CN109887638B - Multi-scale nano silver paste mixed by nano silver particles and silver-plated silicon carbide particles and preparation method thereof - Google Patents
Multi-scale nano silver paste mixed by nano silver particles and silver-plated silicon carbide particles and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multi-scale nano silver paste mixed by nano silver particles and silver-plated silicon carbide particles and a preparation method thereof, relates to a novel interface interconnection material, and particularly relates to a multi-scale nano silver paste added with silver-plated silicon carbide particles, which comprises a formula and a preparation process thereof. The invention is prepared from triethylene glycol, polyvinyl butyral, terpineol, nano silver particles and submicron silver-plated silicon carbide particles, and the mass percentages of the components are as follows: 0.5-1.2% of triethylene glycol, 5.6-12.2% of polyvinyl butyral, 3.89-8.56% of terpineol, 76-90% of nano silver particles and 0.5-2% of silver-plated silicon carbide particles. According to the invention, silicon carbide particles are used for replacing part of nano silver particles to be added into the silver paste, so that the porosity of the silver paste after sintering is reduced, the performance of the silver paste is improved, the cost of the nano silver paste is reduced, and the performance of the silver paste after sintering is improved.
Description
Technical Field
The invention relates to a nano silver material and a preparation method thereof, in particular to a nano silver paste and a preparation method thereof, which are applied to the technical field of interface interconnection materials and processes.
Background
With the development of semiconductor technology, chip output power is increased, frequency is increased, electronic products are miniaturized, and particularly, with the emergence of novel silicon carbide integrated circuit chips capable of working in a high-temperature environment of more than 250 ℃, the ambient temperature of the chip working is greatly increased, solder remelting can be caused at high temperature to influence the reliability of the chip, the lower thermal conductivity of the traditional interface material cannot meet the requirement of a high-power-density packaging system on heat dissipation, and the nano silver paste becomes the most promising interface interconnection material at present by virtue of the excellent performance of low-temperature sintering and high-temperature service.
The nano silver particles are used as main fillers of the nano silver paste, and the development and the application of the nano silver paste are restricted by the high cost of the nano silver particles. Silicon carbide has heat conduction performance comparable to silver, but the price of silicon carbide is several times lower than that of silver, so that the silicon carbide is a low-cost heat conduction material expected to replace silver particles, and in addition, the silicon carbide also has a plurality of excellent characteristics, such as high hardness, high strength, good creep resistance, chemical corrosion resistance, good oxidation resistance, small thermal expansion coefficient, high heat conductivity and the like, but the sintering temperature of the silicon carbide particles is high, the porosity after sintering is high, the brittleness of the material after sintering of the silicon carbide particles is large, the interconnection with a semiconductor substrate is not ideal, and the heat dissipation effect is influenced.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art and provide the multi-scale nano silver paste with the mixed nano silver particles and silver-plated silicon carbide particles and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a multi-scale nano silver paste mixed by nano silver particles and silver-plated silicon carbide particles is prepared from triethylene glycol, polyvinyl butyral, terpineol, nano silver particles and submicron silver-plated silicon carbide particles, and the mass percentages of the components are as follows:
the sum of the mass percentages of all the components is 100 percent.
As the preferred technical scheme of the invention, the multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles comprises the following components in percentage by mass:
the sum of the mass percentages of all the components is 100 percent.
As a preferred technical scheme of the invention, the silver-plated silicon carbide particles are beta-silicon carbide, the average particle size of the beta-silicon carbide particles is 0.1-5 microns, and the structure of the silver-plated silicon carbide particles is as follows: and coating a silver layer with the thickness of 10-100 nanometers on the surface of the silicon carbide particle to form the composite silicon carbide particle which wraps the silver shell and has a metal-inorganic nonmetal composite structure.
Preferably, the silver layer on the surface of the silver-plated silicon carbide particles is formed on the surface of the silicon carbide particles by electroless plating, deposition or sputtering.
The average particle diameter of the nano silver particles is preferably 5 to 30 nm.
Preferably, the above-mentioned triethylene glycol is used as a dispersant and starts to decompose at not less than 100 ℃.
The above-mentioned polyvinyl butyral is preferably used as an organic vehicle and starts to decompose at not less than 300 ℃.
Terpineol is preferably used as a diluent to start decomposition at not less than 60 ℃.
