CN114822992A - Preparation method of conductive silver paste for aerosol spraying process of electronic circuit - Google Patents
Preparation method of conductive silver paste for aerosol spraying process of electronic circuit Download PDFInfo
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- CN114822992A CN114822992A CN202210732519.3A CN202210732519A CN114822992A CN 114822992 A CN114822992 A CN 114822992A CN 202210732519 A CN202210732519 A CN 202210732519A CN 114822992 A CN114822992 A CN 114822992A
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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
- H01B1/20—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
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
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Abstract
The invention is suitable for the technical field of electronic circuits, and provides a preparation method of conductive silver paste for an aerosol spraying process for electronic circuits, which comprises the following steps: step one, mixing an anti-settling agent, a coupling agent, a surfactant, a diluent and a solvent in a certain proportion to prepare an organic additive; step two, taking an organic additive, and preparing an organic carrier from ethyl cellulose and terpineol according to a certain proportion to serve as a non-conductive group; and step three, adding the flake silver powder, the light-weight quasi-spherical hollow structure silver powder and a certain amount of absolute ethyl alcohol into the non-conductive group within two hours before aerosol spraying, and fully mixing to obtain the conductive silver paste. The invention researches the influence of different proportions of each component of the conductive silver paste on the performance of the conductive silver paste which can be atomized and sprayed by aerosol, and researches the influence according to different modes of an atomization process.
Description
Technical Field
The invention belongs to the technical field of electronic circuits, and particularly relates to a preparation method of conductive silver paste for an aerosol spraying process for an electronic circuit.
Background
In the development of the microelectronic industry, higher requirements are put on the process conditions of chip assembly and environmental protection, and therefore, the conductive paste is more and more widely applied. Conductive silver paste using ultrafine silver powder as a main conductive component plays an important role, for example, in patent No. CN 104858437 a, silver paste is prepared by relying on a high-dispersion machine, and a full-printed electronic technology is adopted to be applied to printed conductive circuits.
The existing printing technology comprises a screen printing technology and an aerosol printing technology, and compared with the screen printing technology, the aerosol printing technology is non-contact printing, an aerosol nozzle is not in direct contact with a substrate sheet, and a silicon wafer cannot be broken; meanwhile, the common aerosol printing also has the influence of factors such as coffee ring effect and the like to cause uneven spraying.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of conductive silver paste for an electronic circuit by using an aerosol spraying process, and aims to solve the problem of atomization of the conductive silver paste for the existing electronic circuit in the aerosol spraying process.
The invention is realized in such a way that a preparation method of conductive silver paste for aerosol spraying process of electronic circuit comprises the following steps:
step one, mixing an anti-settling agent, a coupling agent, a surfactant, a diluent and a solvent in a certain proportion to prepare an organic additive, and taking quantitative flake silver powder and light quasi-spherical hollow structure silver powder for later use;
step two, taking the organic additive in the step one, and preparing an organic carrier as a non-conductive group by using ethyl cellulose and terpineol according to a certain proportion;
and step three, adding the flake silver powder, the light-weight quasi-spherical hollow-structure silver powder and a certain amount of absolute ethyl alcohol into the non-conductive group obtained in the step two within two hours before aerosol spraying, and fully mixing to obtain the conductive silver paste for aerosol spraying.
According to a further technical scheme, in the first step, the organic additive comprises, by mass, 10% -13% of an anti-settling agent, 28% -30% of a coupling agent, 32% -35% of a surfactant, 10% -12% of a diluent and 10% -20% of a solvent.
According to a further technical scheme, in the second step, the mass percentages of all raw materials in the non-conductive group are respectively 10.5% -16% of ethyl cellulose, 0.5% -2% of organic additives and 82% -89% of terpineol.
According to a further technical scheme, the anti-settling agent is specifically polyamide wax, the coupling agent is KH-570 silane coupling agent, the surfactant is a mixture of soybean lecithin and brown trimethylammonium bromide, the mass ratio of the soybean lecithin to the brown trimethylammonium bromide in the surfactant is 9:1, the diluent is A6360, and the solvent is ECS (ECS).
