CN113314249A - Silver paste for 5G ceramic dielectric filter and preparation method thereof - Google Patents
Silver paste for 5G ceramic dielectric filter and preparation method thereof Download PDFInfo
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- CN113314249A CN113314249A CN202110579730.1A CN202110579730A CN113314249A CN 113314249 A CN113314249 A CN 113314249A CN 202110579730 A CN202110579730 A CN 202110579730A CN 113314249 A CN113314249 A CN 113314249A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 25
- 239000004332 silver Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 31
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 9
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 9
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 8
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 3
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 229940116411 terpineol Drugs 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 5
- 238000009472 formulation Methods 0.000 description 4
- 239000012634 fragment Substances 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004110 Zinc silicate Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 2
- 235000019352 zinc silicate Nutrition 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
-
- 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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Organic Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
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- Glass Compositions (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a silver paste for a 5G ceramic dielectric filter and a preparation method thereof, and relates to the field of electronic paste for the 5G ceramic dielectric filter. The silver paste comprises the following components in parts by weight: 70% -85% of silver oxide powder; 1% -5% of low-melting-point glass powder; the organic solvent comprises 1-10% of ethyl cellulose; 1% -5% of an alcohol solvent; organic binder PVA 1% -5%; CE-640.5% -5%; the sum of the weight percentages of the components is 100 percent. The silver paste of the invention has the same expansion coefficient with the ceramic dielectric filter substrate, high binding force, good weldability and uniform distribution.
Description
Technical Field
The invention belongs to the technical field of electronic paste for electronic ceramics, and particularly relates to silver paste for a 5G ceramic dielectric filter and a preparation method thereof.
Background
With the popularization of the 5G communication, the base station, the Internet of things, the intelligent factory and the unmanned technology in our country, the market demand of the 5G ceramic dielectric filter is more and more vigorous, the number of the ceramic dielectric filters is developed from 2 x 2 and 4 x 4 in the 4G era to 16 x 16 and 64 x 64 in the 5G era, and the market demand of the electronic paste is driven. The important characteristic of the dielectric filter is easy miniaturization, and practice proves that the volume of the dielectric filter made of the ceramic material with high dielectric constant can reach only a fraction of that of the cavity resonator type filter, and more importantly, the variation of the resonant frequency of the dielectric filter along with temperature can be controlled in a small range. The present invention relates to a ceramic material, and more particularly to a ceramic material having a high dielectric constant. The electronic paste is one of the key raw materials of the ceramic dielectric filter, and an electronic paste manufacturer and a ceramic manufacturer are urgently needed to develop a material and a production process for matching the ceramic filter and the electronic paste together, so that the problems of uniformity, binding force and the like of the silver-coated ceramic dielectric filter are solved, and the silver layer is prevented from peeling, layering and foaming.
Disclosure of Invention
(1) Technical problem to be solved
The expansion coefficient of the electronic paste is not matched with that of the ceramic dielectric filter, and the bonding force of the electronic paste and the ceramic dielectric filter is small, so that the silver layer is peeled off, layered and foamed.
(2) Technical scheme
In order to solve the technical problems, the invention provides a silver paste for a 5G ceramic dielectric filter, which comprises the following components in percentage by weight: 70-85% of silver oxide powder, 1-5% of low-melting-point glass powder, 1-10% of ethyl cellulose, 1-5% of alcohol solvent, 1-5% of organic binder PVA and CE-640.5-5%, wherein the sum of the weight percentages of the components is 100%.
Further, the particle size of the silver powder is 0.5-1.5 μm, the main components of the low-melting-point glass powder are Bi-B-Si-Zn-Mn, the expansion coefficient of the glass can be changed by adjusting the component proportion, the particle size is 0.5-1.5 μm, the ethyl cellulose is 7%, the alcohol solvent is 1.5%, the organic binder is 1.0%, the CE is 641.5%, and the alcohol solvent is at least one of terpineol and n-octanol.