The invention relates to a preparation method of multi-scale nano silver paste mixed by nano silver particles and silver-plated silicon carbide particles, which takes raw materials of each component according to a component formula in the multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles prepared by a target, and comprises the following steps:
a. adding absolute ethyl alcohol into a beaker as a basic solvent, heating, adding polyvinyl butyral into the beaker while stirring, and fully mixing the polyvinyl butyral and the ethyl alcohol to form a carrier solvent for later use; preferably the heating temperature is not lower than 60 ℃ and lower than the boiling point temperature of ethanol;
b. cooling the mixed carrier solvent prepared in the step a, adding triethylene glycol and terpineol into the mixed carrier solvent after cooling to room temperature, and dispersing and diluting the mixed carrier solvent to obtain carrier dispersion liquid;
c. b, stirring the carrier dispersion liquid prepared in the step b at room temperature, adding the nano silver particles and the silver-plated silicon carbide particles into the carrier dispersion liquid while stirring, and controlling the stirring time for at least 15min to obtain mixed slurry of the nano silver particles and the silver-plated silicon carbide particles;
d. and c, post-treating the mixed slurry prepared in the step c, performing ultrasonic homogenization treatment, and when performing ultrasonic treatment on the mixed slurry, adding ice blocks or ice water into the mixed slurry to cool, controlling the temperature of the mixed slurry to be not higher than 28 ℃, and performing ultrasonic treatment for not less than 30min to obtain the multi-scale nano silver slurry mixed by the nano silver particles and the silver-plated silicon carbide particles after the ultrasonic homogenization treatment process is finished.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. according to the invention, by mixing the nano particles and the submicron silver-plated silicon carbide particles, the small-sized nano silver particles are filled in gaps among the large-sized silver-plated silicon carbide particles, so that the porosity of the silver paste after sintering can be reduced, the performance of the silver paste is improved, the silicon carbide also has a lower thermal expansion coefficient, the reliability of the silver paste can be improved, and the performance of the silver paste after sintering is improved;
2. the silicon carbide particles are adopted to replace a small amount of nano silver particles, so that the cost of the silver paste is reduced;
3. the preparation method of the composite nano silver paste is simple and easy to control, fully utilizes the material performance advantages of the nano silver particles and the silicon carbide particles, fully fuses the silicon carbide particles and the nano silver by modifying and optimizing the surfaces of the silicon carbide particles to form a nano silver particle-silicon carbide particle composite silver paste system, and can be better used as a precursor slurry material of an interface interconnection material.
Drawings
FIG. 1 is an SEM image of silver-plated silicon carbide particles according to a preferred embodiment of the present invention.
Fig. 2 is a schematic diagram of multi-scale particle mixing of a sintered material obtained after sintering of multi-scale nano silver paste mixed with nano silver particles and silver-plated silicon carbide particles according to a preferred embodiment of the present invention.
Fig. 3 is a flow chart of a silver paste preparation process according to a preferred embodiment of the invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in this embodiment, referring to fig. 1 to fig. 3, a method for preparing a multi-scale nano silver paste with nano silver particles mixed with silver-plated silicon carbide particles includes the following steps:
a. adding 30ml of absolute ethyl alcohol into a beaker as a basic solvent, placing the beaker on a heating table, heating the beaker to 60 ℃, weighing 0.8g of polyvinyl butyral by using a balance, adding the polyvinyl butyral into the beaker while stirring, and fully mixing the polyvinyl butyral and the ethyl alcohol to form a carrier solvent for later use; the heating temperature is lower than the boiling point temperature of the ethanol, so that the volatilization amount of the ethanol is reduced, the solvent is saved, the solvent consumption is reduced, and the polyvinyl butyral polymer is beneficial to uniformly mixing in the ethanol base solvent under the heating condition;
b. cooling the mixed carrier solvent prepared in the step a, placing a beaker on a balance after cooling to room temperature, adding 0.08g of triethylene glycol and 0.56g of terpineol into the mixed carrier solvent, and dispersing and diluting the mixed carrier solvent to obtain carrier dispersion liquid;
c. b, placing the beaker under a mechanical stirrer at room temperature, stirring the carrier dispersion liquid prepared in the step b, adding 6.52g of nano-silver particles and 0.04g of silver-plated silicon carbide particles into the carrier dispersion liquid while stirring, and controlling the stirring time to be 15min to obtain mixed slurry of the nano-silver particles and the silver-plated silicon carbide particles; the average grain diameter of the nano silver particles is 5-30 nanometers;
d. and c, post-treating the mixed slurry prepared in the step c, performing ultrasonic homogenization treatment, and when performing ultrasonic treatment on the mixed slurry, adding ice blocks or ice water into the mixed slurry to cool, controlling the temperature of the mixed slurry to be lower than 28 ℃, performing ultrasonic treatment for 30min, and obtaining the multi-scale nano silver slurry mixed by the nano silver particles and the silver-plated silicon carbide particles after the ultrasonic homogenization treatment process is finished.
