CN111363493A - Conducting resin with nano core-shell structure and preparation equipment and preparation method thereof - Google Patents
Conducting resin with nano core-shell structure and preparation equipment and preparation method thereof Download PDFInfo
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- CN111363493A CN111363493A CN202010248820.8A CN202010248820A CN111363493A CN 111363493 A CN111363493 A CN 111363493A CN 202010248820 A CN202010248820 A CN 202010248820A CN 111363493 A CN111363493 A CN 111363493A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J193/00—Adhesives based on natural resins; Adhesives based on derivatives thereof
- C09J193/04—Rosin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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Abstract
The invention relates to a nanometer core-shell structure conductive adhesive and a preparation method thereof, wherein the nanometer conductive adhesive comprises, by weight, 0-80 parts of copper, 0-100 parts of silver, 0-79 parts of tin, 16-24 parts of rosin powder, 0-5000 PPM parts of indium, germanium, selenium, cobalt and nickel, and 1-5 parts of additives; the preparation method comprises the steps of firstly preparing nano silver-copper-tin powder by adopting a direct-current hydrogen arc plasma evaporation method, then preparing the nano silver-coated nano silver-copper-tin powder with the nano core-shell structure by utilizing a displacement reaction method, finally mixing the formula in proportion to prepare the conductive adhesive with the nano core-shell structure containing silver, copper and tin elements, filling and storing at constant temperature, wherein the preparation material and preparation cost are low, the prepared conductive adhesive with the nano core-shell structure containing silver, copper and tin elements has excellent electrical conductivity, thermal conductivity and stability and better performance, and the preparation method is easy to realize mass production and processing.
Description
Technical Field
The invention relates to a conductive adhesive with a nano core-shell structure, and preparation equipment and a preparation method thereof, in particular to a conductive adhesive (paste) with a nano core-shell structure containing tin, silver, copper and other elements, and preparation equipment and a preparation method thereof.
Background
With the development of science and technology, the power of 3C products is higher, the frequency is higher, and the heating value is larger and larger! The thermal hazard is more and more serious, for example, the heat dissipation efficiency of the fan is high, but the service life is generally short, certain noise is generated, and how to face the hazard of high heat to the product, the occurrence of the nano conductive adhesive has a positive effect on improving the heat dissipation tongchang performance of the shell; the existing nano conductive adhesive is composed of resin, a filler, an auxiliary agent and the like, and the nano silver powder is used as the filler, so that the conductive adhesive has excellent conductivity and heat conductivity, but the silver is used as a noble metal, and the development of the silver as a conventional material is limited by the reserve and the cost; or the cost can be well controlled by using the nano copper powder as the filler, but the nano copper powder is easy to oxidize in the processing and using processes and has harsh processing and using conditions.
The proportion of the components of the prior heat conducting paste with the nano core-shell structure containing tin, silver, copper and other elements is as follows: 0-70% of copper, 0-65% of silver, 0-98.5% of tin, 8-10% of bisphenol A diglycidyl ether, 8-10% of 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexanecarboxylic acid, 2-8% of neodecanoic acid-epoxypropane methyl ester, 0-5000 PPM of indium In, germanium Ge, selenium Xi, cobalt Co, nickel Ni and 1-5% of additives, but the nonmetal organic polymers In the formula cannot volatilize when meeting high temperature during manufacturing, so that the manufactured heat conducting paste with the nano core-shell structure containing tin, silver and copper elements contains trace auxiliary material components and has poor performance.
Disclosure of Invention
The invention aims to solve the technical problem that the non-metallic organic high molecular material in the formula of the heat conducting paste containing tin, silver, copper and other elements in the existing nano core-shell structure is not volatilized at high temperature, and heat is not easy to dissipate when the heat conducting paste is used, so that the temperature of an electronic element is too high, and the overall performance of the electronic element is influenced.
In order to solve the problems in the prior art, the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, and further comprises rosin powder and an additive in parts by mass, wherein 0-80 parts of copper, 0-100 parts of silver, 0-79 parts of tin, 16-24 parts of rosin powder, 1-5 parts of the additive and polyvinyl pyrrolidone are used as the additive.
