CN113658756B - Preparation method of electrode silver paste for 5G ceramic pedestal filter - Google Patents
Preparation method of electrode silver paste for 5G ceramic pedestal filter Download PDFInfo
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- CN113658756B CN113658756B CN202110915196.7A CN202110915196A CN113658756B CN 113658756 B CN113658756 B CN 113658756B CN 202110915196 A CN202110915196 A CN 202110915196A CN 113658756 B CN113658756 B CN 113658756B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/20—Frequency-selective devices, e.g. filters
- H01P1/2002—Dielectric waveguide filters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
- Y02A50/2351—Atmospheric particulate matter [PM], e.g. carbon smoke microparticles, smog, aerosol particles, dust
Abstract
The invention relates to a preparation method of electrode silver paste for a 5G ceramic pedestal filter, which comprises the following steps of: 85% of silver powder; 1% -3% of Bi glass powder added with zinc oxide and bismuth oxide; 0.1% -0.5% of a sintering cosolvent; 1% -5% of ethyl cellulose; 1% -5% of one or more alcohol solvents; the ester solvent is butyl ester and rosin modified phenolic resin 0.5-5 wt%, and the sum of the weight percentages of the components is 100%. The silver paste has a high Q value of 1800-2000, has good adhesion to a filter ceramic matrix and weldability, and is suitable for 5G ceramic base filter electrodes.
Description
Technical Field
The invention relates to the technical field of electronic materials for 5G ceramic bases, in particular to a preparation method of electrode silver paste for a 5G ceramic base.
Background
With the popularization and popularization of new technologies such as 5G communication and Internet of things, the construction and demand of 5G base stations are exponentially increased, and a filter serving as one of core devices of a radio frequency unit in the 5G base stations is also becoming increasingly popular. Compared with metal cavity filters and plastic filters, the ceramic filter has the characteristics of high dielectric constant, high Q value, low loss, small volume, light weight, low cost, good temperature drift resistance and the like, and is a main product of the future 5G filter market. Electrode slurry is used as one of key raw materials of the ceramic base filter, and is also required to be matched with the ceramic base filter for development, so that the practical application of the ceramic base filter is further accelerated.
Although there are many silver paste preparation methods on the market, silver paste products with adhesive force and higher Q value are very few, which greatly limits the development and practical use of 5G ceramic base filters.
Disclosure of Invention
Aiming at the technical defects, the invention provides a preparation method of electrode silver paste for a filter, which has higher Q value and better adhesive force and is suitable for a 5G ceramic base.
The invention provides a preparation method of electrode silver paste for a 5G ceramic pedestal filter, which comprises the following components:
(1) The silver powder comprises coarse silver powder and fine silver powder, and the spherical powder of the coarse silver powder and the fine silver powder are mixed in proportion;
(2) Bi-based glass powder;
(3) Ethylcellulose and ester solvents.
The preparation method of the electrode silver paste for the 5G ceramic pedestal filter comprises the following steps: the weight ratio of the fine silver powder to the coarse silver powder was 10% to 90%, or 20% to 80%, or 33% to 67%, or 50% to 50%, or 67% to 33%, respectively.
The preparation method of the electrode silver paste for the 5G ceramic pedestal filter comprises the following steps: the grain diameter of the crude silver powder is 1.6-2.0 mu m, and the specific surface area is 0.3-0.5m 2 /g; the grain diameter of the fine silver powder is 0.2-0.6 mu m, and the specific surface area is 1.3-2.2m 2 And/g. The preparation method of the electrode silver paste for the 5G ceramic pedestal filter comprises the following steps: the Bi-based glass powder comprises Bi-B-Al-Cu-Ti with the particle size of 0.8-1.5 microns, and zinc oxide and bismuth oxide metal oxide with the particle size of 0.5-3% are added into the Bi-based glass powder.
The preparation method of the electrode silver paste for the 5G ceramic pedestal filter comprises the following steps: the ethyl cellulose is one or more of polyvinyl butyral (PVB) resin, polyvinyl chloride (PVC) resin, rosin modified phenolic resin, PCB resin fiber powder, bismaleimide (BMI) resin and polyether sulfone (PES).
