CN114473103A - Liquid metal tin assisted nano-silver sintering process - Google Patents
Liquid metal tin assisted nano-silver sintering process Download PDFInfo
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- CN114473103A CN114473103A CN202210407223.4A CN202210407223A CN114473103A CN 114473103 A CN114473103 A CN 114473103A CN 202210407223 A CN202210407223 A CN 202210407223A CN 114473103 A CN114473103 A CN 114473103A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/10—Bump connectors ; Manufacturing methods related thereto
- H01L24/11—Manufacturing methods
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/10—Bump connectors ; Manufacturing methods related thereto
- H01L24/12—Structure, shape, material or disposition of the bump connectors prior to the connecting process
- H01L24/13—Structure, shape, material or disposition of the bump connectors prior to the connecting process of an individual bump connector
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
- H01L24/81—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a bump connector
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/36—Electric or electronic devices
- B23K2101/40—Semiconductor devices
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/10—Bump connectors; Manufacturing methods related thereto
- H01L2224/11—Manufacturing methods
- H01L2224/113—Manufacturing methods by local deposition of the material of the bump connector
- H01L2224/1131—Manufacturing methods by local deposition of the material of the bump connector in liquid form
- H01L2224/1132—Screen printing, i.e. using a stencil
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
- H01L2224/81—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a bump connector
- H01L2224/812—Applying energy for connecting
- H01L2224/81201—Compression bonding
- H01L2224/81203—Thermocompression bonding, e.g. diffusion bonding, pressure joining, thermocompression welding or solid-state welding
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/01—Chemical elements
- H01L2924/01047—Silver [Ag]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/01—Chemical elements
- H01L2924/0105—Tin [Sn]
Abstract
The invention discloses a liquid metal tin-assisted nano silver sintering process, which specifically comprises the following operation steps: s1: preparation of nano silver particles, S2: preparation of nano-silver solder paste, S3: preparation of nano tin-nano silver composite solder paste, S4: the organic carrier is dissolved in the organic solvent, the metal tin particles are added in the nano silver paste in a non-agglomerated dispersed manner, and the nano silver paste is sintered by the aid of the metal tin to assist the nano silver, so that the thermal, electrical and mechanical property reliability of the silver sintering paste can be effectively improved, the silver sintering paste can be applied to a high-temperature environment, the shrinkage of tissues during secondary sintering of a sintered body is effectively reduced, the connection strength is improved, the heat conductivity is improved, and the service life is prolonged.
Description
Technical Field
The invention belongs to the technical field of solder sintering, and particularly relates to a liquid metal tin-assisted nano silver sintering process.
Background
With the continuous development of power electronic technology, the demand of high-power devices is increasing day by day. The third generation semiconductor materials represented by SiC and GaN have the properties of wide forbidden band, high breakdown voltage, high thermal conductivity and the like, can work at the temperature higher than 500 ℃, and are widely applied to electronic packaging. Therefore, high temperature resistant interconnect materials are urgently needed to meet the use of the third generation of semiconductors.
The nano silver paste has the advantages of low sintering temperature, high electric conductivity, high thermal conductivity, high bonding strength, stable performance and the like, is widely used for completing low-temperature and low-pressure sintering packaging of high-temperature electronic devices, and occupies an extremely important position in the field of microelectronics.
However, the nano silver is expensive, the sintering time is long, the porosity of the obtained sintered body is high, and meanwhile, the nano silver sintered structure can be subjected to secondary sintering under high-temperature service and thermal cycle states, so that the sintered structure is shrunk, the internal stress is increased continuously, different regions in the sintered structure are locally shrunk, cracks are generated among the shrunk structures, the cracks are gradually enlarged, the mechanical performance of the sintered joint is reduced, and even the sintered joint is failed. The silver nanoparticles serving as a thermal interface material for chip packaging should have excellent high-temperature service reliability. In order to reduce the cost of materials and production process and improve the packaging reliability, the component structure and sintering process of the nano silver paste need to be optimized.