Further, the preferential scheme is that the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, rosin powder and an additive, and the conductive adhesive with the nano core-shell structure comprises, by mass, 0-80 parts of copper, 0-100 parts of silver, 0-79 parts of tin, 16-24 parts of rosin powder and 1-5 parts of additive, and further comprises trace indium, germanium, selenium, cobalt and nickel; according to the mass part ratio, the indium, the germanium, the selenium, the cobalt and the nickel are 0-5000 PPM.
Furthermore, the preferred scheme is that the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, and further comprises rosin powder and an additive, wherein the copper is 0.01-75 parts, the silver is 0.1-52 parts, the tin is 0.01-75 parts, the rosin powder is 16.2-23 parts, the indium, germanium, selenium, cobalt and nickel are 0.1-4700 PPM parts, and the additive is 1.5-4.8 parts by mass.
Still further, according to a preferred scheme, the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, and further comprises rosin powder and an additive, wherein in parts by mass, the copper is 5-70 parts, the silver is 10-50 parts, the tin is 0.5-70 parts, the rosin powder is 16.5-22 parts, the indium, germanium, selenium, cobalt and nickel are 100-4600 PPM parts, and the additive is 1.6-4.5 parts.
Still further, according to a preferred scheme, the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, and further comprises rosin powder and an additive, wherein 16-65 parts of copper, 15-48 parts of silver, 10-68 parts of tin, 17-21 parts of rosin powder, 500-3000 PPM parts of indium, germanium, selenium, cobalt and nickel, and 1.8-4.3 parts of the additive are calculated according to the mass parts.
Still further, the preferred scheme is that the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, and further comprises rosin powder and an additive, wherein the copper is 21-50 parts, the silver is 20-47 parts, the tin is 20-64 parts, the rosin powder is 17.3-20 parts, the indium, germanium, selenium, cobalt and nickel are 800-2000 PPM parts, and the additive is 2-4 parts by mass.
Still further, the preferred scheme is that the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, and further comprises rosin powder and an additive, wherein the copper accounts for 25-46 parts, the silver accounts for 28-40 parts, the tin accounts for 26-50 parts, the rosin powder accounts for 17.5-19 parts, the indium, germanium, selenium, cobalt and nickel accounts for 800-1500 PPM parts, and the additive accounts for 2.5-3.9 parts.
Still further, according to a preferred scheme, the conductive adhesive with the nano core-shell structure at least comprises any one element of tin, silver and copper elements, and further comprises rosin powder and an additive, wherein 34-40 parts of copper, 30-32 parts of silver, 30-45 parts of tin, 18-18.5 parts of rosin powder, 850-1300 parts of indium, germanium, selenium, cobalt and nickel, and 2.8-3.6 parts of the additive are calculated according to the mass parts.
In addition, the equipment for preparing the conductive adhesive with the nano core-shell structure comprises a circulating gas path, a nano powder manufacturing chamber, a circulating fan and a nano powder collecting chamber, wherein an outlet of the nano powder manufacturing chamber is arranged in the nano powder collecting chamber, a powder collecting bag arranged in the nano powder collecting chamber is sleeved at the outlet of the nano powder manufacturing chamber, the circulating gas path is communicated with the nano powder manufacturing chamber and the nano powder collecting chamber, and the circulating gas path is provided with the circulating fan; the nanometer powder producing chamber is also provided with a crucible, an electrode, a water-cooled cavity and a water-cooled lower copper mold, the end of the circulating gas path is provided with a blowpipe facing the opening of the crucible, the water-cooled lower copper mold is placed on the water-cooled cavity, and the crucible is placed in the water-cooled cavity.
Furthermore, the preparation method for preparing the conductive adhesive with the nano core-shell structure by using the equipment for preparing the conductive adhesive with the nano core-shell structure is characterized by comprising the following preparation steps,
firstly, preparing nano silver-copper-tin powder,
the method comprises the steps of putting silver-copper-tin alloy into a crucible 22 by a direct current hydrogen arc plasma evaporation method, sealing, vacuumizing to 3 × 10-3-6 × 10-3Pa, filling a proper amount of high-purity argon, starting water circulation in a water-cooling cavity 24, igniting an electrode 23, controlling the current to be 350-500A, starting a fan, blowing silver-copper-tin steam from a mouth of the crucible 22 by a blowing pipe 11, transferring the silver-copper-tin steam to a nano powder collecting chamber 4, closing the electrode 23 after 20-40 minutes, cooling to normal temperature, filling the high-purity argon to normal pressure, and collecting metal nano silver-copper-tin powder in the nano powder collecting chamber 4 for later use, wherein the silver-copper-tin alloy contains trace elements such as indium, germanium, selenium, cobalt and nickel.