In the further technical scheme, the weight ratio of the non-conductive group to the absolute ethyl alcohol in the third step is 1: 4.
According to the further technical scheme, the total mass of the silver powder with the light quasi-spherical hollow structure and the silver powder with the flake-like hollow structure in the third step and the mass percentage of the non-conductive group are respectively 78% and 22%.
According to a further technical scheme, the mass ratio of the flake silver powder to the light-weight quasi-spherical hollow-structure silver powder is 1: 4.
According to a further technical scheme, the specification of the flake silver powder is 2-3 microns, and the specification of the light quasi-spherical hollow structure silver powder is 1-2 microns.
According to the preparation method of the conductive silver paste for the aerosol spraying process of the electronic circuit, the influence of different proportions of each component of the conductive silver paste on the performance of the conductive silver paste which can be atomized and sprayed by the aerosol is researched, particularly the influence is researched according to different modes of the aerosol spraying process, such as ultrasonic aerosol atomization, pressure type aerosol atomization, centrifugal type aerosol atomization and the like, and meanwhile, the design principle of environmental protection is followed.
Drawings
Fig. 1 is a diagram illustrating a result of one-time spraying of conductive silver paste prepared by a method for preparing conductive silver paste by an aerosol spraying process for electronic circuits according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Specific implementations of the present invention are described in detail below with reference to specific embodiments.
Example one
A preparation method of conductive silver paste for aerosol spraying process of electronic circuit comprises the following steps:
step one, mixing an anti-settling agent, a coupling agent, a surfactant, a diluent and a solvent in a certain proportion to prepare an organic additive, and taking quantitative light quasi-spherical hollow structure silver powder and flake silver powder for later use; the mass percentages of all raw materials in the organic additive are respectively 10 percent of anti-settling agent, 28 percent of coupling agent, 32 percent of surface active agent, 10 percent of diluent and 20 percent of solvent; the anti-settling agent is polyamide wax, the coupling agent is KH-570 silane coupling agent, the surfactant is a mixture of soybean lecithin and brown trimethylammonium bromide, the mass ratio of the soybean lecithin to the brown trimethylammonium bromide in the surfactant is 9:1, the diluent is A6360, and the solvent is ECS; the mass ratio of the flake silver powder to the light quasi-spherical hollow structure silver powder is 1:4, the specification of the flake silver powder is 2-3 mu m, and the specification of the light quasi-spherical hollow structure silver powder is 1-2 mu m;
step two, taking the organic additive in the step one, and preparing an organic carrier as a non-conductive group by using ethyl cellulose and terpineol according to a certain proportion; the mass percentages of the raw materials in the non-conductive group are respectively 10.5% of ethyl cellulose, 0.5% of organic additive and 89% of terpineol;
step three, adding the light-weight quasi-spherical hollow-structure silver powder, the flake silver powder and a certain amount of absolute ethyl alcohol into the non-conductive group in the step two within two hours before aerosol spraying, and fully mixing to obtain conductive silver paste for aerosol spraying; the weight ratio of the non-conductive group to the absolute ethyl alcohol is 1: 4; the total mass of the light quasi-spherical hollow structure silver powder and the flake silver powder and the mass percentage of the non-conductive group are respectively 78 percent and 22 percent.
