CN113823438B - Silver paste recycling preparation method for spraying dielectric filter - Google Patents
Silver paste recycling preparation method for spraying dielectric filter Download PDFInfo
- Publication number
- CN113823438B CN113823438B CN202111264949.9A CN202111264949A CN113823438B CN 113823438 B CN113823438 B CN 113823438B CN 202111264949 A CN202111264949 A CN 202111264949A CN 113823438 B CN113823438 B CN 113823438B
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- China
- Prior art keywords
- silver paste
- target product
- dielectric filter
- spraying
- filtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 40
- 239000004332 silver Substances 0.000 title claims abstract description 40
- 238000005507 spraying Methods 0.000 title claims abstract description 19
- 238000004064 recycling Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 238000011084 recovery Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 239000006185 dispersion Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 14
- 239000003960 organic solvent Substances 0.000 claims description 13
- 239000012752 auxiliary agent Substances 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- 239000011297 pine tar Substances 0.000 claims description 10
- 229940068124 pine tar Drugs 0.000 claims description 10
- 239000004925 Acrylic resin Substances 0.000 claims description 9
- 229920000178 Acrylic resin Polymers 0.000 claims description 9
- 239000002318 adhesion promoter Substances 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002518 antifoaming agent Substances 0.000 claims description 5
- 239000000701 coagulant Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 3
- -1 alcohol ester Chemical class 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 3
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 3
- 229940116411 terpineol Drugs 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 description 8
- 230000001276 controlling effect Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a silver paste recycling preparation method for spraying a dielectric filter, and relates to the technical field of electronic paste. The preparation method at least comprises the following steps: step 1: adding absolute ethyl alcohol into the recovered silver paste according to the mass ratio of 1:1.5 for dispersion grinding for 30min; step 2: pumping the slurry dispersed in the step 1 into a filtering mechanism for pressurized filtering separation, and filtering the chips and fine chips remained in the recovery to obtain recovered slurry; step 3: and (3) carrying out centrifugal separation on the slurry filtered in the step (2), and obtaining a first target product after the treatment is completed. According to the invention, through the design of the method, the waste of silver paste caused by the traditional spraying mode is greatly reduced, so that the production cost of the dielectric filter is directly reduced; on the other hand, the recovery preparation method has the advantages of high recovery rate, simple process, short recovery period, low cost and sales in equipment markets.
Description
Technical Field
The invention relates to the technical field of electronic paste, in particular to a silver paste recycling preparation method for spraying a dielectric filter.
Background
With the great development of the 5G infrastructure industry, the 5G base station key component, namely the 5G ceramic dielectric filter, is also coming into great burst. The surface of the ceramic filter is metallized by silver paste, which plays a role in the whole process of the ceramic filter, and determines whether the ceramic filter has the possibility of mass production.
At present, most of the metalizing processes adopted by the domestic ceramic filters are spray-coated silver paste, but the utilization rate of the spray-coated silver paste is extremely low.
Disclosure of Invention
The invention aims to provide a silver paste recycling preparation method for spraying a dielectric filter, which aims to solve the existing problems: the silver paste utilization rate of the spraying process is extremely low.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method for recycling silver paste for spraying a dielectric filter at least comprises the following steps:
step 1: adding absolute ethyl alcohol into the recovered silver paste according to the mass ratio of 1:1.5 for dispersion grinding for 30min;
step 2: pumping the slurry dispersed in the step 1 into a filtering mechanism for pressurized filtering separation, and filtering the chips and fine chips remained in the recovery to obtain recovered slurry;
step 3: centrifuging the slurry filtered in the step 2, and obtaining a first target product after the treatment is completed;
step 4: weighing a first target product, resin, an organic solvent, an auxiliary agent and pine tar according to parts by mass, mixing, and dispersing for 45min at the rotating speed of 900rmp on a dispersing machine to obtain a second target product;
step 5: weighing the second target product obtained in the step 4 according to the parts by mass, adding an aging adhesion promoter, glass powder and a coagulant, and dispersing for 70 minutes by adopting a dispersing machine at the rotating speed of 100rpm to obtain a third target product;
step 6: and (3) grinding the third target product obtained in the step (5) on a three-roller grinder for 10 times, controlling the particle size to be smaller than 10 mu m, and filtering to obtain silver paste.