Disclosure of Invention
The invention aims to provide a liquid metal tin-assisted nano silver sintering process to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a liquid metal tin assisted nano silver sintering process specifically comprises the following operation steps:
s1: preparing nano silver particles by using a silver nitrate solution, a sodium borohydride solution and polyvinylpyrrolidone, and calculating the silver nitrate solution and the sodium borohydride solution according to the mass fraction ratio: 1:3.2-4.3, preparing nano silver particles, adding polyvinylpyrrolidone into the mixture for dispersion, filtering out powder after reacting for 5-10 minutes, drying, ionizing by using current with voltage of 300-350V to prepare silver ions, adding the silver ions into 5-6mol/L salt solution, neutralizing the silver ions, filtering and drying again for later use;
s2: preparing nano silver soldering paste, namely mixing the prepared nano silver particles with an organic solvent to prepare the nano silver soldering paste;
s3: preparing nano tin-nano silver composite soldering paste, wherein the mass ratio of nano tin to the total mass of the nano tin-nano silver composite soldering paste is 0.5-2.5%, adding the metal tin into the prepared nano silver slurry, adding an organic solvent, and stirring to obtain a liquid mixture;
s4: and dissolving the organic carrier in an organic solvent, mixing the organic carrier with the solution obtained in the step S3, fully stirring, and performing ultrasonic dispersion to obtain the nano tin-nano silver composite soldering paste.
S5: coating the composite soldering paste on a substrate by adopting a screen printing method;
s6: attaching the chip to the coating composite soldering paste;
s7: and controlling the pressure and the temperature to sinter the substrate, and cooling to obtain the sintered connecting device.
Preferably, the nano silver particles prepared in step S1 have a grain size ranging from 40 to 80 nm.
Preferably, the organic solvent in steps S2 and S3 is ethanol, ethylene glycol, or propylene glycol.
Preferably, the organic vehicle in step S4 is ethyl cellulose, polyvinyl alcohol, terpineol, etc., and the mass percentage of the organic vehicle is 1-5%.
Preferably, the mass percentage of the organic solvent in the step S4 is 10-20%, and the balance is nano silver and nano tin.
Preferably, the sintering pressure in the step S7 is 8-10MPa, the sintering temperature is 195-220 ℃, and the sintering time is 25-30 min.
The invention has the technical effects and advantages that:
according to the invention, the metal tin particles are added in the nano silver paste in a non-agglomerated dispersed manner, and the nano silver sintering is assisted by the metal tin, so that the thermal property, the electrical property and the mechanical property reliability of the silver sintering paste can be effectively improved, the silver sintering paste can be applied to a high-temperature environment, the shrinkage of the structure of a sintered body during secondary sintering can be effectively reduced, the connection strength can be improved, the heat conductivity can be improved, and the service life can be prolonged.
Drawings
FIG. 1 is an SEM image of a sintering structure of nano-silver solder paste without nano-tin;
FIG. 2 is an SEM image of the sintering structure of the composite solder paste after nano silver is added.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A liquid metal tin assisted nano silver sintering process specifically comprises the following operation steps:
s1: preparing nano silver particles by using a silver nitrate solution, a sodium borohydride solution and polyvinylpyrrolidone, and calculating the silver nitrate solution and the sodium borohydride solution according to the mass fraction ratio: mixing according to the proportion of 1:4.3 to prepare nano silver particles, adding polyvinylpyrrolidone into the nano silver particles for dispersion, filtering out powder after reacting for 10 minutes, drying, ionizing by using current with 350V voltage to prepare silver ions, adding the silver ions into 6mol/L salt solution, neutralizing the silver ions, filtering and drying again for later use, wherein the grain range of the nano silver particles is 80 nm;
s2: preparing nano silver soldering paste, namely mixing the prepared nano silver particles with an organic solvent to prepare the nano silver soldering paste, wherein the organic solvent is any combination of ethanol, ethylene glycol and propylene glycol;
s3: preparing nano-tin and nano-silver composite soldering paste, wherein the mass ratio of nano-tin to the total mass of the nano-tin and nano-silver composite soldering paste is 2.5%, adding metallic tin into the prepared nano-silver slurry, adding an organic solvent, and stirring to obtain a liquid mixture;
s4: and dissolving an organic carrier into an organic solvent, mixing the organic carrier with the solution obtained in the step S3, fully stirring, and performing ultrasonic dispersion to obtain the nano-tin nano-silver composite soldering paste, wherein the organic carrier is ethyl cellulose, polyvinyl alcohol, terpineol and the like, the mass percent of the organic carrier is 5%, the mass percent of the organic solvent is 20%, and the balance is nano-silver and nano-tin.