Example two
A preparation method of conductive silver paste for aerosol spraying process of electronic circuit comprises the following steps:
step one, mixing an anti-settling agent, a coupling agent, a surfactant, a diluent and a solvent in a certain proportion to prepare an organic additive, and taking quantitative light quasi-spherical hollow structure silver powder and flake silver powder for later use; the mass percentages of the raw materials in the organic additive are respectively 13% of anti-settling agent, 30% of coupling agent, 35% of surfactant, 12% of diluent and 10% of solvent; the anti-settling agent is polyamide wax, the coupling agent is KH-570 silane coupling agent, the surfactant is a mixture of soybean lecithin and brown trimethylammonium bromide, the mass ratio of the soybean lecithin to the brown trimethylammonium bromide in the surfactant is 9:1, the diluent is A6360, and the solvent is ECS; the mass ratio of the flake silver powder to the light quasi-spherical hollow structure silver powder is 1:4, the specification of the flake silver powder is 2-3 mu m, and the specification of the light quasi-spherical hollow structure silver powder is 1-2 mu m;
step two, taking the organic additive in the step one, and preparing an organic carrier as a non-conductive group by using ethyl cellulose and terpineol according to a certain proportion; the mass percentages of the raw materials in the non-conductive group are respectively 16% of ethyl cellulose, 2% of organic additive and 82% of terpineol;
step three, adding the light-weight quasi-spherical hollow-structure silver powder, the flake silver powder and a certain amount of absolute ethyl alcohol into the non-conductive group in the step two within two hours before aerosol spraying, and fully mixing to obtain conductive silver paste for aerosol spraying; the weight ratio of the non-conductive group to the absolute ethyl alcohol is 1: 4; the total mass of the light quasi-spherical hollow structure silver powder and the flake silver powder and the mass percentage of the non-conductive group are respectively 78 percent and 22 percent.
EXAMPLE III
A preparation method of conductive silver paste for aerosol spraying process of electronic circuit comprises the following steps:
step one, mixing an anti-settling agent, a coupling agent, a surfactant, a diluent and a solvent in a certain proportion to prepare an organic additive, and taking quantitative light quasi-spherical hollow structure silver powder and flake silver powder for later use; the mass percentages of the raw materials in the organic additive are respectively 12% of anti-settling agent, 29% of coupling agent, 33% of surfactant, 11% of diluent and 15% of solvent; the anti-settling agent is polyamide wax, the coupling agent is KH-570 silane coupling agent, the surfactant is a mixture of soybean lecithin and brown trimethylammonium bromide, the mass ratio of the soybean lecithin to the brown trimethylammonium bromide in the surfactant is 9:1, the diluent is A6360, and the solvent is ECS; the mass ratio of the flake silver powder to the light quasi-spherical hollow structure silver powder is 1:4, the specification of the flake silver powder is 2-3 mu m, and the specification of the light quasi-spherical hollow structure silver powder is 1-2 mu m;
step two, taking the organic additive in the step one, and preparing an organic carrier as a non-conductive group by using ethyl cellulose and terpineol according to a certain proportion; the mass percentages of the raw materials in the non-conductive group are respectively 13% of ethyl cellulose, 1.25% of organic additive and 85.75% of terpineol;
step three, adding the light-weight quasi-spherical hollow-structure silver powder, the flake silver powder and a certain amount of absolute ethyl alcohol into the non-conductive group in the step two within two hours before aerosol spraying, and fully mixing to obtain conductive silver paste for aerosol spraying; the weight ratio of the non-conductive group to the absolute ethyl alcohol is 1: 4; the total mass of the light quasi-spherical hollow structure silver powder and the flake silver powder and the mass percentage of the non-conductive group are respectively 78 percent and 22 percent.