Compared with the prior art, the invention has the following beneficial effects:
in the invention, the silver paste silver powder is mixed with coarse powder and fine powder according to a proportion, wherein the grain diameter of the coarse silver powder is 1.6-2.0 mu m, and the specific surface area is 0.3-0.5m 2 /g; the grain diameter of the fine silver powder is 0.2-0.6 mu m, and the specific surface area is 1.3-2.2m 2 And/g. According to researches such as tunnel conduction theory, good conduction paths can be formed only when the intervals of conductive particles are small or the conductive particles are in direct contact, so that when the intervals of silver powder are large or the lap joint is not tight enough, the conductivity of the silver paste electrode is reduced, and the resistance value is high. The coarse powder and the fine powder are matched according to a proper proportion, so that the contact probability between the coarse powder and the fine powder particles can be increased, a relatively complete conductive path is formed, and the effect of improving the conductivity of the silver paste is remarkable. In addition, compared with other powder with single particle diameter, the mixture of coarse powder and fine powder can effectively improve the powder stacking density, reduce the gaps among particles and reduce the contact resistance, thereby obtaining good conductive performance.
Further, the silver paste comprises the following components in parts by weight: 85% of silver powder; 1% -3% of glass; 0.1% -0.5% of a sintering cosolvent; 1% -5% of ethyl cellulose; 1% -5% of one or more alcohol solvents; the ester solvent is 0.5-5% of butyl ester and rosin fused rosin, and the sum of the weight percentages of the components is 100%. Wherein, the glass powder is Bi glass, and the main components are as follows: bi-B-Al-Cu-Ti with a particle size of 0.8-1.5 μm, and 0.5-3% zinc oxide and bismuth oxide metal oxide are added to the Bi-based glass powder. The thermal expansion coefficients of all components in the glass powder are comprehensively regulated through Bi-B-Al-Cu-Ti glass powder and metal oxide, so that the wettability of silver in the sintering process is improved, a more compact electrode structure is obtained, defects are reduced, loss is further reduced, and the Q value of silver paste is improved. Further, the silver powder system and the glass powder system are mixed with 0.1 percent
The silver paste has high Q value (1900) and good adhesive force, can be drawn, has good weldability, has smooth appearance without bubbles after sintering, and is suitable for a filter electrode of a 5G ceramic base when the mixture ratio of coarse powder to fine powder is 80 percent to 20 percent.
Drawings
FIG. 1 is a schematic view of the solderability and wetting angle of silver pastes prepared at different weight ratios for coarse and fine powders in accordance with the present invention;
FIG. 2 is a schematic view showing the appearance of sintered silver paste prepared from coarse powder and fine powder in different weight ratios according to the present invention;
FIG. 3 is a schematic representation of the viscosity, stringiness and thixotropic values of silver pastes prepared at different weight ratios for coarse and fine powders in accordance with the present invention;
fig. 4 is a schematic drawing showing the adhesion of the silver paste prepared by the coarse powder and the fine powder according to the present invention at different weight ratios.
Detailed Description
The following specifically describes the conductive silver paste and the preparation method thereof according to the embodiment of the invention: electrode silver paste for 5G ceramic pedestal filterComprises the following components in parts by weight: silver powder, glass frit, resin and organic solvent. Wherein the total content of silver powder is 85%, the grain diameter of the crude silver powder is 1.6-2.0 mu m, and the specific surface area is 0.3-0.5m 2 /g; the grain diameter of the fine silver powder is 0.2-0.6 mu m, and the specific surface area is 1.3-2.2m 2 /g; 1-3% of glass content, and 0.5-3% of zinc oxide and bismuth oxide metal oxide are added; 0.1% -0.5% of a sintering cosolvent; the resin and the organic solvent mainly comprise 1% -5% of ethyl cellulose; 1% -5% of one or more alcohol solvents; the ester solvent is butyl ester and rosin modified phenolic resin 0.5-5 wt%, and the sum of the weight percentages of the components is 100%.