Preferably, in the step 4 and the step 5, the components in mass percent are as follows: 75-82% of a first target product, 8-14% of resin, 7-15% of an organic solvent, 1-3% of an auxiliary agent, 0.1-0.5% of pine tar, 0.5-1% of an aging adhesion promoter and 0.1-3% of glass powder.
Preferably, the resin is a hydroxy acrylic resin.
The content of inorganic powder such as silver powder, glass powder and the like in the silver paste of the filter reaches more than 75%, the viscosity of the paste is required to be 0.5-1.0Pa.s in the spraying process, and the resin content in the paste formula is required to be regulated in order to ensure the spraying smoothness, so that the hydroxyl acrylic resin is used as a bonding phase after the paste is dried, more hydrogen bonds can be formed between hydroxyl groups in the hydroxyl acrylic resin and the ceramic surface, and the adhesive force between a dry film and the ceramic surface is enhanced;
in addition, the hydroxy acrylic resin has the characteristics of high solid and low viscosity, and can reduce the viscosity of silver paste to achieve the viscosity required by spraying;
when the dosage of the silver paste reaches 8-14%, more resin molecules play a role in the slurry and inorganic powder, so that the good dispersing and supporting effects are achieved, the storage stability of the silver paste is enhanced, and meanwhile, after the silver paste sprayed on the ceramic filter is dried, the strength of the dried film is improved due to the high content of hydroxy acrylic resin in the silver film.
Preferably, the organic solvent includes: one or more of terpineol, alcohol ester twelve, propylene glycol methyl ether acetate, butyl carbitol and butyl carbitol acetate.
The pine tar, the organic solvent and the auxiliary agent have good compatibility, and a stable emulsifying system can be formed.
The glass powder is prepared by uniformly mixing raw material components, melting into glass liquid, and then sequentially carrying out water quenching, drying, ball milling and drying, wherein the raw material components of the glass powder comprise 15-35% of Bi2O3, 2 3-10% of SiO, 20-35% of ZnO and 310-25% of B2O by weight percent; 5-15% of CaO; the particle size of the glass powder is 0.5-3um.
Preferably, the auxiliary agent comprises a leveling agent, a surfactant and an antifoaming agent, wherein the antifoaming agent is one or more of sodium dodecyl sulfonate, 2-ethyl-4-methylimidazole and 4, 4-diaminodiphenylmethane.
Preferably, the step 6 at least includes the following steps:
s1: weighing a first target product, hydroxy acrylic resin, an organic solvent, an auxiliary agent and pine tar according to mass parts, mixing, and dispersing for 0.5-1h at the rotating speed of 600-1200rmp on a dispersing machine;
s2: adding an ageing adhesion promoter, glass powder and a coagulant, and dispersing for 50-90min by adopting a dispersing machine at the rotating speed of 50-120 rpm;
s3: grinding for 10 times on a three-roller grinder, controlling the grain diameter to be smaller than 10um, and filtering to obtain silver paste. .
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through the design of the method, the waste of silver paste caused by the traditional spraying mode is greatly reduced, so that the production cost of the dielectric filter is directly reduced; on the other hand, the recovery preparation method has the advantages of high recovery rate, simple process, short recovery period and low cost, and the equipment market is sold.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the overall process of the present invention;
fig. 2 is a schematic view of a pressurized filtration apparatus of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Embodiment one:
referring to fig. 1, a method for recycling silver paste for spraying a dielectric filter, the method at least comprises the following steps:
step 1: adding absolute ethyl alcohol into the recovered silver paste according to the mass ratio of 1:1.5 for dispersion grinding for 30min;
step 2: pumping the slurry dispersed in the step 1 into a filtering mechanism for pressurized filtering separation, and filtering the chips and fine chips remained in the recovery to obtain recovered slurry;
step 3: centrifuging the slurry filtered in the step 2, and obtaining a first target product after the treatment is completed;
step 4: weighing a first target product, resin, an organic solvent, an auxiliary agent and pine tar according to parts by mass, mixing, and dispersing for 45min at the rotating speed of 900rmp on a dispersing machine to obtain a second target product;
step 5: weighing the second target product obtained in the step 4 according to the parts by mass, adding an aging adhesion promoter, glass powder and a coagulant, and dispersing for 70 minutes by adopting a dispersing machine at the rotating speed of 100rpm to obtain a third target product;
step 6: and (3) grinding the third target product obtained in the step (5) on a three-roller grinder for 10 times, controlling the particle size to be smaller than 10 mu m, and filtering to obtain silver paste.
