENCE AND ENGINEERING B》 * |
| SHALINI BAHEL，S. BINDRA NARANG: "Temperature Dependent Dielectric Properties of Ba-La-Sm-Bi-Ti-O Ceramic System", 《INTEGRATED FERROELECTRICS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114180956A (en) * | 2021-12-20 | 2022-03-15 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Microwave dielectric ceramic for high-dielectric-constant 5G waveguide and preparation method and application thereof |
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Application publication date: 20210319 |