2) Preparing silver-coated nano silver-copper-tin powder with a nano core-shell structure,
mixing silver nitrate crystals and distilled water according to the proportion of 1-3%, and stirring for 20-40 minutes by using a magnetic stirrer to obtain a silver nitrate solution;
washing the silver-copper-tin powder I with 15-30% dilute sulfuric acid for 5-15 minutes, keeping the pH value between 1 and 2, repeatedly washing the acid-washed silver-copper-tin powder I with distilled water until no silver-copper-tin ions exist, repeatedly washing until the pH value is neutral, and spin-drying with a centrifuge to obtain silver-copper-tin powder II;
then, sensitizing the treated silver-copper-tin powder II in 30g/L stannous chloride hydrochloric acid sensitizing solution for 5-15 minutes, and then washing with distilled water to obtain silver-copper-tin powder solution A;
then filtering the silver-copper-tin powder liquid A, dropwise adding a silver nitrate solution, adjusting the pH value of the silver-copper-tin powder liquid A to 4, dropwise adding a silver-ammonia solution, fully mixing and reacting for 8-15 minutes, dropwise adding ammonia water until the pH value is 9, reacting for 25-40 minutes, finally separating and washing by using a centrifugal machine to obtain silver-coated silver-copper-tin powder liquid B, placing the prepared silver-coated silver-copper-tin powder liquid B into a container, adding a proper amount of distilled water, placing into a 70 ℃ constant temperature tank, standing for 3H, performing suction filtration by using the centrifugal machine, and drying to obtain silver-coated silver-copper-tin powder;
3) preparing the conductive adhesive with the nano core-shell structure containing silver, copper and tin elements,
and mixing the prepared silver-coated silver-copper-tin powder, rosin powder and additive according to the proportion, fully stirring to prepare the conductive adhesive with the nano core-shell structure containing silver, copper and tin elements, filling, and preserving at constant temperature.
The conductive adhesive with the nano core-shell structure has low manufacturing material and preparation cost, and the manufactured nano silver-coated copper conductive adhesive has excellent electrical conductivity, thermal conductivity and stability and better performance.
Where PPM concentration (parts per million) is the concentration expressed in parts per million of solute mass in the total solution mass, also known as parts per million concentration. It is often used in very small concentrations, and similarly ppb (parts per billion).
The invention relates to a prepared conductive adhesive with a nano core-shell structure, in particular to a conductive adhesive with a nano core-shell structure containing elements such as tin, silver and copper and a heat conducting slurry, wherein high molecular components such as bisphenol A diglycidyl ether, 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexane carboxylic acid, neodecanoic acid-propylene oxide methyl ester and the like are replaced by rosin powder on the basis of the prior art, the original organic polymer has no volatility, the existing rosin powder has volatility, so that auxiliary materials can be volatilized at high temperature during the preparation of the whole conductive adhesive, no residual auxiliary materials are remained in the finished conductive adhesive with the nano core-shell structure, and the whole conductive adhesive with the nano core-shell structure containing elements such as tin, silver and copper has the characteristics that: the oxide layer can be effectively prevented from being generated on the surface of the copper powder, the cost of the material used for manufacturing is low, and the manufactured silver-coated nano silver-copper-tin powder conductive adhesive with the nano core-shell structure has excellent electrical conductivity, thermal conductivity and stability, and is easy to realize mass production processing.
Drawings
Fig. 1 is a schematic diagram of the apparatus for preparing a conductive adhesive with a nano core-shell structure according to the present invention.
Detailed Description
In order that those skilled in the art can better understand the technical solution of the present invention, the following embodiments are further described with reference to the accompanying drawings and examples.
