CN111517786A - Microwave dielectric ceramic powder, preparation method thereof, microwave dielectric ceramic and microwave component - Google Patents
Microwave dielectric ceramic powder, preparation method thereof, microwave dielectric ceramic and microwave component Download PDFInfo
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Abstract
The invention discloses microwave dielectric ceramic powder, a preparation method thereof, microwave dielectric ceramic and a microwave component, wherein the microwave dielectric ceramic powder is microwave dielectric ceramic powder with a dielectric constant of 20 and a ceramic quality factor value of more than 80000, and the microwave dielectric ceramic powder comprises powder comprising titanium dioxide, magnesium oxide, zinc oxide, calcium titanate, zirconium dioxide and trace additive MnSO in a weight ratio of 270: 155: 40: 30: 54.H2And O. The invention can obtain higher Q value and more stable temperature coefficient than the common ceramic raw material with the dielectric constant of 20Q xfo ceramic quality factor]The invention also discloses a preparation method of the microwave dielectric ceramic powder, microwave dielectric ceramic using the microwave dielectric ceramic powder and a microwave component, wherein the original 58000 is improved to more than 80000.
Description
Technical Field
The invention relates to the technical field of ceramic powder, in particular to microwave dielectric ceramic powder, a preparation method thereof, microwave dielectric ceramic and a microwave component.
Background
The 5G mobile communication base station system needs to use a dielectric ceramic filter, and the most core raw material for producing the dielectric ceramic filter is microwave dielectric ceramic powder with the dielectric constant of 20 and the QXFO value of more than 80000. The ceramic powder is mainly used for dielectric ceramic filters, and can be used for mobile communication, satellite communication, military radars and other aspects. With the development of scientific technology, the amount of communication information is rapidly increased, and the requirements of people on wireless communication, the use of microwave communication systems such as satellite communication and satellite direct broadcast television becomes a necessary trend for the development of current communication technology.
The microwave dielectric ceramic is a novel functional ceramic developed in recent decades and is a key material for manufacturing microwave dielectric resonators and filters. On the basis of the original microwave ferrite, the formula and the manufacturing process are greatly upgraded and updated, so that the microwave ferrite has excellent performances of high dielectric constant, low microwave loss, small temperature coefficient and the like, is suitable for manufacturing various modern microwave devices, such as frequency stabilization oscillators, filters, duplexers and the like in equipment such as electronic countermeasure, navigation, communication, radar, household satellite direct broadcast television receivers, mobile phones and the like, and can meet the requirements of microwave circuit miniaturization, integration, high reliability and low cost.
The microwave dielectric ceramic material with a dielectric constant of 20 is developed most rapidly and preferably in Japan, and the production level of microwave ceramic materials and devices is highest by Murata [ Cuntia ] company, Trans-Tech company in Japan, Filtronic [ Feika ] company in England and the like, and the annual value is more than billion dollars. With the development of the international and domestic mobile communication industry toward 5G, a large number of dielectric ceramic filters having a dielectric constant of 20 are required for the construction of base stations for mobile communication. At present, the high QxFo (ceramic quality factor) value of the dielectric constant 20 in China is between 58000 and 60000, and the ceramic quality factor value is lower, so that the use requirement cannot be met.
Disclosure of Invention
In view of the above, the present invention provides a microwave dielectric ceramic powder, a method for preparing the same, a microwave dielectric ceramic, and a microwave device, which can significantly improve the electrical performance of a microwave device 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 practical use of the filter, and according to the ceramic material formula of the present invention, a higher Q value and a more stable temperature coefficient can be obtained compared with the ceramic material with a general dielectric constant of 20. The dielectric constant is a very critical characteristic, and different dielectric constants and ceramic powders have different compositions.
In order to achieve the purpose, the invention adopts the following technical scheme:
a microwave dielectric ceramic powder with dielectric constant of 20 and ceramic quality factor value up to 80000 or more comprises powder including titanium dioxide, magnesium oxide, zinc oxide, calcium titanate, zirconium dioxide and trace additive MnSO at a weight ratio of 270: 155: 40: 30: 54.H2O; wherein, the microwave dielectric ceramic powder also comprises deionized water, a dispersing agent, glue, a release agent and a defoaming agent during centrifugal spraying; the weight ratio of the powder, deionized water, dispersant, glue, release agent and defoamer is 500: 375: 2.5: 60: 3.5: 0.5.
