CN112037963A - Conductive silver paste and preparation method thereof - Google Patents
Conductive silver paste and preparation method thereof Download PDFInfo
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- CN112037963A CN112037963A CN202010907135.1A CN202010907135A CN112037963A CN 112037963 A CN112037963 A CN 112037963A CN 202010907135 A CN202010907135 A CN 202010907135A CN 112037963 A CN112037963 A CN 112037963A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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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Abstract
The invention discloses a conductive silver paste and a preparation method thereof, relating to the technical field of conductive silver paste, and the key points of the technical scheme are that the conductive silver paste comprises the following components in parts by weight: 9-11 parts of resin; 4-6 parts of an auxiliary agent; 78-83 parts of silver powder; 9-11 parts of a solvent. According to the invention, the conductive silver paste is prepared by adopting the components with proper weight parts, the resin consisting of the epoxy resin, the bismaleimide resin and the polyimide resin is added, and the fatty acid amide dispersant is used as the dispersant, so that the obtained conductive silver paste has the effects of high stability, low curing temperature and remarkably reduced synthesis process difficulty.
Description
Technical Field
The invention relates to the technical field of conductive silver paste, in particular to conductive silver paste and a preparation method thereof.
Background
The silver conductive paste is divided into two types, namely polymer silver conductive paste (dried or solidified into a film and taking an organic polymer as a bonding phase) and sintered silver conductive paste (sintered into a film, the sintering temperature is higher than 500 ℃, and glass powder or oxide is taken as a bonding phase).
In the prior art, the electric conduction and heat conduction bonding in normal temperature curing welding occasions, such as quartz crystal, infrared pyroelectric detector, piezoelectric ceramics, potentiometer, flash lamp tube, shielding, circuit repair and the like, can also be used for electric conduction bonding in the radio instrument industry, can also replace tin paste to realize electric conduction bonding, and has the tendency of gradually replacing the traditional tin soldering welding, so the application range is wider and wider, and the yield is gradually enlarged.
However, the content of the components in the formula of the existing conductive silver paste is not effectively combined with the content of the corresponding components, so that the problems of difficult storage caused by poor stability, high use difficulty caused by high curing temperature and high production and manufacturing costs caused by complex synthesis process are solved.
Disclosure of Invention
In view of the defects in the prior art, the first object of the present invention is to provide a conductive silver paste which has the effects of high stability and convenience for production and manufacture.
In order to achieve the purpose, the invention provides the following technical scheme:
the conductive silver paste comprises the following components in parts by weight:
9-11 parts of resin;
4-6 parts of an auxiliary agent;
78-83 parts of silver powder;
9-11 parts of a solvent.
By adopting the technical scheme, the formula for preparing the conductive silver paste is formed by adopting the components in proper parts by weight, so that the obtained conductive silver paste has the effects of high stability, low curing temperature and remarkably reduced difficulty of the synthesis process.
The invention is further configured to: the resin is epoxy resin, bismaleimide resin and polyimide resin; and the epoxy resin, the bismaleimide resin and the polyimide resin are mixed according to the weight ratio of 2: 1-2: 0.5-1.
Through adopting above-mentioned technical scheme, bismaleimide resin has excellent heat resistance, electrical insulation, wave permeability, resistant radiation, fire resistance, good mechanical properties and dimensional stability, in the time of coordinating each other with epoxy resin and polyimide resin, through its active end group and epoxy resin and polyimide resin inter combination to increase the overall structure density of resin on epoxy resin solidification forms network structure, in order to reach the purpose that shows the stability that promotes this electrically conductive silver thick liquid.
The invention is further configured to: the auxiliary agent comprises one or two of a dispersing agent, a flatting agent and a coupling agent.
By adopting the technical scheme, the production and manufacturing difficulty of the conductive silver paste is remarkably reduced.
The invention is further configured to: the dispersant is a fatty acid amide dispersant.
