CN110790576A - Microwave ceramic powder material and preparation method thereof - Google Patents

Microwave ceramic powder material and preparation method thereof Download PDF

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CN110790576A
CN110790576A CN201911217017.1A CN201911217017A CN110790576A CN 110790576 A CN110790576 A CN 110790576A CN 201911217017 A CN201911217017 A CN 201911217017A CN 110790576 A CN110790576 A CN 110790576A
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ceramic powder
powder material
microwave ceramic
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王孝国
宋永生
陈繁欢
周永响
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Guangdong Fenghua Advanced Tech Holding Co Ltd
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Abstract

The invention discloses a microwave ceramic powder material, which comprises a main crystal phase and a modified additive, wherein the structural formula of the main crystal phase is Ca1+xSm1‑xAl1‑xTixO4The modifying additive is Mg (OH)2、MnCO3、SiO2、CeO2、Y2O3At least one of; wherein x is 0 to 0.4. The CaSmAlO4 system functional material provided by the invention can obtain higher Q value, the total temperature drift (-40-85 ℃) is close to 0, the K value is 20.5 +/-0.5 and can be adjusted, and expensive Japanese imported porcelain powder can be replaced. Meanwhile, the invention also discloses a preparation method of the microwave ceramic powder material.

Description

Microwave ceramic powder material and preparation method thereof
Technical Field
The invention relates to a ceramic powder material, in particular to a microwave ceramic powder material and a preparation method thereof.
Background
At present, microwave dielectric ceramics are mainly used for manufacturing resonators, filters, microwave capacitors, dielectric substrates, dielectric antennas, dielectric waveguides and the like, play more and more roles in the aspects of portable mobile phones, automobile phones, cordless phones, microwave base stations, satellite television receivers, W-LANs, automobile anti-collision radars, military radars and the like, and are widely applied.
With the advent of 5G technology, higher frequencies (7.5GHz) have been used, and the demand for microwave ceramic powders with low dielectric constants of 20 + -1 has increased. The Mg0.95Ca0.05TiO3 system is generally used in the market at present, but the machining performance of the bulk system material after being made into porcelain is poor: bending strength is less than 150MPa, and hardness is less than 600Kg/mm2And because the terminal resonator product is mostly a special-shaped piece, the periphery is very easy to break when a customer polishes or drills the porcelain body, and the inside of the porcelain body also has the defects of invisible cracking and the like, so that the performance of a finished product is deteriorated, and the resonance frequency drifts and is unstable. The main reason is that the system material is sensitive to the firing temperature when being made into porcelain, and the interior of the porcelain body is easy to crystallize and is in a glass state, so that the machining characteristics of the porcelain body such as bending strength, hardness and the like and stable temperature drift are difficult to ensure.
Therefore, a new material system with excellent machining characteristics, controllable K value, total temperature drift close to 0 and high Q value is urgently needed to be found.
Disclosure of Invention
Due to Mg0.95Ca0.05TiO3The poor machining characteristics of the system can not be found in China, so that the device manufacturers have to import expensive Japanese porcelain powder. In order to break the technical monopoly of Japan in the field, the application independently develops a new material system with better machining characteristics, preferably CaSmAlO4System, but CaSmAlO alone4Dielectric constant ε r of single crystal: 19.2, Qf: 77800,. tau.f (ppm/. degree. C.): and 11, increasing the epsilon r and the tau f on the premise of ensuring the Qf value on the premise that the epsilon r is slightly low and the tau f is negative. This patent is based on a material with a positive τ f: ca2TiO4(a non-existent substance), with CaSmAlO4Solid solution, the two forms a solid solution, the crystal structure can be effectively cut, and the chemical formula (1-x) CaSmAlO is synthesized after cutting4-xCa2TiO4Or Ca1+xSm1-xAl1-xTixO4A solid solution of (2).
The CaSmAlO4 system functional material provided by the invention can well solve the problems, can obtain a higher Q value, has a total temperature drift of (-40-85 ℃) close to 0 and an adjustable K value of 20.5 +/-0.5, and can replace expensive Japanese imported porcelain powder.
The CaSmAlO4 system adopted by the invention belongs to a K2NiF4 layered perovskite structure, and the bulk material has the advantages of small lattice mismatch, excellent dielectric property, stable chemical property, no structural phase change, no twin crystal and the like, thereby showing the machining characteristics of higher bending strength, hardness and the like, high Q value and stable temperature drift.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a microwave ceramic powder material comprises a main crystal phase and a modified additive, wherein the structural formula of the main crystal phase is Ca1+xSm1-xAl1-xTixO4The modifying additive is Mg (OH)2、MnCO3、SiO2、CeO2、Y2O3At least one of; wherein x is 0 to 0.4.
Preferably, the microwave ceramic powder material comprises the following components in parts by mole: main crystal phase Ca1+xSm1-xAl1- xTixO492.5-97.5 parts and 2.5-7.5 parts of modified additive.