Example 1:
1) The raw materials are as follows: and weighing and proportioning four raw materials of silver powder, glass powder, resin and organic solvent according to the total proportion of the silver powder, the glass powder, the resin and the organic solvent. Wherein the specific surface area is 0.3-0.5m 2 Per g, coarse silver powder with particle diameter of 1.6-2.0 μm and specific surface area of 1.3-2.2m 2 The specific gravity of the fine silver powder with the grain diameter of 0.2-0.6 mu m is 10 percent to 90 percent;
2) Mixing four raw materials of silver powder, glass powder, resin and organic solvent which are prepared according to specific gravity at the rotating speed of 40RPM and the temperature of less than 35 ℃ and stirring for 30min;
3) Grinding the mixed raw material obtained in the step 2 on a three-roller machine under the conditions of 200RPM (revolutions per minute) and 30 ℃ of temperature, gradually shrinking the intervals of rollers, and carrying out grinding for 12 times, wherein the fineness is 2.5 mu m;
4) After finishing grinding, passing through a 250-mesh filter screen, and performing viscosity adjustment treatment;
5) The silver paste obtained in the 4 steps is subjected to relevant performance tests to obtain the silver paste with the adhesive force of 80.8, the weldability of 100, the wetting angle of 70, the appearance of flatness, the viscosity of 0.8, the wiredrawing property, the thixotropic value of 2.11 and the Q value of 1800, and the silver paste can be used for a 5G ceramic base filter.
Example 2:
1) The raw materials are as follows: and weighing and proportioning four raw materials of silver powder, glass powder, resin and organic solvent according to the total proportion of the silver powder, the glass powder, the resin and the organic solvent.Wherein the specific surface area is 0.3-0.5m 2 Per g, coarse silver powder with particle diameter of 1.6-2.0 μm and specific surface area of 1.3-2.2m 2 80% of fine silver powder with the grain diameter of 0.2-0.6 mu m and the specific gravity of 20%;
2) Mixing four raw materials of silver powder, glass powder, resin and organic solvent which are prepared according to specific gravity at the rotating speed of 40RPM and the temperature of less than 35 ℃ and stirring for 30min;
3) Grinding the mixed raw material obtained in the step 2 on a three-roller machine under the conditions of 200RPM (revolutions per minute) and 30 ℃ of temperature, gradually shrinking the intervals of rollers, and carrying out grinding for 12 times, wherein the fineness is 2.5 mu m;
4) After finishing grinding, passing through a 250-mesh filter screen, and performing viscosity adjustment treatment;
5) The silver paste obtained in the 4 steps is subjected to relevant performance tests to obtain the silver paste with the adhesive force of 83.6, the weldability of 80, the wetting angle of 70, the appearance of flatness, the viscosity of 0.9, the wiredrawing property, the thixotropic value of 2.25 and the Q value of 2000, and can be used for a 5G ceramic base filter.
Example 3:
1) The raw materials are as follows: and weighing and proportioning four raw materials of silver powder, glass powder, resin and organic solvent according to the total proportion of the silver powder, the glass powder, the resin and the organic solvent. Wherein the specific surface area is 0.3-0.5m 2 Per g, coarse silver powder with particle diameter of 1.6-2.0 μm and specific surface area of 1.3-2.2m 2 The specific weight of the fine silver powder with the grain diameter of 0.2-0.6 mu m is 33 percent/g, 67 percent;
2) Mixing four raw materials of silver powder, glass powder, resin and organic solvent which are prepared according to specific gravity at the rotating speed of 40RPM and the temperature of less than 35 ℃ and stirring for 30min;
3) Grinding the mixed raw material obtained in the step 2 on a three-roller machine under the conditions of 200RPM (revolutions per minute) and 30 ℃ of temperature, gradually shrinking the intervals of rollers, and grinding for 12 times, wherein the fineness is less than 2.5;
4) After finishing grinding, passing through a 250-mesh filter screen, and performing viscosity adjustment treatment;