By adopting the technical scheme, the fatty acid amide dispersing agent releases amide groups in the stirring and mixing process so as to play a role in increasing friction; meanwhile, a single-layer film for adsorbing polar groups is formed on the surface of the fatty acid amide after stirring and mixing, so that the stirring and mixing uniformity of the resin and the solvent is improved, and simultaneously, the fatty acid amide dispersing agent which is uniformly dispersed is combined with the solvent at the corresponding position, so that the mixing uniformity of the resin and the solvent is further improved, and the effect of uniformly distributing the silver powder is realized after the silver powder is added.
The invention is further configured to: the solvent is an organic solvent, and the diameter of the silver powder is 0.2-0.4 μm.
Through adopting above-mentioned technical scheme, showing the electrically conductive effect that promotes this electrically conductive silver thick liquid to play the effect that effectively promotes this electrically conductive silver thick liquid stability.
The second purpose of the invention is to provide a preparation method of conductive silver paste, which comprises the following steps:
step 1, adding 9-11 parts of resin, 4-6 parts of auxiliary agent and 9-11 parts of solvent in parts by weight into a mixer, and mixing to obtain a mixed colloid;
step 2, controlling the temperature of the mixer to 140 ℃ at 120-;
step 3, adding 78-83 parts of silver powder by weight into a mixer, and fully stirring to obtain conductive adhesive;
and 4, sequentially grinding, dispersing, filtering and then defoaming in vacuum to obtain the conductive silver paste.
By adopting the technical scheme, the conductive silver paste with high stability and convenient production and manufacture effects is obtained.
The invention is further configured to: the silver powder is modified silver powder, and the preparation method of the modified silver powder comprises the following steps of 1) adding the silver powder into a roller ball mill, and adding hydrochloric acid which is 5:1 in parts by weight and has a concentration of 37.5 for primary grinding; 2) adding the primarily ground silver powder into a disc type dryer for drying; 3) adding the dried silver powder into a flat jet mill for further crushing; 4) and screening the silver powder with corresponding particle size by using an airflow classifier to obtain the modified silver powder.
Through adopting above-mentioned technical scheme, obtain the silver powder of corresponding granule size, and effectively get rid of impurity in the silver powder through the mixture of hydrochloric acid and silver powder, promote the purity of modified silver powder, and then reach and show the purpose that promotes this conductive silver thick liquid's stability.
The invention is further configured to: the resin comprises the following components in parts by weight: 1-2: 0.5-1 of epoxy resin, bismaleimide resin and polyimide resin.
Through adopting above-mentioned technical scheme, bismaleimide resin has excellent heat resistance, electrical insulation, wave permeability, resistant radiation, fire resistance, good mechanical properties and dimensional stability, in the time of coordinating each other with epoxy resin and polyimide resin, through its active end group and epoxy resin and polyimide resin inter combination to increase the overall structure density of resin on epoxy resin solidification forms network structure, in order to reach the purpose that shows the stability that promotes this electrically conductive silver thick liquid.
The invention is further configured to: the auxiliary agent comprises one or two of a dispersing agent, a flatting agent and a coupling agent.
By adopting the technical scheme, the production and manufacturing difficulty of the conductive silver paste is remarkably reduced.
The invention is further configured to: the dispersant is a fatty acid amide dispersant.
By adopting the technical scheme, the fatty acid amide dispersing agent releases amide groups in the stirring and mixing process so as to play a role in increasing friction; meanwhile, a single-layer film for adsorbing polar groups is formed on the surface of the fatty acid amide after stirring and mixing, so that the stirring and mixing uniformity of the resin and the solvent is improved, and simultaneously, the fatty acid amide dispersing agent which is uniformly dispersed is combined with the solvent at the corresponding position, so that the mixing uniformity of the resin and the solvent is further improved, and the effect of uniformly distributing the silver powder is realized after the silver powder is added.