Preferably, the modifying additive is Mg (OH)2、MnCO3、SiO2、CeO2And Y2O3And (4) compounding. The selection of the modified additive can better improve the Qf value and finely adjust the Tf value and is beneficial to adjusting the burning temperature.
More preferably, the modifying additive comprises the following components in molar parts: mg (OH)20.5 to 1.5 parts of MnCO30.5 to 2.5 parts of SiO20.5 to 1.0 part of CeO20.5 to 1.0 part and Y2O30.5 to 1.5 portions. The selection of the modifying additive can improve the Qf value and finely adjust the Tf value, and is helpful for adjusting the burning temperature.
Preferably, the specific technical indexes of the microwave ceramic powder material are as follows: ε r: 20 to 21 parts by weight; qf value: 80000 or more; τ f (ppm/. degree. C.): +/-1.5 ppm (-40-25 deg.C; 25-85 deg.C; 40-85 deg.C; respectively negative temperature section, positive temperature section and full temperature section).
Meanwhile, the invention also discloses a preparation method of the microwave ceramic powder material, which comprises the following steps:
(1) using superfine, high-purity main raw material CaCO3、Sm2O3、Al2O3、TiO2Solid-phase one-step synthesis of main crystal phase Ca1+ xSm1-xAl1-xTixO4(x＝0-0.4)；
(2) And (2) mixing the main crystal phase obtained in the step (1) with a modified additive by a wet method, grinding, refining and granulating to obtain the microwave ceramic powder material.
Preferably, the specific surface area of the main raw material is 9-11 m2/g。
Preferably, the specific process in step (1) is as follows: the method comprises the following steps of mixing, grinding and drying the main raw materials by a wet method, then putting the main raw materials into a roller kiln or a high-temperature tunnel long furnace, heating the main raw materials from room temperature to the temperature of a high-temperature area, preserving heat in the high-temperature area, and finally cooling the main raw materials to the room temperature, wherein the heating process is 3-6 hours, the heat preservation process is 2.5-5 hours, the room temperature is 0-40 ℃, and the temperature of the high-temperature area is 1180-1220 ℃.
Preferably, in the step (2), the particle size of the microwave ceramic powder material (after glue adding and granulation) is 60-100 μm.
In the application, the superfine raw materials are selected, so that the complete synthesis of the main crystal phase is facilitated; the heat preservation time is sufficient, which is beneficial to the synthesis of crystal phase; the particle size of the granulated powder is 60-100 mu m, and the granules have good fluidity and good distribution and are beneficial to molding.
Compared with the prior art, the invention has the beneficial effects that:
the product of the invention achieves the same machining characteristics and excellent microwave dielectric property of the Japanese imported porcelain powder, has low loss, high Q value and full temperature drift close to 0, realizes the localization of the porcelain powder, and greatly reduces the manufacturing cost for domestic microwave device manufacturers: more than 50 yuan/Kg.
The K21A porcelain powder manufactured by the invention is supplied to customers for batch use, the molding pressure is less than 90Mpa, the machining performance is excellent, and the microwave dielectric property is stable.
Drawings
FIG. 1 is a sectional view of a ceramic body of the microwave ceramic powder material of the present application.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
The components and contents of the embodiments 1 to 10 are shown in Table 1:
TABLE 1
The specific surface area of the alloy is 9 to 11m in examples 1 to 10 in Table 12CaCO/g as a superfine, highly pure main raw material3、Sm2O3、Al2O3、TiO2Fully mixing by a wet method, selecting zirconium balls with phi of 0.3mm and phi of 0.1mm, grinding and refining in a grading way, spraying and drying by a two-fluid spraying tower, putting the mixture into a roller kiln or a high-temperature tunnel long furnace, raising the temperature from room temperature to the temperature of a high-temperature area, preserving the heat of the high-temperature area, and finally cooling to the room temperature, wherein the temperature raising process is 3-6 hours, the heat preservation process is 2.5-5 hours, the room temperature is 20 +/-20 ℃, and the temperature of the high-temperature area is 1200 +/-20 ℃. And dispersing the obtained pre-sintered material and a modification additive for the second time, grinding, adding glue, and performing spray granulation to obtain solid spherical particles with high apparent density and the particle size of 60-100 microns. The functional material is made into various special-shaped parts of resonators and filters by dry pressing and molding of customers, and is sintered at 1400 ℃ in an air atmosphere, and the performance test parameters of the functional material are shown in materials 1-10 in Table 2.
TABLE 2 Ca1+xSm1-xAl1-xTixO4Performance of functional material
Figure BDA0002296937360000042
Figure BDA0002296937360000051
And (4) conclusion: the microwave ceramic powder materials in the embodiments 1-10 of the application have good machining characteristics, excellent microwave dielectric properties, low loss, high Q value and total temperature drift close to 0; in particular, in example 8, when x is 0.28 and a proper amount of the modifying additive is added, the dielectric constant is 20 to 21, the Qf value is the highest, the machining characteristics are good, the ceramic body is also reflected on the crystal grains of the section of the ceramic body, and the ceramic body is dense and has few pores, as shown in fig. 1.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (9)