Preferably, the type of the dispersant is SF 8;
preferably, the glue is polyvinyl alcohol with the model number of 1750.
Preferably, the mold release agent is LU 6418;
preferably, the DEFOAMER is DEFOAMER-466.
A preparation method of microwave dielectric ceramic powder comprises the following steps:
a. weighing: in parts by weightTitanium dioxide, magnesium oxide, zinc oxide, calcium titanate, zirconium dioxide and trace amounts of MnSO 1 part by weight at a ratio of 270: 155: 40: 30: 54.H2O obtaining the powder;
b. mixing, by weight parts, the powder, deionized water, and dispersant at a ratio of 500: 375: 2.5 to obtain a mixture;
c. ball milling, namely pouring the mixture into a circulating stirring ball milling barrel added with phi 6 grinding balls for grinding for 8 hours, wherein the particle size of ground slurry is less than 0.6 mu m after grinding;
d. drying, namely using a centrifugal spray drying tower to induce air at the temperature of 100 +/-5 ℃, blowing air at the temperature of 250 +/-5 ℃, and carrying out atomization at the rotation speed of 22Hz and feeding at the speed of 40 Hz;
e. calcining, namely filling the powder obtained in the step d into an alumina crucible, and circulating the tunnel kiln at the temperature of 1100 +/-5 ℃ for 4.0 hours;
f. crushing: all pass through a 100-mesh screen;
g. and (3) secondary grinding: mixing powder (500: 250: 2.5: 60: 3.5: 0.5 wt.%), deionized water, dispersant, glue, demoulding agent and defoaming agent, and grinding in a circulating stirring ball mill with 6 grinding balls for 2 hr;
h. and (3) granulation: and g, granulating the slurry obtained in the step g by using a centrifugal spraying tower, wherein the induced air temperature is 100 +/-5 ℃, the air supply temperature is 250 +/-5 ℃, the rotating speed of an atomizing disc is 20Hz, and the particle size of the produced powder is 80-120 mu m.
A microwave dielectric ceramic is prepared from the microwave dielectric ceramic powder.
A microwave component is made of the microwave dielectric ceramic powder.
Preferably, the microwave component is one of a resonator, a filter, a dielectric antenna and a dielectric guided wave loop.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
the microwave dielectric ceramic powder prepared by the formula has the dielectric constant of 20, the QxFo (ceramic quality factor) is improved to more than 80000 from 58000 (compared with the common microwave dielectric ceramic raw material with the dielectric constant of 20), has very high physical and electrical characteristics, can be compared with similar products abroad, has no worse comprehensive performance than that of foreign manufacturers, and achieves the perfect balance of the dielectric constant and the QxFo (ceramic quality factor) value at the frequency lower than 10 GHZ.
Detailed Description
The invention discloses microwave dielectric ceramic powder, which is microwave dielectric ceramic powder with a dielectric constant of 20 and a ceramic quality factor value of more than 80000, and comprises powder comprising titanium dioxide (TiO) with a weight ratio of 270: 155: 40: 30: 52) Magnesium oxide (MgO), zinc oxide (ZnO), calcium titanate (CaTiO)3) Zirconium dioxide (ZrO)2) And trace additive manganese sulfate MnSO4.H2O; wherein, the microwave dielectric ceramic powder also comprises deionized water, a dispersing agent, glue, a release agent and a defoaming agent during centrifugal spraying; the weight ratio of the powder, deionized water, dispersant, glue, release agent and defoamer is 500: 375: 2.5: 60: 3.5: 0.5. Of course, additives such as pigments and the like which do not change the properties of the respective components may also be suitably added in the present invention.
In this embodiment, the deionized water is deionized purified water. The type of the dispersing agent is SF8, the dispersing agent is a special macromolecular amine salt copolymer, colorless transparent liquid, a special dispersing agent for electronic ceramic products and a dispergator, other conductive particles cannot be introduced when the dispersing agent is used, and the sintering degree is low. The glue is polyvinyl alcohol with the model number of 1750, and the danger data are as follows: ignition point, above 70 deg.C (sealed); ignition point, 440 ℃ (laminar), 520 ℃ (floating); flammability, which is a non-hazardous material in the fire law: specifying a combustible; dust outbreak, lower limit of outbreak 35g/m3. The mold release agent is LU6418, means NOPCOCERA stearate LU-6418, has a melting point of 53 ℃ and 30 percent, is a mold release agent for pressing and molding fine ceramics, and is very effective. The model of the defoaming agent is DEFAMER-466 which is aqueous, and has the advantages of quick defoaming, small using amount, no toxicity and easy loss due to burning.