As shown in fig. 1, a device for preparing a conductive adhesive with a nano core-shell structure comprises a circulating gas path 1, a nano powder production chamber 2, a circulating fan 3 and a nano powder collection chamber 4, wherein an outlet 21 of the nano powder production chamber 2 is arranged in the nano powder collection chamber 4, a powder collection bag 41 arranged in the nano powder collection chamber 4 is sleeved at the outlet 21, the circulating gas path 1 is communicated with the nano powder production chamber 2 and the nano powder collection chamber 4, and the circulating fan 3 is arranged on the circulating gas path 1; a crucible 22, an electrode 23, a water-cooling cavity 24 and a water-cooling lower copper mold 25 are also arranged in the nano powder manufacturing chamber 2, a blowpipe 11 facing the opening of the crucible 22 is arranged at the end of the circulating gas path 1, the water-cooling lower copper mold 25 is arranged on the water-cooling cavity 24, and the crucible 22 is arranged in the water-cooling cavity 24.
The formulas of a specific example and a comparative example of the conductive adhesive with the nano core-shell structure are shown in the following table (in parts by mass, the unit is gram), wherein the performances of the conductive adhesive (paste) with the nano core-shell structure containing silver, copper and tin elements are compared with those of the examples.
The preparation method of the conductive adhesive with the nano core-shell structure containing silver, copper, tin and other elements, which is prepared in the above 1-18 embodiments, comprises the following steps:
1) preparing the nano silver-copper-tin powder,
adopting a direct current hydrogen arc plasma evaporation method, putting the silver-copper-tin alloy into the crucible 22, sealing and vacuumizing to 3 × 10-3Pa～6×10-3Pa, then filling a proper amount of high-purity argon, starting water circulation in the water-cooling cavity 24, igniting the electrode 23, and controlling the current within the range of 350-500A; then, a fan is started, the blowpipe 11 blows out silver, copper and tin steam from a mouth of the crucible 22, the silver, copper and tin steam is transferred to the nano powder collecting chamber 4, after 20-40 minutes, the electrode 23 is closed, after cooling to normal temperature, high-purity argon is filled to normal pressure, and metal nano silver, copper and tin powder in the nano powder collecting chamber 4 is collected for later use; wherein the silver-copper-tin alloy contains indium, germanium, selenium, cobalt and nickel microelements.
2) Preparing silver-coated nano silver-copper-tin powder with a nano core-shell structure,
mixing silver nitrate crystals and distilled water according to the proportion of 1-3%, and stirring for 20-40 minutes by using a magnetic stirrer to obtain a silver nitrate solution;
washing the silver-copper-tin powder I with 15-30% dilute sulfuric acid for 5-15 minutes, keeping the pH value between 1 and 2, repeatedly washing the acid-washed silver-copper-tin powder I with distilled water until no silver-copper-tin ions exist, repeatedly washing until the pH value is neutral, and spin-drying with a centrifuge to obtain silver-copper-tin powder II;
then, sensitizing the treated silver-copper-tin powder II in 30g/L stannous chloride hydrochloric acid sensitizing solution for 5-15 minutes, and then washing with distilled water to obtain silver-copper-tin powder solution A;
then filtering the silver-copper-tin powder liquid A, dropwise adding a silver nitrate solution, adjusting the pH value of the silver-copper-tin powder liquid A to 4, dropwise adding a silver-ammonia solution, fully mixing and reacting for 8-15 minutes, dropwise adding ammonia water until the pH value is 9, reacting for 25-40 minutes, finally separating and washing by using a centrifugal machine to obtain silver-coated silver-copper-tin powder liquid B, placing the prepared silver-coated silver-copper-tin powder liquid B into a container, adding a proper amount of distilled water, placing into a 70 ℃ constant temperature tank, standing for 3H, performing suction filtration by using the centrifugal machine, and drying to obtain silver-coated silver-copper-tin powder;
3) preparing the conductive adhesive with the nano core-shell structure containing silver, copper and tin elements,
and mixing the prepared silver-coated silver-copper-tin powder, rosin powder and additive according to the proportion, fully stirring to prepare the conductive adhesive with the nano core-shell structure containing silver, copper and tin elements, filling, and preserving at constant temperature.