1. The microwave ceramic powder material is characterized by comprising a main crystal phase and a modified additive, wherein the structural formula of the main crystal phase is Ca1+xSm1-xAl1-xTixO4The modifying additive is Mg (OH)2、MnCO3、SiO2、CeO2、Y2O3At least one of; wherein x is 0 to 0.4.
2. The microwave ceramic powder material according to claim 1, comprising the following components in parts by mole: main crystal phase Ca1+xSm1-xAl1-xTixO492.5-97.5 parts and 2.5-7.5 parts of modified additive.
3. The microwave ceramic powder material according to claim 1, wherein the modifying additive is Mg (OH)2、MnCO3、SiO2、CeO2And Y2O3And (4) compounding.
4. The microwave ceramic powder of claim 3The material is characterized in that the modified additive comprises the following components in parts by mole: mg (OH)20.5 to 1.5 parts of MnCO30.5 to 2.5 parts of SiO20.5 to 1.0 part of CeO20.5 to 1.0 part and Y2O30.5 to 1.5 portions.
5. The microwave ceramic powder material according to any one of claims 1 to 4, wherein the specific technical indexes of the microwave ceramic powder material are as follows: ε r: 20 to 21 parts by weight; qf value: 80000 or more; τ f (ppm/. degree. C.): +/-1.5 ppm (-40-25 deg.C; 25-85 deg.C; 40-85 deg.C; respectively negative temperature section, positive temperature section and full temperature section).
6. The method for preparing the microwave ceramic powder material according to any one of claims 1 to 5, comprising the following steps:
(1) using superfine, high-purity main raw material CaCO3、Sm2O3、Al2O3、TiO2Solid-phase one-step synthesis of main crystal phase Ca1+xSm1- xAl1-xTixO4；
(2) And (2) mixing the main crystal phase obtained in the step (1) with a modified additive by a wet method, grinding, refining and granulating to obtain the microwave ceramic powder material.
7. The method for preparing a microwave ceramic powder material according to claim 6, wherein the specific surface area of the main raw material is 9-11 m2/g。
8. The method for preparing a microwave ceramic powder material according to claim 6, wherein the specific process in the step (1) is as follows: the method comprises the following steps of mixing, grinding and drying the main raw materials by a wet method, then putting the main raw materials into a roller kiln or a high-temperature tunnel long furnace, heating the main raw materials from room temperature to the temperature of a high-temperature area, preserving heat in the high-temperature area, and finally cooling the main raw materials to the room temperature, wherein the heating process is 3-6 hours, the heat preservation process is 2.5-5 hours, the room temperature is 0-40 ℃, and the temperature of the high-temperature area is 1180-1220 ℃.
9. The method for preparing the microwave ceramic powder material according to claim 6, wherein in the step (2), the particle size of the microwave ceramic powder material is 60-100 μm.
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CN113213932A (en) * 2021-05-28 2021-08-06 齐鲁工业大学 Calcium-samarium-titanium microwave dielectric ceramic and preparation method thereof
CN113354413A (en) * 2021-07-05 2021-09-07 清华大学 Layered medium-high dielectric constant low-loss microwave dielectric ceramic and preparation method thereof
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111302787A (en) * 2020-04-03 2020-06-19 厦门松元电子有限公司 Microwave dielectric ceramic material with high Qf and high strength and preparation method thereof
CN113213932A (en) * 2021-05-28 2021-08-06 齐鲁工业大学 Calcium-samarium-titanium microwave dielectric ceramic and preparation method thereof
CN113354413A (en) * 2021-07-05 2021-09-07 清华大学 Layered medium-high dielectric constant low-loss microwave dielectric ceramic and preparation method thereof
CN116969760A (en) * 2023-08-01 2023-10-31 陕西华星电子开发有限公司 Ca-Sm-Al-Ti-based microwave dielectric ceramic material and preparation method thereof

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