In conclusion, the invention has the following beneficial effects: the formula for preparing the conductive silver paste is prepared by adopting components with proper weight parts, the resin consisting of epoxy resin, bismaleimide resin and polyimide resin is added, and the fatty acid amide dispersant is used as a dispersant, so that the obtained conductive silver paste has the effects of high stability, low curing temperature and remarkably reduced synthesis process difficulty.
Detailed Description
The following description specifically describes the conductive silver paste and the preparation method thereof according to the embodiment of the present invention:
the conductive silver paste comprises the following components in parts by weight:
9-11 parts of resin;
4-6 parts of an auxiliary agent;
78-83 parts of silver powder;
9-11 parts of a solvent.
Wherein the resin is epoxy resin, bismaleimide resin and polyimide resin; and the epoxy resin, the bismaleimide resin and the polyimide resin are mixed according to the weight ratio of 2: 1-2: 0.5-1.
The auxiliary agent comprises fatty acid amide dispersing agent and one or two of flatting agent and coupling agent.
The solvent is organic solvent, and the diameter of the silver powder is 0.2-0.4 μm.
The preparation method of the conductive silver paste comprises the following steps:
step 1, adding 9-11 parts of resin, 4-6 parts of auxiliary agent and 9-11 parts of solvent in parts by weight into a mixer, and mixing to obtain a mixed colloid;
step 2, controlling the temperature of the mixer to 140 ℃ at 120-;
step 3, adding 78-83 parts of silver powder by weight into a mixer, and fully stirring to obtain conductive adhesive;
and 4, sequentially grinding, dispersing, filtering and then defoaming in vacuum to obtain the conductive silver paste.
The silver powder is modified silver powder, and the preparation method of the modified silver powder comprises the following steps of 1) adding the silver powder into a roller ball mill, and adding hydrochloric acid which is 5:1 in parts by weight and has a concentration of 37.5 for primary grinding; 2) adding the primarily ground silver powder into a disc type dryer for drying; 3) adding the dried silver powder into a flat jet mill for further crushing; 4) and screening the silver powder with corresponding particle size by using an airflow classifier to obtain the modified silver powder.
And the resin is prepared from the following components in parts by weight: 1-2: 0.5-1 of epoxy resin, bismaleimide resin and polyimide resin. The auxiliary agent comprises fatty acid amide dispersing agent and one or two of flatting agent and coupling agent.
Example one
The conductive silver paste comprises the following components in parts by weight:
9 parts of resin;
4 parts of an auxiliary agent;
78 parts of silver powder;
and 9 parts of a solvent.
Wherein the resin is epoxy resin, bismaleimide resin and polyimide resin; and the epoxy resin, the bismaleimide resin and the polyimide resin are mixed according to the weight ratio of 2: 1: 0.5.
the auxiliary agent comprises fatty acid amide dispersing agent, flatting agent and coupling agent.
The solvent is organic solvent, and the diameter of the silver powder is 0.2-0.4 μm.
The preparation method of the conductive silver paste comprises the following steps:
step 1, adding 9 parts of resin, 4 parts of auxiliary agent and 9 parts of solvent in parts by weight into a mixer for mixing to obtain a mixed colloid;
step 2, controlling the temperature of the mixer to 120 ℃, and standing for 2 hours;
step 3, adding 78 parts of silver powder by weight into a mixer, and fully stirring to obtain conductive adhesive;
and 4, sequentially grinding, dispersing, filtering and then defoaming in vacuum to obtain the conductive silver paste.
The silver powder is modified silver powder, and the preparation method of the modified silver powder comprises the following steps of 1) adding the silver powder into a roller ball mill, and adding hydrochloric acid which is 5:1 in parts by weight and has a concentration of 37.5 for primary grinding; 2) adding the primarily ground silver powder into a disc type dryer for drying; 3) adding the dried silver powder into a flat jet mill for further crushing; 4) and screening the silver powder with corresponding particle size by using an airflow classifier to obtain the modified silver powder.