In this example, microscopic SEM observation is performed on the silver-plated silicon carbide particles adopted in this example, fig. 1 is an SEM image of the silver-plated silicon carbide particles, the silver-plated silicon carbide particles are β -silicon carbide, the average particle size of the silver-plated silicon carbide particles is 0.1 to 5 μm, and the structure of the silver-plated silicon carbide particles is: coating a silver layer with the thickness of 10-100 nanometers on the surface of the silicon carbide particle to form composite carbonized with a metal-inorganic nonmetal composite structure wrapping a silver shellSilicon particles. The surface of the silicon carbide particles is modified and optimized through chemical vapor deposition, and a surface silver layer is generated on the surfaces of the silicon carbide particles to prepare the silver-plated silicon carbide particles. The thermal conductivity of the sintered material obtained by sintering the multi-scale nano silver paste mixed with the nano silver particles and the silver-plated silicon carbide particles as the interconnection material is 124W/m-K, and the thermal expansion coefficient is 2.82 multiplied by 10-5and/K. Fig. 2 is a schematic diagram of a multi-scale particle mixture of a sintered material obtained after sintering a multi-scale nano silver paste in which nano silver particles and silver-plated silicon carbide particles are mixed, the nano silver particles with small sizes are filled in gaps among the silver-plated silicon carbide particles with larger sizes by mixing the nano particles and the submicron silver-plated silicon carbide particles, so that the porosity of the silver paste after sintering is reduced, the performance of the silver paste is improved, and the silicon carbide also has a lower thermal expansion coefficient, so that the reliability of the silver paste can be improved.
Example two:
this embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, referring to fig. 1 to fig. 3, a method for preparing a multi-scale nano silver paste with nano silver particles mixed with silver-plated silicon carbide particles includes the following steps:
a. adding 30ml of absolute ethyl alcohol into a beaker as a basic solvent, placing the beaker on a heating table, heating the beaker to 60 ℃, weighing 0.444g of polyvinyl butyral by using a balance, adding the polyvinyl butyral into the beaker while stirring, and fully mixing the polyvinyl butyral and the ethyl alcohol to form a carrier solvent for later use; the heating temperature is lower than the boiling point temperature of the ethanol, so that the volatilization amount of the ethanol is reduced, the solvent is saved, the solvent consumption is reduced, and the polyvinyl butyral polymer is beneficial to uniformly mixing in the ethanol base solvent under the heating condition;
b. cooling the mixed carrier solvent prepared in the step a, placing a beaker on a balance after cooling to room temperature, adding 0.044g of triethylene glycol and 0.311g of terpineol into the mixed carrier solvent, and dispersing and diluting the mixed carrier solvent to obtain carrier dispersion liquid;
c. b, placing the beaker under a mechanical stirrer at room temperature, stirring the carrier dispersion liquid prepared in the step b, adding 7.16g of nano-silver particles and 0.04g of silver-plated silicon carbide particles into the carrier dispersion liquid while stirring, and controlling the stirring time to be 15min to obtain mixed slurry of the nano-silver particles and the silver-plated silicon carbide particles;
d. and c, post-treating the mixed slurry prepared in the step c, performing ultrasonic homogenization treatment, and when performing ultrasonic treatment on the mixed slurry, adding ice blocks or ice water into the mixed slurry to cool, controlling the temperature of the mixed slurry to be lower than 28 ℃, performing ultrasonic treatment for 30min, and obtaining the multi-scale nano silver slurry mixed by the nano silver particles and the silver-plated silicon carbide particles after the ultrasonic homogenization treatment process is finished.
