CN113823438B - Silver paste recycling preparation method for spraying dielectric filter - Google Patents

Silver paste recycling preparation method for spraying dielectric filter Download PDF

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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
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CN202111264949.9A
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CN113823438A (en
Inventor
唐小能
蒋涛
王飞
谈正
杜乐德
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Pivotone Communication Technologies Inc
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Pivotone Communication Technologies Inc
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/22Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01PWAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
    • H01P1/00Auxiliary devices
    • H01P1/20Frequency-selective devices, e.g. filters
    • H01P1/2002Dielectric waveguide filters

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  • 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

Silver paste recycling preparation method for spraying dielectric filter
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.
CN202111264949.9A 2021-10-28 2021-10-28 Silver paste recycling preparation method for spraying dielectric filter Active CN113823438B (en)

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CN113823438B true CN113823438B (en) 2024-04-12

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Citations (4)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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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