The method comprises the following components in percentage by mass in the step 4 and the step 5: 75-82% of a first target product, 8-14% of resin, 7-15% of an organic solvent, 1-3% of an auxiliary agent, 0.1-0.5% of pine tar, 0.5-1% of an aging adhesion promoter and 0.1-3% of glass powder;
the resin is hydroxy acrylic resin;
the organic solvents include: one or more of terpineol, alcohol ester twelve, propylene glycol methyl ether acetate, butyl carbitol and butyl carbitol acetate;
the auxiliary agent comprises a leveling agent, a surfactant and a defoaming agent;
step 6 comprises at least the following steps:
s1: weighing a first target product, hydroxy acrylic resin, an organic solvent, an auxiliary agent and pine tar according to mass parts, mixing, and dispersing for 0.5-1h at the rotating speed of 600-1200rmp on a dispersing machine;
s2: adding an ageing adhesion promoter, glass powder and a coagulant, and dispersing for 50-90min by adopting a dispersing machine at the rotating speed of 50-120 rpm;
s3: grinding for 10 times on a three-roller grinder, controlling the grain diameter to be smaller than 10um, and filtering to obtain silver paste.
Embodiment two:
by the first embodiment, a second embodiment is a method for recycling silver paste for spraying a dielectric filter, which specifically comprises the following steps:
step 1: 1Kg of recovered silver paste is added with 1.5Kg of absolute ethyl alcohol according to the mass ratio of 1:1.5, the mixture of the recovered silver paste and the absolute ethyl alcohol is placed in a dispersing machine, and the mixture is dispersed for 30 minutes by adopting the rotating speed of 100rpm of the dispersing machine, so as to obtain mixed silver paste;
step 2: pumping the slurry dispersed in the step 1 into a filtering mechanism for pressurized filtering separation, and filtering the chips and fine chips remained in the recovery to obtain recovered slurry;
step 3: centrifuging the recovered slurry obtained in the step 2, and obtaining 780g of a first target product after the treatment is completed;
step 4: 780g of a first target product, 100g of resin, 80g of an organic solvent, 1g of pine tar, 4g of a leveling agent, 4g of a surfactant and 3g of a defoaming agent are weighed according to parts by mass, and the mixture is mixed and then dispersed for 45min at the rotating speed of 900rmp on a dispersing machine to obtain a second target product;
step 5: weighing and adding 8g of ageing adhesion promoter and 20g of glass powder according to the mass parts, and dispersing for 70min by adopting a dispersing machine at the rotating speed of 100rpm to obtain a third target product;
step 6: and (3) grinding the third target product obtained in the step (5) on a three-roller grinder for 10 times, controlling the particle size to be smaller than 10 mu m, and filtering to obtain silver paste.
The silver paste prepared by recycling and reusing the method is verified by experiments for many times, and the silver paste has excellent comprehensive performance and can meet the requirement of daily metallization spraying operation of a 5G dielectric filter.