5) The silver paste obtained in the 4 steps is subjected to relevant performance tests, so that the silver paste has the adhesive force of 89.7, the weldability of 60, the wetting angle of 60, few bubbles in appearance, the viscosity of 4, no wiredrawing, the thixotropic value of 3.08 and the Q value of 1900, and can be used for a 5G ceramic base filter. The invention provides an electrode silver paste method for a 5G ceramic base filter, which is characterized in that through proper selection and proportion of silver powder, glass powder, resin and organic solvent, the prepared silver paste has higher Q value, better adhesive force, good wire drawing property, good welding property, smooth appearance and no bubbles after sintering, and is suitable for the filter electrode of the 5G ceramic base. The weight ratio of fine powder and coarse powder in silver powder is 10% to 90%, or 20% to 90%, respectively
80%, or 33%:67%, or 50%:50%, or 67%:33%.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
Claims (3)
1. The preparation method of the electrode silver paste for the 5G ceramic pedestal filter is characterized by comprising the following components:
(1) The silver powder comprises coarse silver powder and fine silver powder, and the spherical powder of the coarse silver powder and the fine silver powder are mixed in proportion;
(2) Bi-based glass powder;
(3) Ethyl cellulose and ester solvents;
the weight ratio of the fine silver powder to the coarse silver powder is 10 percent respectively: 90%, or 20%:80%, or 33%:67%;
the Bi-based glass powder comprises Bi-B-Al-Cu-Ti with the particle size of 0.8-1.5 microns, and zinc oxide and bismuth oxide metal oxide with the particle size of 0.5-3% are added into the Bi-based glass powder.
2. The method for preparing the electrode silver paste for the 5G ceramic pedestal filter according to claim 1, wherein the method comprises the following steps of: the grain diameter of the crude silver powder is 1.6-2.0 mu m, and the specific surface area is 0.3-0.5m 2 /g; the grain diameter of fine silver powder is 0.2-0.6 mu m, and the ratio tableThe area is 1.3-2.2m 2 /g。
3. The method for preparing the electrode silver paste for the 5G ceramic pedestal filter according to claim 1, wherein the method comprises the following steps of: the ethyl cellulose is one or more of polyvinyl butyral PVB resin, polyvinyl chloride PVC resin, rosin modified phenolic resin, PCB resin fiber powder, bismaleimide BMI resin and polyether sulfone PES.
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| JP4212035B2 (en) * | 2003-06-05 | 2009-01-21 | 株式会社ノリタケカンパニーリミテド | Conductive paste mainly composed of silver powder and method for producing the same |
| CN103545012B (en) * | 2013-11-11 | 2016-04-27 | 广东风华高新科技股份有限公司 | Filter conductive silver paste and preparation method thereof |
| CN105825911B (en) * | 2016-05-13 | 2017-05-31 | 浙江光达电子科技有限公司 | A kind of laminated inductive silver paste of inner electrode and preparation method thereof |
| CN106128555B (en) * | 2016-09-23 | 2017-12-01 | 苏州柏特瑞新材料有限公司 | A kind of highly conductive crystal silicon solar batteries front electrode silver slurry and preparation method thereof |
| CN109859878A (en) * | 2019-02-22 | 2019-06-07 | 肇庆市辰业电子有限公司 | A kind of 5G base of ceramic filter high q-factor electrode silver plasm and preparation method thereof |
| JP6930578B2 (en) * | 2019-12-20 | 2021-09-01 | 三菱マテリアル株式会社 | Manufacturing method of silver paste and bonded body |
| CN112117026B (en) * | 2020-10-29 | 2022-05-17 | 无锡晶睿光电新材料有限公司 | Ceramic filter silver paste for dip coating and preparation method thereof |
| CN112951479B (en) * | 2021-02-07 | 2022-08-05 | 北京中科纳通电子技术有限公司 | Conductive silver paste for filter and preparation method thereof |
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Denomination of invention: A Preparation Method of Electrode Silver Paste for 5G Ceramic Base Filter Effective date of registration: 20230914 Granted publication date: 20230620 Pledgee: Industrial Bank Co.,Ltd. Shanghai Minhang sub branch Pledgor: SHANGHAI YINJIANG TECHNOLOGY CO.,LTD. Registration number: Y2023310000548 |