And the resin is prepared from the following components in parts by weight: 1: 0.5 epoxy resin, bismaleimide resin, and polyimide resin. The auxiliary agent comprises fatty acid amide dispersing agent, flatting agent and coupling agent.
Example two
The conductive silver paste comprises the following components in parts by weight:
10 parts of resin;
5 parts of an auxiliary agent;
80 parts of silver powder;
10 parts of a solvent.
Wherein the resin is epoxy resin, bismaleimide resin and polyimide resin; and the epoxy resin, the bismaleimide resin and the polyimide resin are mixed according to the weight ratio of 2: 1.5: 0.75.
the auxiliary agent comprises fatty acid amide dispersing agent, flatting agent and coupling agent.
The solvent is organic solvent, and the diameter of the silver powder is 0.2-0.4 μm.
The preparation method of the conductive silver paste comprises the following steps:
step 1, adding 10 parts by weight of resin, 5 parts by weight of auxiliary agent and 10 parts by weight of solvent into a mixer for mixing to obtain a mixed colloid;
step 2, controlling the temperature of the mixer to 130 ℃, and standing for 2.5 hours;
step 3, adding 80 parts by weight of silver powder into a mixer, and fully stirring to obtain conductive adhesive;
and 4, sequentially grinding, dispersing, filtering and then defoaming in vacuum to obtain the conductive silver paste.
The silver powder is modified silver powder, and the preparation method of the modified silver powder comprises the following steps of 1) adding the silver powder into a roller ball mill, and adding hydrochloric acid which is 5:1 in parts by weight and has a concentration of 37.5 for primary grinding; 2) adding the primarily ground silver powder into a disc type dryer for drying; 3) adding the dried silver powder into a flat jet mill for further crushing; 4) and screening the silver powder with corresponding particle size by using an airflow classifier to obtain the modified silver powder.
And the resin is prepared from the following components in parts by weight: 1.5: 0.75 epoxy resin, bismaleimide resin, and polyimide resin. The auxiliary agent comprises fatty acid amide dispersing agent, flatting agent and coupling agent.
EXAMPLE III
The conductive silver paste comprises the following components in parts by weight:
11 parts of resin;
6 parts of an auxiliary agent;
83 parts of silver powder;
and 11 parts of a solvent.
Wherein the resin is epoxy resin, bismaleimide resin and polyimide resin; and the epoxy resin, the bismaleimide resin and the polyimide resin are mixed according to the weight ratio of 2: 2: 1.
the auxiliary agent comprises fatty acid amide dispersing agent, flatting agent and coupling agent.
The solvent is organic solvent, and the diameter of the silver powder is 0.2-0.4 μm.
The preparation method of the conductive silver paste comprises the following steps:
step 1, adding 11 parts by weight of resin, 6 parts by weight of auxiliary agent and 11 parts by weight of solvent into a mixer for mixing to obtain a mixed colloid;
step 2, controlling the temperature of the mixer to 140 ℃, and standing for 3 hours;
step 3, adding 83 parts by weight of silver powder into a mixer, and fully stirring to obtain conductive adhesive;
and 4, sequentially grinding, dispersing, filtering and then defoaming in vacuum to obtain the conductive silver paste.
The silver powder is modified silver powder, and the preparation method of the modified silver powder comprises the following steps of 1) adding the silver powder into a roller ball mill, and adding hydrochloric acid which is 5:1 in parts by weight and has a concentration of 37.5 for primary grinding; 2) adding the primarily ground silver powder into a disc type dryer for drying; 3) adding the dried silver powder into a flat jet mill for further crushing; 4) and screening the silver powder with corresponding particle size by using an airflow classifier to obtain the modified silver powder.
And the resin is prepared from the following components in parts by weight: 2: 1, a bismaleimide resin, and a polyimide resin. The auxiliary agent comprises fatty acid amide dispersing agent, flatting agent and coupling agent.
Example four
Example four differs from example one in that the auxiliary in example four includes a fatty acid amide dispersant and a leveling agent.