In the electronic paste, the particle size of the silver oxide powder is 0.5-1.5 mu m, the silver oxide powder is uniformly distributed after sintering and has consistent thickness, the low-melting-point glass powder mainly comprises Bi-B-Si-Zn-Mn, the expansion coefficient of the glass can be changed by adjusting the component proportion, the particle size is 0.5-1.5 mu m, and the bonding force between the electronic paste and the substrate of the 5G ceramic dielectric filter can be enhanced. The organic solvent ethyl cellulose is used as a carrier, so that the cohesive force of the electronic paste at low temperature can be improved, the organic solvent alcohol is mainly n-octanol, so that bubbles in the electronic paste can be eliminated, the organic solvent PVA can adjust the surface film forming property and the fluidity of the electronic paste, so that excellent printing performance is provided for the paste, and the solid content of the electronic paste can be adjusted by CE-64.
The preparation method of the silver paste for the 5G ceramic dielectric filter is characterized by comprising the steps of preparing silver oxide powder, low-melting-point glass powder, ethyl cellulose, an alcohol solvent, an organic binder and CE-64 according to a weight ratio, then carrying out ball milling dispersion by using a ball mill, filtering, removing impurities and packaging.
(3) Advantageous effects
The invention has the beneficial effects that: compared with the prior art, the electronic paste disclosed by the invention is narrow in particle size distribution and good in uniformity. The self-developed Bi-B-Si-Zn-Mn low-melting-point glass powder can adjust the expansion coefficient of the electronic paste to be matched with the ceramic, improve the binding force of the two materials and cannot reduce the performance of the ceramic dielectric filter; the electronic paste has fine granularity, leads to compact silver layer and has good weldability.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is an XRD pattern of the precipitated primary crystalline phases of BBSZM low-melting glass frit.
Detailed Description
The technical solutions in the embodiments of the present invention are further clearly and completely described below with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example one
In the embodiment, through the research and development of Bi-B-Si-Zn-Mn low-melting-point glass powder, the expansion coefficient of the electronic paste is adjusted to be matched with the ceramic dielectric filter, the binding force of the electronic paste and the ceramic dielectric filter is improved, and the silver layer is prevented from being peeled off, layered and foamed.
In this example, a composition of 20.0 mol% Bi was used2O3、35.0mol％B2O3、35.0mol％SiO2、40.0mol％ZnO、5.0mol％MnO2The BBSZM glass is used as low-melting-point high-expansion glass, has a low glass transition temperature (700 ℃) and an expansion coefficient of 2.0-3.0 multiplied by 10～6/℃。
In this example, BBSZM glass frit can be prepared by a conventional glass fusion process. The specific process for preparing the BBSMM glass powder can comprise the following steps: the weight (wt%) of various raw materials required by the BBSZM glass is calculated according to the proportion (mol%), namely the raw materials are mixed according to the weight ratio of 20.0: 35.0: 40.0: a molar ratio of 5.0 to a source of Bi (e.g., Bi)2O3) B source (e.g. H)3BO3) Si source (e.g. SiO)2) Zn source (e.g., ZnO), Mn source (e.g., MnO)2、MnCO3) Mixing to obtain a raw material mixture. And melting the raw material mixture, and quenching to obtain glass fragments. And then grinding, drying and sieving the glass fragments to obtain the BBSZM glass powder. The purity of the used raw material powder is more than 99.0%, iron is removed in advance, and the BBSZM glass powder is prepared by adopting the raw material with the purity of more than 99.0%, so that the influence of impurities on dielectric properties is reduced. The melting system can be as follows: 900-1100 ℃; 1.0 to 3.0 hours. Before melting, a proper amount of water can be added for stirring to prevent the raw materials from generating flying dust. During quenching, the melted glass solution can be quickly poured into deionized water for quenching.
Grinding the glass fragments by adopting a wet ball milling mode, and grinding the obtained glass fragments into powderProportioning materials: ball: water 1: 4: 3, putting the mixture into an alumina ceramic pot, and carrying out planetary ball milling for 1.0-2.0 h to obtain the average particle diameter D50About 1.0 +/-0.5 um of glass powder. And finally, placing the ground glass powder slurry in a constant-temperature drying oven to be dried for 2.0-4.0 h at 150 ℃, and sieving the glass powder slurry with a 100-mesh sieve after drying to obtain the glass powder for later use.