In this embodiment, as shown in fig. 1-3. Microscopic SEM observation is performed on the silver-plated silicon carbide particles adopted in the embodiment, and FIG. 1 is an SEM picture of the silver-plated silicon carbide particles, the silver-plated silicon carbide particles are beta-silicon carbide, the average particle size of the silver-plated silicon carbide particles is 0.1-5 microns, and the structures of the silver-plated silicon carbide particles are as follows: and coating a silver layer with the thickness of 10-100 nanometers on the surface of the silicon carbide particle to form the composite silicon carbide particle which wraps the silver shell and has a metal-inorganic nonmetal composite structure. The surface of the silicon carbide particles is modified and optimized by chemical plating, and a surface silver layer is generated on the surfaces of the silicon carbide particles to prepare the silver-plated silicon carbide particles. The thermal conductivity of the sintered material obtained by sintering the multi-scale nano silver paste mixed with the nano silver particles and the silver-plated silicon carbide particles as the interconnection material is 124W/m-K, and the thermal expansion coefficient is 2.82 multiplied by 10-5and/K. Fig. 2 is a schematic diagram of a multi-scale particle mixture of a sintered material obtained after sintering a multi-scale nano silver paste in which nano silver particles and silver-plated silicon carbide particles are mixed, the nano silver particles with small sizes are filled in gaps among the silver-plated silicon carbide particles with larger sizes by mixing the nano particles and the submicron silver-plated silicon carbide particles, so that the porosity of the silver paste after sintering is reduced, the performance of the silver paste is improved, and the silicon carbide also has a lower thermal expansion coefficient, so that the reliability of the silver paste can be improved.
Example three:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, referring to fig. 1 to fig. 3, a method for preparing a multi-scale nano silver paste with nano silver particles mixed with silver-plated silicon carbide particles includes the following steps:
a. adding 30ml of absolute ethyl alcohol into a beaker as a basic solvent, placing the beaker on a heating table, heating the beaker to 60 ℃, weighing 0.8g of polyvinyl butyral by using a balance, adding the polyvinyl butyral into the beaker while stirring, and fully mixing the polyvinyl butyral and the ethyl alcohol to form a carrier solvent for later use; the heating temperature is lower than the boiling point temperature of the ethanol, so that the volatilization amount of the ethanol is reduced, the solvent is saved, the solvent consumption is reduced, and the polyvinyl butyral polymer is beneficial to uniformly mixing in the ethanol base solvent under the heating condition;
b. cooling the mixed carrier solvent prepared in the step a, placing a beaker on a balance after cooling to room temperature, adding 0.08g of triethylene glycol and 0.56g of terpineol into the mixed carrier solvent, and dispersing and diluting the mixed carrier solvent to obtain carrier dispersion liquid;
c. b, placing the beaker under a mechanical stirrer at room temperature, stirring the carrier dispersion liquid prepared in the step b, adding 6.4g of nano-silver particles and 0.16g of silver-plated silicon carbide particles into the carrier dispersion liquid while stirring, and controlling the stirring time to be 15min to obtain mixed slurry of the nano-silver particles and the silver-plated silicon carbide particles;
d. and c, post-treating the mixed slurry prepared in the step c, performing ultrasonic homogenization treatment, and when performing ultrasonic treatment on the mixed slurry, adding ice blocks or ice water into the mixed slurry to cool, controlling the temperature of the mixed slurry to be lower than 28 ℃, performing ultrasonic treatment for 30min, and obtaining the multi-scale nano silver slurry mixed by the nano silver particles and the silver-plated silicon carbide particles after the ultrasonic homogenization treatment process is finished.
In this embodiment, as shown in fig. 1-3. Microscopic SEM observation is performed on the silver-plated silicon carbide particles adopted in the embodiment, and FIG. 1 is an SEM picture of the silver-plated silicon carbide particles, the silver-plated silicon carbide particles are beta-silicon carbide, the average particle size of the silver-plated silicon carbide particles is 0.1-5 microns, and the structures of the silver-plated silicon carbide particles are as follows: the surface of the silicon carbide particles is coated with a thickness of 10 to 100 nanometersAnd a silver layer is arranged on the surface of the silicon substrate to form composite silicon carbide particles which wrap the silver shell and have a metal-inorganic nonmetal composite structure. The surface of the silicon carbide particles is modified and optimized by a sputtering method, and a surface silver layer is generated on the surfaces of the silicon carbide particles to prepare the silver-plated silicon carbide particles. The thermal conductivity of the sintered material obtained by sintering the multi-scale nano silver paste mixed with the nano silver particles and the silver-plated silicon carbide particles as the interconnection material is 124W/m-K, and the thermal expansion coefficient is 2.82 multiplied by 10-5and/K. Fig. 2 is a schematic diagram of a multi-scale particle mixture of a sintered material obtained after sintering a multi-scale nano silver paste in which nano silver particles and silver-plated silicon carbide particles are mixed, the nano silver particles with small sizes are filled in gaps among the silver-plated silicon carbide particles with larger sizes by mixing the nano particles and the submicron silver-plated silicon carbide particles, so that the porosity of the silver paste after sintering is reduced, the performance of the silver paste is improved, and the silicon carbide also has a lower thermal expansion coefficient, so that the reliability of the silver paste can be improved.