EXAMPLE five
Example five differs from example one in that the adjuvant in example five includes a fatty acid amide dispersant and a coupling agent.
EXAMPLE six
The sixth embodiment is different from the first embodiment in that the resin in the sixth embodiment is a resin prepared from the following components in parts by weight: 2: 0.5 epoxy resin, bismaleimide resin, and polyimide resin.
EXAMPLE seven
The seventh embodiment is different from the first embodiment in that the resin in the seventh embodiment is prepared from the following components in parts by weight: 1: 1, a bismaleimide resin, and a polyimide resin.
Comparative example 1
Comparative example one differs from example one in that silver powder having a diameter of 0.2 to 0.8 μm is directly added in comparative example one.
Comparative example No. two
Comparative example two differs from example one in that the resin in comparative example two is an epoxy resin.
Comparative example No. three
Comparative example three differs from example one in that no fatty acid amide dispersant was added to comparative example three.
The first to seventh examples and the first to third comparative examples were tested for performance tests, and the viscosity, adhesive strength and thermal decomposition temperature were measured by conventional techniques, respectively, as shown in table one below.
Table one: test result of conductive silver paste performance test
| Test items | Viscosity (Pas) | Adhesive Strength (MPa) | Temperature of thermal decomposition (. degree.C.) |
| Example one | 23.6 | 29.2 | 375 |
| Example two | 24.1 | 30.3 | 389 |
| EXAMPLE III | 23.5 | 29.6 | 371 |
| Example four | 23.3 | 28.3 | 376 |
| EXAMPLE five | 23.2 | 28.7 | 382 |
| EXAMPLE six | 24.0 | 29.8 | 387 |
| EXAMPLE seven | 23.5 | 28.6 | 373 |
| Comparative example 1 | 26.3 | 22.7 | 323 |
| Comparative example No. two | 25.9 | 23.3 | 316 |
| Comparative example No. three | 26.1 | 21.6 | 322 |
In conclusion, according to the experimental data result in table one, the formula for preparing the conductive silver paste is formed by adopting the components in appropriate parts by weight, and the bismaleimide resin has excellent heat resistance, electrical insulation, wave permeability, radiation resistance, flame retardance, and good mechanical property and dimensional stability, and is mutually cooperated with the epoxy resin and the polyimide resin, so that the overall structural density of the resin is increased on the reticular structure formed by curing the epoxy resin through the mutual combination of the active end group of the bismaleimide resin and the epoxy resin and the polyimide resin, and the purpose of remarkably improving the stability of the conductive silver paste is achieved; the fatty acid amide dispersant releases amide groups in the stirring and mixing process to play a role in increasing friction; meanwhile, a single-layer film for adsorbing polar groups is formed on the surface of the fatty acid amide after stirring and mixing, so that the stirring and mixing uniformity of the resin and the solvent is improved, and simultaneously, the fatty acid amide dispersing agent which is uniformly dispersed is combined with the solvent at the corresponding position, so that the mixing uniformity of the resin and the solvent is further improved, and the effect of uniformly distributing the silver powder is realized after the silver powder is added; the modified silver powder with the corresponding particle size is obtained by adopting a corresponding method, impurities in the silver powder are effectively removed by mixing hydrochloric acid and the silver powder, the purity of the modified silver powder is improved, and the purpose of remarkably improving the stability of the conductive silver paste is further achieved; so that the obtained conductive silver paste has the effects of high stability, low curing temperature and obvious reduction of the difficulty of the synthesis process, and further has the effects of high stability and convenience in production and manufacturing.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiment, but all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the present invention may occur to those skilled in the art without departing from the principle of the present invention, and such modifications and embellishments should also be considered as within the scope of the present invention.
Claims (10)
1. The conductive silver paste is characterized by comprising the following components in parts by weight:
9-11 parts of resin;
4-6 parts of an auxiliary agent;
78-83 parts of silver powder;
9-11 parts of a solvent.