Weighing according to the proportion of the formula: 70-85% of silver oxide powder; 1 to 5 percent of BBSZM low-melting-point glass powder; the organic solvent comprises 1 to 10 percent of ethyl cellulose; 1-5% of alcohol solvent; organic binder PVA 1% -5%; CE to 64 and 1 to 5 percent of each component, the sum of the weight percentages is 100 percent.
The formulation design of the BBSMM low melting glass frit in this example is shown in table 1:
TABLE 1.1 formulation design for BBSZM Low melting glass powder
The formulation of the electronic paste in this example is shown in table 1.2:
TABLE 1.2 electronic paste formulation
The results of the performance test of this example after the filter is silvered are shown in table 1.3:
TABLE 1.3 Performance test results after silver coating of filters
As can be seen from table 1.1: with the increase of the content of the zinc oxide, the expansion coefficient of the low-melting-point glass is improved from 12.0 to 13.0, and the expansion coefficient of the zinc silicate precipitated from the low-melting-point glass can be adjusted, but the maximum expansion coefficient of the zinc silicate can not exceed 13.0, so that the low-expansion-coefficient electronic paste can be selected according to the expansion coefficient of the 5G ceramic dielectric filter, the expansion coefficients of the electronic paste and the ceramic dielectric filter are matched, and the silver layer is prevented from falling off and cracking due to the mismatching of the expansion coefficients in the silver firing process.
As can be seen from table 1.3: the silver paste of the formula meets the electrical performance requirements of the ceramic dielectric filter, such as center frequency and insertion loss, and meanwhile, the binding force is in a descending trend along with the increase of the proportion of the silver oxide powder, which shows that the low-melting-point glass powder can improve the binding force of silver and ceramic, and is mainly caused by the approach of systems of the glass powder and the ceramic; and meanwhile, the ratio of the silver oxide can improve the thickness of the silver layer.
The above examples are merely representative of preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. The silver paste for the 5G ceramic dielectric filter is characterized by comprising the following components in percentage by weight: 70-85% of silver oxide powder, 1-5% of low-melting-point glass powder, 1-10% of ethyl cellulose, 1-5% of alcohol solvent, 1-5% of organic binder PVA and CE-640.5-5%, wherein the sum of the weight percentages of the components is 100%.
2. The silver paste for the 5G ceramic dielectric filter as recited in claim 1, wherein the silver powder has a particle size of 0.5-1.5 μm.
3. The silver paste for the 5G ceramic dielectric filter as claimed in claim 1, wherein the low-melting-point glass powder mainly comprises Bi-B-Si-Zn-Mn and has a particle size of 0.5-1.5 μm.
4. The silver paste for the 5G ceramic dielectric filter, according to claim 1, is characterized in that the ethyl cellulose accounts for 7%, the alcohol solvent accounts for 1.5%, the organic binder accounts for 1.0%, and the CE accounts for 641.5%.
5. The silver paste for the 5G ceramic dielectric filter, according to claim 1, wherein the alcohol solvent is at least one of terpineol and n-octanol.
6. The preparation method of the silver paste for the 5G ceramic dielectric filter is characterized by comprising the steps of preparing silver oxide powder, low-melting-point glass powder, ethyl cellulose, an alcohol solvent, an organic binder and CE-64 according to a weight ratio, then carrying out ball milling dispersion by using a ball mill, filtering, removing impurities and packaging.
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| CN202110579730.1A CN113314249A (en) | 2021-05-26 | 2021-05-26 | Silver paste for 5G ceramic dielectric filter and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116994795A (en) * | 2023-08-22 | 2023-11-03 | 昆明理工大学 | Silver paste for medium-temperature sintered ceramic filter and preparation method thereof |
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Application publication date: 20210827 |