TABLE 1 (Properties of conductive silver paste obtained in examples)
| Specific resistance (mu omega cm) | Adhesion force | Viscosity mPas | Gas atomization performance | |
| Example one | 12.1 | Level 1 | 12 | Good effect |
| Example two | 14.3 | Level 1 | 15 | Is better |
| EXAMPLE III | 15 | Level 1 | 19 | In general |
The invention provides a preparation method of conductive silver paste for an aerosol spraying process of an electronic circuit, which researches the influence of different proportions of each component of the conductive silver paste on the performance of the conductive silver paste which can be atomized and sprayed by the aerosol, especially researches according to different modes of the aerosol spraying process, such as ultrasonic aerosol, pressure aerosol, centrifugal aerosol and the like, and simultaneously follows the design principle of environmental protection, the main conductive material is formed by mixing silver powder with a light quasi-spherical hollow structure and flake silver powder, so that the silver paste can form a compact conductive layer after sintering, and the cost of the silver paste is reduced, the invention can be finally used in the field of aerosol spraying processes of electronic information products such as precise electronic circuits, PDS antenna processes and the like, and has higher practical application value, the basic principle of the innovative aerosol printing technology adopted by the invention is to print the conductive atomized silver paste into the aerosol, simultaneously, this spout seal technique does not rely on the spraying size to carry out the spraying, but adjusts spraying dispersion area, its advantage through the air current restraint at the shower nozzle outer lane: firstly, liquid drops after gas atomization are uniformly dispersed, particles are not easy to agglomerate, and the output of a spraying medium is uniform; secondly, the requirement on the precision of the spray head is low, meanwhile, the processing technology of the spray head is simple, and the selection of the spray head material is not limited; thirdly, the process performance is excellent, the aerosol printing technology is not easy to block the nozzle, the long-time work is suitable, the automation degree of the equipment is high, and the industrial application is facilitated; fourthly, the conductive silver paste has low viscosity requirement and high printing resolution; the conductive silver paste prepared by the method is specially developed for printing a conductive circuit by the innovative aerosol spraying process, has excellent gas atomization performance, can be matched with various existing gas atomization processes, has good conductive performance, and can reduce environmental pollution.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A preparation method of conductive silver paste for aerosol spraying process of electronic circuit is characterized by comprising the following steps:
step one, mixing an anti-settling agent, a coupling agent, a surfactant, a diluent and a solvent in a certain proportion to prepare an organic additive, and taking quantitative flake silver powder and light quasi-spherical hollow structure silver powder for later use;
step two, taking the organic additive in the step one, and preparing an organic carrier as a non-conductive group by using ethyl cellulose and terpineol according to a certain proportion;
and step three, adding the flake silver powder, the light-weight quasi-spherical hollow-structure silver powder and a certain amount of absolute ethyl alcohol into the non-conductive group obtained in the step two within two hours before aerosol spraying, and fully mixing to obtain the conductive silver paste for aerosol spraying.
2. The method for preparing the conductive silver paste by the aerosol spraying process for electronic circuits according to claim 1, wherein the organic additive in the first step comprises, by mass, 10% -13% of an anti-settling agent, 28% -30% of a coupling agent, 32% -35% of a surfactant, 10% -12% of a diluent and 10% -20% of a solvent.
3. The method for preparing the conductive silver paste by the aerosol spraying process for electronic circuits according to claim 2, wherein the mass percentages of the raw materials in the non-conductive group in the second step are respectively 10.5% -16% of ethyl cellulose, 0.5% -2% of organic additives and 82% -89% of terpineol.
4. The method for preparing the conductive silver paste for the aerosol spraying process of the electronic circuit according to claim 1 or 2, wherein the anti-settling agent is polyamide wax, the coupling agent is KH-570 silane coupling agent, the surfactant is a mixture of soybean lecithin and brown trimethylammonium bromide, the mass ratio of the soybean lecithin to the brown trimethylammonium bromide in the surfactant is 9:1, the diluent is A6360, and the solvent is ECS.
5. The method for preparing the conductive silver paste for the aerosol spraying process for electronic circuits according to claim 1, wherein the weight ratio of the non-conductive group to the absolute ethyl alcohol in the third step is 1: 4.
6. The method for preparing the conductive silver paste by the aerosol spraying process for electronic circuits according to claim 1, wherein the total mass of the silver powder with the light quasi-spherical hollow structure and the silver powder with the flake shape in the third step is 78% and 22% of the mass of the non-conductive group respectively.
7. The method for preparing the conductive silver paste by the aerosol spraying process for electronic circuits according to claim 6, wherein the mass ratio of the flake silver powder to the silver powder with the light quasi-spherical hollow structure is 1: 4.
8. The method for preparing conductive silver paste by aerosol spraying process for electronic circuit according to claim 7, wherein the silver flakes have a size of 2-3 μm, and the silver powder with light quasi-spherical hollow structure has a size of 1-2 μm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116072350A (en) * | 2023-04-07 | 2023-05-05 | 江西理工大学南昌校区 | Method for preparing conductive silver paste for solar cell electrode in situ |
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