The silver paste prepared by recycling through the method has the following specific parameter indexes:
while the present invention has been described in detail with reference to the drawings, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Embodiment III:
referring to fig. 2, a pressurized filter apparatus is shown for both embodiments;
the supercharged filter equipment comprises a booster pump, a primary filter screen, a secondary filter screen and a slurry collecting bin.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (4)
1. A preparation method for recycling silver paste for spraying a dielectric filter is characterized by comprising the following steps: the preparation method at least comprises the following steps:
step 1: adding absolute ethyl alcohol into the recovered silver paste according to the mass ratio of 1:1.5 for dispersion grinding for 30min;
step 2: pumping the slurry dispersed in the step 1 into a filtering mechanism for pressurized filtering separation, and filtering the chips and fine chips remained in the recovery to obtain recovered slurry;
step 3: centrifuging the slurry filtered in the step 2, and obtaining a first target product after the treatment is completed;
step 4: weighing a first target product, resin, an organic solvent, an auxiliary agent and pine tar according to parts by mass, mixing, and dispersing for 45min at the rotating speed of 900rmp on a dispersing machine to obtain a second target product;
step 5: weighing the second target product obtained in the step 4 according to the parts by mass, adding an aging adhesion promoter, glass powder and a coagulant, and dispersing for 70 minutes by adopting a dispersing machine at the rotating speed of 100rpm to obtain a third target product;
step 6: grinding the third target product obtained in the step 5 on a three-roller grinder for 10 times, controlling the grain diameter to be smaller than 10 mu m, and filtering to obtain silver paste;
the method comprises the following components in percentage by mass in the step 4 and the step 5: 75-82% of a first target product, 8-14% of resin, 7-15% of an organic solvent, 1-3% of an auxiliary agent, 0.1-0.5% of pine tar, 0.5-1% of an aging adhesion promoter and 0.1-3% of glass powder.
2. The method for recycling and preparing silver paste for spraying a dielectric filter according to claim 1, which is characterized by comprising the following steps: the resin is hydroxy acrylic resin.
3. The method for recycling and preparing silver paste for spraying a dielectric filter according to claim 1, which is characterized by comprising the following steps: the organic solvent includes: terpineol, alcohol ester twelve, propylene glycol methyl ether acetate, butyl carbitol acetate.
4. The method for recycling and preparing silver paste for spraying a dielectric filter according to claim 1, which is characterized by comprising the following steps: the auxiliary agent comprises a leveling agent, a surfactant and a defoaming agent.
Priority Applications (1)
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CN202111264949.9A CN113823438B (en) | 2021-10-28 | 2021-10-28 | Silver paste recycling preparation method for spraying dielectric filter |
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CN202111264949.9A CN113823438B (en) | 2021-10-28 | 2021-10-28 | Silver paste recycling preparation method for spraying dielectric filter |
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CN113823438B true CN113823438B (en) | 2024-04-12 |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2019053856A (en) * | 2017-09-13 | 2019-04-04 | 株式会社ノリタケカンパニーリミテド | Silver paste |
WO2019180913A1 (en) * | 2018-03-23 | 2019-09-26 | 三菱マテリアル株式会社 | Method for manufacturing electronic-component-mounted module |
CN110769678A (en) * | 2019-11-11 | 2020-02-07 | 北京中科纳通电子技术有限公司 | Electromagnetic shielding silver paste applied to 5G personal communication equipment and preparation method thereof |
CN110993148A (en) * | 2019-12-10 | 2020-04-10 | 北京中科纳通电子技术有限公司 | Flexible slurry applied to 5G mobile terminal and preparation method thereof |
-
2021
- 2021-10-28 CN CN202111264949.9A patent/CN113823438B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2019053856A (en) * | 2017-09-13 | 2019-04-04 | 株式会社ノリタケカンパニーリミテド | Silver paste |
WO2019180913A1 (en) * | 2018-03-23 | 2019-09-26 | 三菱マテリアル株式会社 | Method for manufacturing electronic-component-mounted module |
CN110769678A (en) * | 2019-11-11 | 2020-02-07 | 北京中科纳通电子技术有限公司 | Electromagnetic shielding silver paste applied to 5G personal communication equipment and preparation method thereof |
CN110993148A (en) * | 2019-12-10 | 2020-04-10 | 北京中科纳通电子技术有限公司 | Flexible slurry applied to 5G mobile terminal and preparation method thereof |
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