In summary, in the multi-scale nano silver paste in which the nano silver particles and the silver-plated silicon carbide particles are mixed, silicon carbide particles are used for replacing part of the nano silver particles to be added into the silver paste, the silicon carbide has heat conduction performance comparable to that of silver, but the price of the silicon carbide is several times lower than that of the silver, and submicron silicon carbide particles are used for replacing part of the nano silver particles, so that the cost of the silver paste can be reduced. In order to solve the problem that the silicon carbide cannot be interconnected with the silver particles in the sintering process, the embodiment plates the nano silver layer on the silicon carbide surface by chemical plating, evaporation and sputtering. The multi-scale silver paste is prepared from triethylene glycol, polyvinyl butyral, terpineol, nano silver particles and submicron silver-plated silicon carbide particles. The novel interface interconnection material is prepared, the multi-scale nano silver paste with the silver-plated silicon carbide particles is added, the formula and the preparation process are adopted, the silicon carbide particles are used for replacing part of nano silver particles to be added into the silver paste, the cost can be reduced, the mechanical reliability of the nano silver paste can be well improved, and the novel interface interconnection material has good application value in the field of microelectronics, particularly in the field of aerospace electronics. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles prepared in the embodiment is used as a sintering material precursor material, and ethanol is continuously volatilized in the sintering temperature rise process and the sintering process; terpineol is used as a diluent to start decomposition at 60 ℃; triethylene glycol is used as a dispersant to start decomposition at 100 ℃; polyvinyl butyral was used as the organic vehicle and decomposition started at 300 ℃. The composite nano silver paste prepared by the embodiment becomes the interface interconnection material with the most prospect at present by virtue of the excellent performance of low-temperature sintering and high-temperature service, the cost of the nano silver paste can be reduced, and the performance of the silver paste after sintering is improved. The multi-scale nano silver paste is prepared by the embodiment, and the nano particles and the submicron silver-plated silicon carbide particles are mixed, so that the small-sized nano silver particles are filled in gaps among the large-sized silver-plated silicon carbide particles, the porosity of the silver paste after sintering can be reduced, the performance of the silver paste is improved, the silicon carbide also has a lower thermal expansion coefficient, and the reliability of the silver paste can be improved. In addition, the silicon carbide particles are adopted to replace a small amount of nano silver particles, so that the cost of the silver paste can be reduced.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and all changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitution ways, so long as the purpose of the present invention is met, and the multi-scale nano silver paste mixed by nano silver particles and silver-plated silicon carbide particles and the preparation method thereof and the inventive concept thereof shall not depart from the technical principle and inventive concept of the present invention.
Claims (10)
1. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles is characterized by being prepared from triethylene glycol, polyvinyl butyral, terpineol, nano silver particles and submicron silver-plated silicon carbide particles, and the components are as follows in percentage by mass:
the sum of the mass percentages of all the components is 100 percent.
2. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 1 is characterized by comprising the following components in percentage by mass:
the sum of the mass percentages of all the components is 100 percent.
3. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 1, is characterized in that: the silver-plated silicon carbide particles are beta-silicon carbide, the average particle size of the beta-silicon carbide particles is 0.1-5 microns, and the structure of the silver-plated silicon carbide particles is as follows: and coating a silver layer with the thickness of 10-100 nanometers on the surface of the silicon carbide particle to form the composite silicon carbide particle which wraps the silver shell and has a metal-inorganic nonmetal composite structure.
4. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 3, wherein the nano silver paste is characterized in that: the silver layer on the surface of the silver-plated silicon carbide particles is generated on the surface of the silicon carbide particles by an electroless plating, deposition or sputtering method.
5. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 1, is characterized in that: the average grain diameter of the nano silver particles is 5-30 nanometers.
6. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 1, is characterized in that: the triethylene glycol acts as a dispersant and starts to decompose at not less than 100 ℃.
7. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 1, is characterized in that: the polyvinyl butyral is used as an organic vehicle and starts to decompose at a temperature of not less than 300 ℃.