The conductive adhesive with the nano core-shell structure provided by the invention is described in detail above. The description of the embodiments is only for the purpose of helping understanding the method of the present invention and the core idea thereof, and it should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims (10)
1. The conductive adhesive with the nano core-shell structure at least comprises any one of tin, silver and copper elements, and is characterized by further comprising rosin powder and an additive in parts by mass, wherein 0-80 parts of copper, 0-100 parts of silver, 0-79 parts of tin, 16-24 parts of rosin powder, 1-5 parts of additive and polyvinyl pyrrolidone as the additive.
2. The core-shell nanostructure conductive adhesive of claim 1, further comprising trace amounts of indium, germanium, selenium, cobalt, nickel; according to the mass part ratio, the indium, the germanium, the selenium, the cobalt and the nickel are 0-5000 PPM.
3. The conductive adhesive with a nano core-shell structure according to claim 2, wherein the copper is 0.01 to 75 parts, the silver is 0.1 to 52 parts, the tin is 0.01 to 75 parts, the rosin powder is 16.2 to 23 parts, the indium, germanium, selenium, cobalt and nickel are 0.1 to 4700PPM parts, and the additive is 1.5 to 4.8 parts by mass.
4. The conductive adhesive with a nano core-shell structure according to claim 3, wherein the copper is 5-70 parts, the silver is 10-50 parts, the tin is 0.5-70 parts, the rosin powder is 16.5-22 parts, the indium, the germanium, the selenium, the cobalt and the nickel are 100-4600 PPM parts, and the additive is 1.6-4.5 parts by weight.
5. The conductive adhesive with a nano core-shell structure according to claim 4, wherein the copper is 16-65 parts, the silver is 15-48 parts, the tin is 10-68 parts, the rosin powder is 17-21 parts, the indium, germanium, selenium, cobalt and nickel are 500-3000 PPM parts, and the additive is 1.8-4.3 parts by mass.
6. The conductive adhesive with a nano core-shell structure according to claim 5, wherein the copper is 21-50 parts, the silver is 20-47 parts, the tin is 20-64 parts, the rosin powder is 17.3-20 parts, the indium, the germanium, the selenium, the cobalt and the nickel are 800-2000 PPM parts, and the additive is 2-4 parts by mass.
7. The conductive adhesive with a nano core-shell structure according to claim 6, wherein the copper is 25-46 parts, the silver is 28-40 parts, the tin is 26-50 parts, the rosin powder is 17.5-19 parts, the indium, the germanium, the selenium, the cobalt and the nickel are 800-1500 PPM parts, and the additive is 2.5-3.9 parts by mass.
8. The conductive adhesive with a nano core-shell structure according to claim 7, wherein the copper is 34-40 parts, the silver is 30-32 parts, the tin is 30-45 parts, the rosin powder is 18-18.5 parts, the indium, germanium, selenium, cobalt and nickel are 850-1300 PPM parts, and the additive is 2.8-3.6 parts by mass.
9. The apparatus for preparing conducting resin with nano core-shell structure according to claim 2-8, comprising a circulating gas path, a nano powder producing chamber, a circulating fan and a nano powder collecting chamber, wherein the outlet of the nano powder producing chamber is disposed in the nano powder collecting chamber, and the outlet is sleeved with a powder collecting bag disposed in the nano powder collecting chamber, the circulating gas path is communicated with the nano powder producing chamber and the nano powder collecting chamber, and the circulating gas path is provided with the circulating fan; the nanometer powder producing chamber is also provided with a crucible, an electrode, a water-cooled cavity and a water-cooled lower copper mold, the end of the circulating gas path is provided with a blowpipe facing the opening of the crucible, the water-cooled lower copper mold is placed on the water-cooled cavity, and the crucible is placed in the water-cooled cavity.