2. The conductive silver paste of claim 1, wherein: the resin is epoxy resin, bismaleimide resin and polyimide resin; and the epoxy resin, the bismaleimide resin and the polyimide resin are mixed according to the weight ratio of 2: 1-2: 0.5-1.
3. The conductive silver paste of claim 1, wherein: the auxiliary agent comprises one or two of a dispersing agent, a flatting agent and a coupling agent.
4. The conductive silver paste of claim 3, wherein: the dispersant is a fatty acid amide dispersant.
5. The conductive silver paste of claim 1, wherein: the solvent is an organic solvent, and the diameter of the silver powder is 0.2-0.4 μm.
6. The preparation method of the conductive silver paste is characterized by comprising the following steps:
step 1, adding 9-11 parts of resin, 4-6 parts of auxiliary agent and 9-11 parts of solvent in parts by weight into a mixer, and mixing to obtain a mixed colloid;
step 2, controlling the temperature of the mixer to 140 ℃ at 120-;
step 3, adding 78-83 parts of silver powder by weight into a mixer, and fully stirring to obtain conductive adhesive;
and 4, sequentially grinding, dispersing, filtering and then defoaming in vacuum to obtain the conductive silver paste.
7. The method for preparing conductive silver paste according to claim 6, wherein the method comprises the following steps: the silver powder is modified silver powder, and the preparation method of the modified silver powder comprises the following steps of 1) adding the silver powder into a roller ball mill, and adding hydrochloric acid which is 5:1 in parts by weight and has a concentration of 37.5 for primary grinding; 2) adding the primarily ground silver powder into a disc type dryer for drying; 3) adding the dried silver powder into a flat jet mill for further crushing; 4) and screening the silver powder with corresponding particle size by using an airflow classifier to obtain the modified silver powder.
8. The method for preparing conductive silver paste according to claim 6, wherein the method comprises the following steps: the resin comprises the following components in parts by weight: 1-2: 0.5-1 of epoxy resin, bismaleimide resin and polyimide resin.
9. The method for preparing conductive silver paste according to claim 6, wherein the method comprises the following steps: the auxiliary agent comprises one or two of a dispersing agent, a flatting agent and a coupling agent.
10. The method for preparing conductive silver paste according to claim 9, wherein the method comprises the following steps: the dispersant is a fatty acid amide dispersant.
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| CN202010907135.1A CN112037963B (en) | 2020-09-02 | 2020-09-02 | Conductive silver paste and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113555145A (en) * | 2021-09-23 | 2021-10-26 | 西安宏星电子浆料科技股份有限公司 | Flexible high-temperature-resistant conductive paste |
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| JP2006245156A (en) * | 2005-03-02 | 2006-09-14 | Ledarts Opto Corp | Light emitting diode device equipped with flip chip structure |
| CN103339685A (en) * | 2011-01-26 | 2013-10-02 | 纳美仕有限公司 | Electroconductive paste and method for manufacturing same |
| CN105139919A (en) * | 2015-08-10 | 2015-12-09 | 东莞市通美电子科技有限公司 | Laser silver paste used for capacitive touch screen as well as preparation method and use method for laser silver paste |
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2020
- 2020-09-02 CN CN202010907135.1A patent/CN112037963B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006245156A (en) * | 2005-03-02 | 2006-09-14 | Ledarts Opto Corp | Light emitting diode device equipped with flip chip structure |
| CN103339685A (en) * | 2011-01-26 | 2013-10-02 | 纳美仕有限公司 | Electroconductive paste and method for manufacturing same |
| CN105139919A (en) * | 2015-08-10 | 2015-12-09 | 东莞市通美电子科技有限公司 | Laser silver paste used for capacitive touch screen as well as preparation method and use method for laser silver paste |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113555145A (en) * | 2021-09-23 | 2021-10-26 | 西安宏星电子浆料科技股份有限公司 | Flexible high-temperature-resistant conductive paste |
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