8. The multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 1, is characterized in that: the terpineol acts as a diluent and starts to decompose at a temperature of not less than 60 ℃.
9. The preparation method of the multi-scale nano silver paste mixed by the nano silver particles and the silver-plated silicon carbide particles according to claim 1 is characterized in that raw materials of each component are taken according to a component formula in the multi-scale nano silver paste mixed by the target prepared nano silver particles and the silver-plated silicon carbide particles, and the preparation method comprises the following steps:
a. adding absolute ethyl alcohol into a beaker as a basic solvent, heating, adding polyvinyl butyral into the beaker while stirring, and fully mixing the polyvinyl butyral and the ethyl alcohol to form a carrier solvent for later use;
b. cooling the mixed carrier solvent prepared in the step a, adding triethylene glycol and terpineol into the mixed carrier solvent after cooling to room temperature, and dispersing and diluting the mixed carrier solvent to obtain carrier dispersion liquid;
c. b, stirring the carrier dispersion liquid prepared in the step b at room temperature, adding the nano silver particles and the silver-plated silicon carbide particles into the carrier dispersion liquid while stirring, and controlling the stirring time for at least 15min to obtain mixed slurry of the nano silver particles and the silver-plated silicon carbide particles;
d. and c, post-treating the mixed slurry prepared in the step c, performing ultrasonic homogenization treatment, and when performing ultrasonic treatment on the mixed slurry, adding ice blocks or ice water into the mixed slurry to cool, controlling the temperature of the mixed slurry to be not higher than 28 ℃, and performing ultrasonic treatment for not less than 30min to obtain the multi-scale nano silver slurry mixed by the nano silver particles and the silver-plated silicon carbide particles after the ultrasonic homogenization treatment process is finished.
10. The method for preparing multi-scale nano silver paste mixed by nano silver particles and silver-plated silicon carbide particles according to claim 9, wherein the method comprises the following steps: in the step a, the heating temperature is not lower than 60 ℃ and is lower than the boiling point temperature of the ethanol.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003106573A1 (en) * | 2002-06-13 | 2003-12-24 | Nanopowders Industries Ltd. | A method for the production of conductive and transparent nano-coatings and nano-inks and nano-powder coatings and inks produced thereby |
| CN106995536A (en) * | 2017-04-20 | 2017-08-01 | 深圳先进技术研究院 | Carborundum line silver hybrid particulates, its preparation method and as filler heat-conductive composite material purposes |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101710497B (en) * | 2009-12-08 | 2011-04-20 | 华中科技大学 | Nano-silver conductive slurry |
| CN102691055A (en) * | 2012-05-11 | 2012-09-26 | 上海上大瑞沪微系统集成技术有限公司 | Preparing method of novel silicon carbide nano-particle |
| US9312231B2 (en) * | 2013-10-31 | 2016-04-12 | Freescale Semiconductor, Inc. | Method and apparatus for high temperature semiconductor device packages and structures using a low temperature process |
| CN105176198B (en) * | 2015-07-17 | 2019-03-05 | 中国科学院合肥物质科学研究院 | The preparation method and application method of ink are stablized in storage with high concentration silver nanowires |
| JP7056552B2 (en) * | 2016-03-17 | 2022-04-19 | 東洋紡株式会社 | Conductive coating and conductive paste for laser etching processing |
| CN107833651A (en) * | 2017-10-25 | 2018-03-23 | 哈尔滨工业大学深圳研究生院 | A kind of composite Nano silver paste and Fast Sintering method for packing |
| CN107955413A (en) * | 2017-12-08 | 2018-04-24 | 马鞍山虹润彩印有限责任公司 | A kind of preparation method for applying the conductive filler on electrically conductive ink |
| CN108372313B (en) * | 2018-03-25 | 2021-08-10 | 湖南皓志纳米技术有限公司 | Nano silver wire dispersion liquid with small wire diameter distribution and preparation method of conductive ink thereof |
-
2019
- 2019-01-14 CN CN201910032445.0A patent/CN109887638B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003106573A1 (en) * | 2002-06-13 | 2003-12-24 | Nanopowders Industries Ltd. | A method for the production of conductive and transparent nano-coatings and nano-inks and nano-powder coatings and inks produced thereby |
| CN106995536A (en) * | 2017-04-20 | 2017-08-01 | 深圳先进技术研究院 | Carborundum line silver hybrid particulates, its preparation method and as filler heat-conductive composite material purposes |
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