10. The preparation method for manufacturing the conductive adhesive with the nano core-shell structure by adopting the equipment of claim 9 is characterized by comprising the following preparation steps,
1) preparing the nano silver-copper-tin powder,
putting silver-copper-tin alloy into a crucible by adopting a direct current hydrogen arc plasma evaporation method, sealing and vacuumizing to 3 × 10-3 Pa-6 × 10-3Pa, then filling a proper amount of high-purity argon, starting water circulation in a water-cooling cavity, igniting an electrode, controlling the current to be within the range of 350-500A, then starting a fan, blowing silver-copper-tin steam emitted from the opening of the crucible by a blowpipe 11, transferring the silver-copper-tin steam to a nano powder collecting chamber, closing the electrode after 20-40 minutes, cooling to normal temperature, filling high-purity argon to normal pressure, collecting metal nano silver-copper-tin powder in the nano powder collecting chamber for later use, wherein the silver-copper-tin alloy contains indium, germanium, selenium, cobalt and nickel microelements,
2) preparing silver-coated nano silver-copper-tin powder with a nano core-shell structure,
mixing silver nitrate crystals and distilled water according to the proportion of 1-3%, and stirring for 20-40 minutes by using a magnetic stirrer to obtain a silver nitrate solution;
washing the silver-copper-tin powder I with 15-30% dilute sulfuric acid for 5-15 minutes, keeping the pH value between 1 and 2, repeatedly washing the acid-washed silver-copper-tin powder I with distilled water until no silver-copper-tin ions exist, repeatedly washing until the pH value is neutral, and spin-drying with a centrifuge to obtain silver-copper-tin powder II;
then, sensitizing the treated silver-copper-tin powder II in 30g/L stannous chloride hydrochloric acid sensitizing solution for 5-15 minutes, and then washing with distilled water to obtain silver-copper-tin powder solution A;
then filtering the silver-copper-tin powder liquid A, dropwise adding a silver nitrate solution, adjusting the pH value of the silver-copper-tin powder liquid A to 4, dropwise adding a silver-ammonia solution, fully mixing and reacting for 8-15 minutes, dropwise adding ammonia water until the pH value is 9, reacting for 25-40 minutes, finally separating and washing by using a centrifugal machine to obtain silver-coated silver-copper-tin powder liquid B, placing the prepared silver-coated silver-copper-tin powder liquid B into a container, adding a proper amount of distilled water, placing into a 70 ℃ constant temperature tank, standing for 3H, performing suction filtration by using the centrifugal machine, and drying to obtain silver-coated silver-copper-tin powder;
3) preparing the conductive adhesive with the nano core-shell structure containing silver, copper and tin elements,
and mixing the prepared silver-coated silver-copper-tin powder, rosin powder and additive according to the proportion, fully stirring to prepare the conductive adhesive with the nano core-shell structure containing silver, copper and tin elements, filling, and preserving at constant temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113528054A (en) * | 2021-07-15 | 2021-10-22 | 山西贝特瑞新能源科技有限公司 | Breathable conductive adhesive for lithium battery crucible and preparation method of breathable conductive adhesive |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486095A (en) * | 2009-02-27 | 2009-07-22 | 北京工业大学 | Oxidation-resistant organic coating method of welding powder |
| CN108160990A (en) * | 2018-01-05 | 2018-06-15 | 广东工业大学 | A kind of nano particle interconnection material of nucleocapsid and preparation method thereof |
| CN109128568A (en) * | 2018-08-09 | 2019-01-04 | 重庆源晶电子材料有限公司 | A kind of nano-core-shell structure soldering paste and preparation method thereof |
| US20200133088A1 (en) * | 2009-03-31 | 2020-04-30 | View, Inc. | Counter electrode for electrochromic devices |
-
2020
- 2020-04-01 CN CN202010248820.8A patent/CN111363493A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486095A (en) * | 2009-02-27 | 2009-07-22 | 北京工业大学 | Oxidation-resistant organic coating method of welding powder |
| US20200133088A1 (en) * | 2009-03-31 | 2020-04-30 | View, Inc. | Counter electrode for electrochromic devices |
| CN108160990A (en) * | 2018-01-05 | 2018-06-15 | 广东工业大学 | A kind of nano particle interconnection material of nucleocapsid and preparation method thereof |
| CN109128568A (en) * | 2018-08-09 | 2019-01-04 | 重庆源晶电子材料有限公司 | A kind of nano-core-shell structure soldering paste and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113528054A (en) * | 2021-07-15 | 2021-10-22 | 山西贝特瑞新能源科技有限公司 | Breathable conductive adhesive for lithium battery crucible and preparation method of breathable conductive adhesive |
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