The microwave dielectric ceramic powder at the present stage reaches the state of being pioneered, great creativity needs to be paid after each step of improvement, the value of the ceramic raw material Qxfo (ceramic quality factor) designed by the scheme of the invention can be increased from 58000 to 80000, and the invention also really brings remarkable effect. The microwave dielectric ceramic powder is a microwave dielectric raw material which is developed by our company and has a high QxFo (ceramic quality factor) value and a low loss and a dielectric constant of 20. The ceramic powder can obviously improve the electrical property of microwave components such as cavity filters, particularly reduce the insertion loss of the filters, and obtain more stable temperature coefficients so as to reduce the influence of the filters on the filters due to use environment factors in actual use. The microwave dielectric ceramic material researched and developed by the invention has the dielectric constant of 20, the QxFo (ceramic quality factor) reaches more than 80000, has very high physical and electrical characteristics, can be comparable with similar products abroad, has no worse comprehensive performance than that of foreign manufacturers, and reaches the perfect balance of the dielectric constant and the QxFo (ceramic quality factor) value at the frequency lower than 10 GHZ.
The research and development department of the company researches various microwave dielectric ceramic powders, the microwave dielectric ceramic powder with the dielectric constant of 23 is researched and developed before, while the microwave dielectric ceramic powder with the dielectric constant of 20 is researched and developed at present, the difference of the components of the microwave dielectric ceramic powder and the microwave dielectric ceramic powder is relatively large, and the technological parameters are improved accordingly. The invention improves QxFo (ceramic quality factor) from 58000 to 80000 on the basis of ensuring the basic performance of the original dielectric constant of 23, thereby realizing lean refinement.
The invention also discloses a preparation method of the microwave dielectric ceramic powder, which comprises the following steps as shown in the following table 1:
a. weighing: titanium dioxide, magnesium oxide, zinc oxide, calcium titanate, zirconium dioxide and trace MnSO 1 part by weight at a ratio of 270: 155: 40: 30: 54.H2O obtaining the powder.
b. Mixing, mixing the powder, deionized water and dispersant at a weight ratio of 500: 375: 2.5 to obtain a mixture.
c. Ball milling, namely pouring the mixture into a circulating stirring ball milling barrel added with phi 6 grinding balls for grinding for 8 hours, wherein the particle size of ground slurry is less than 0.6 mu m after grinding.
d. Drying, namely using a centrifugal spray drying tower to induce air at the temperature of 100 +/-5 ℃, blowing air at the temperature of 250 +/-5 ℃, and carrying out atomization at the rotation speed of 22Hz and feeding at the speed of 40 Hz.
e. And (d) calcining, namely filling the powder obtained in the step (d) into an alumina crucible, and circulating the tunnel kiln at the temperature of 1100 +/-5 ℃ for 4.0 hours.
f. Crushing: all pass through a 100-mesh screen.
g. And (3) secondary grinding: mixing powder (500: 250: 2.5: 60: 3.5: 0.5 wt.%), deionized water, disperser, glue, demoulding agent and defoaming agent, and grinding in a cyclic stirring ball mill with 6 grinding balls for 2 hr.
h. And (3) granulation: and g, granulating the slurry obtained in the step g by using a centrifugal spraying tower, wherein the induced air temperature is 100 +/-5 ℃, the air supply temperature is 250 +/-5 ℃, the rotating speed of an atomizing disc is 20Hz, and the particle size of the produced powder is 80-120 mu m.
Table 1: preparation process of microwave dielectric ceramic powder
Table 2: microwave dielectric ceramic powder sintering temperature and dielectric constant test meter
Table 3: microwave dielectric ceramic powder sintering temperature and QxFo test meter
Table 4: microwave dielectric ceramic powder temperature drift coefficient test meter
The invention is explained in further detail:
table 2 shows that the dielectric constant of the invention has no obvious change to the dielectric constant 20 of the invention when the sintering temperature is about plus or minus 10 ℃, and the dielectric constant of the invention has strong electrical constant stability.
Table 3 confirms that the quality factor QxFo value of the invention has no obvious change when the sintering temperature is about plus or minus 10 ℃, the quality factor QxFo value of the invention is very stable, and the QxFo value can reach more than 85000.
Table 4 confirms that the temperature drift coefficient of the invention has no obvious change when the sintering temperature is about plus or minus 10 ℃, and the temperature drift coefficient of the invention is very stable.
The invention also discloses microwave dielectric ceramic which is prepared from the microwave dielectric ceramic powder.
The invention also discloses a microwave component which is made of the microwave dielectric ceramic powder and is one of a resonator, a filter, a dielectric antenna and a dielectric guided wave loop.
The design of the invention is characterized in that: the microwave dielectric ceramic powder prepared by the formula has the dielectric constant of 20, the QxFo (ceramic quality factor) is improved to more than 80000 from 58000 (compared with the common microwave dielectric ceramic raw material with the dielectric constant of 20), has very high physical and electrical characteristics, can be compared with similar products abroad, has no worse comprehensive performance than that of foreign manufacturers, and achieves the perfect balance of the dielectric constant and the QxFo (ceramic quality factor) value at the frequency lower than 10 GHZ.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (9)
1. A microwave dielectric ceramic powder is characterized in that: it is a ceramic quality factor with a dielectric constant of 20Microwave dielectric ceramic powder with element value of 80000 or more comprises powder comprising titanium dioxide, magnesium oxide, zinc oxide, calcium titanate, zirconium dioxide and trace additive MnSO at a weight ratio of 270: 155: 40: 30: 54.H2O; wherein, the microwave dielectric ceramic powder also comprises deionized water, a dispersing agent, glue, a release agent and a defoaming agent during centrifugal spraying; the weight ratio of the powder, deionized water, dispersant, glue, release agent and defoamer is 500: 375: 2.5: 60: 3.5: 0.5.
2. A microwave dielectric ceramic powder in accordance with claim 1, wherein: the type of the dispersant is SF 8.
3. A microwave dielectric ceramic powder in accordance with claim 1, wherein: the glue is polyvinyl alcohol with the model number of 1750.
4. A microwave dielectric ceramic powder in accordance with claim 1, wherein: the mold release agent is LU 6418.
5. A microwave dielectric ceramic powder in accordance with claim 1, wherein: the model of the defoaming agent is DEFAMER-466.
6. A method of preparing a microwave dielectric ceramic powder as claimed in any one of claims 1 to 5, characterized in that: the method comprises the following steps:
a. weighing: titanium dioxide, magnesium oxide, zinc oxide, calcium titanate, zirconium dioxide and trace MnSO 1 part by weight at a ratio of 270: 155: 40: 30: 54.H2O obtaining the powder;
b. mixing, by weight parts, the powder, deionized water, and dispersant at a ratio of 500: 375: 2.5 to obtain a mixture;
c. ball milling, namely pouring the mixture into a circulating stirring ball milling barrel added with phi 6 grinding balls for grinding for 8 hours, wherein the particle size of ground slurry is less than 0.6 mu m after grinding;
d. drying, namely using a centrifugal spray drying tower to induce air at the temperature of 100 +/-5 ℃, blowing air at the temperature of 250 +/-5 ℃, and carrying out atomization at the rotation speed of 22Hz and feeding at the speed of 40 Hz;
e. calcining, namely filling the powder obtained in the step d into an alumina crucible, and circulating the tunnel kiln at the temperature of 1100 +/-5 ℃ for 4.0 hours;
f. crushing: all pass through a 100-mesh screen;
g. and (3) secondary grinding: mixing powder (500: 250: 2.5: 60: 3.5: 0.5 wt.%), deionized water, dispersant, glue, demoulding agent and defoaming agent, and grinding in a circulating stirring ball mill with 6 grinding balls for 2 hr;
h. and (3) granulation: and g, granulating the slurry obtained in the step g by using a centrifugal spraying tower, wherein the induced air temperature is 100 +/-5 ℃, the air supply temperature is 250 +/-5 ℃, the rotating speed of an atomizing disc is 20Hz, and the particle size of the produced powder is 80-120 mu m.
7. A microwave dielectric ceramic, characterized in that: made of a microwave dielectric ceramic powder according to any one of claims 1 to 5.
8. A microwave component is characterized in that: made of a microwave dielectric ceramic powder according to any one of claims 1 to 5.
9. A microwave component as claimed in claim 8, wherein: the microwave component is one of a resonator, a filter, a dielectric antenna and a dielectric guided wave loop.
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