S5: coating the composite soldering paste on a substrate by adopting a screen printing method;
s6: attaching the chip to the coating composite soldering paste;
s7: and sintering the substrate under the controlled pressure and temperature, and cooling to obtain the sintered connecting device, wherein the sintering pressure is 10MPa, the sintering temperature is 220 ℃, and the sintering time is 30 min.
Example 2
A liquid metal tin assisted nano silver sintering process specifically comprises the following operation steps:
s1: preparing nano silver particles by using a silver nitrate solution, a sodium borohydride solution and polyvinylpyrrolidone, and calculating the silver nitrate solution and the sodium borohydride solution according to the mass fraction ratio: mixing according to the proportion of 1:3.2 to prepare nano silver particles, adding polyvinylpyrrolidone into the nano silver particles for dispersion, filtering out powder after reacting for 5 minutes, drying, ionizing by using current with 300 voltage to prepare silver ions, adding the silver ions into 5mol/L salt solution, neutralizing the silver ions, filtering and drying again for later use, wherein the grain range of the nano silver particles is 40 nm;
s2: preparing nano silver soldering paste, namely mixing the prepared nano silver particles with an organic solvent to prepare the nano silver soldering paste, wherein the organic solvent is any combination of ethanol, ethylene glycol and propylene glycol;
s3: preparing nano-tin and nano-silver composite soldering paste, wherein the mass ratio of nano-tin to the total mass of the nano-tin and nano-silver composite soldering paste is 0.5%, adding metallic tin into the prepared nano-silver slurry, adding an organic solvent, and stirring to obtain a liquid mixture;
s4: and dissolving an organic carrier into an organic solvent, mixing the organic carrier with the solution obtained in the step S3, fully stirring, and performing ultrasonic dispersion to obtain the nano-tin nano-silver composite soldering paste, wherein the organic carrier is ethyl cellulose, polyvinyl alcohol, terpineol and the like, the mass percent of the organic carrier is 1%, the mass percent of the organic solvent is 10%, and the balance is nano-silver and nano-tin.
S5: coating the composite soldering paste on a substrate by adopting a screen printing method;
s6: attaching the chip to the coating composite soldering paste;
s7: and sintering the substrate under controlled pressure and temperature, and cooling to obtain the sintered connecting device, wherein the sintering pressure is 8MPa, the sintering temperature is 195 ℃, and the sintering time is 25 min.
Example 3
A liquid metal tin assisted nano silver sintering process specifically comprises the following operation steps:
s1: preparing nano silver particles by using a silver nitrate solution, a sodium borohydride solution and polyvinylpyrrolidone, and calculating the silver nitrate solution and the sodium borohydride solution according to the mass fraction ratio: mixing according to the proportion of 1:3.8 to prepare nano silver particles, adding polyvinylpyrrolidone into the mixture for dispersing, filtering powder in the mixture after reacting for 7 minutes, drying the powder, ionizing the powder by using a current with a voltage of 336V to prepare silver ions, adding the silver ions into a 5.5mol/L salt solution, neutralizing the silver ions, and filtering and drying the silver ions again for later use, wherein the grain range of the nano silver particles is 66 nm;
s2: preparing nano silver soldering paste, namely mixing the prepared nano silver particles with an organic solvent to prepare the nano silver soldering paste, wherein the organic solvent is any combination of ethanol, ethylene glycol and propylene glycol;
s3: preparing nano-tin and nano-silver composite soldering paste, wherein the mass ratio of nano-tin to the total mass of the nano-tin and nano-silver composite soldering paste is 1.8%, adding metallic tin into the prepared nano-silver slurry, adding an organic solvent, and stirring to obtain a liquid mixture;
s4: and dissolving an organic carrier into an organic solvent, mixing the organic carrier with the solution obtained in the step S3, fully stirring, and performing ultrasonic dispersion to obtain the nano-tin nano-silver composite soldering paste, wherein the organic carrier is ethyl cellulose, polyvinyl alcohol, terpineol and the like, the mass percent of the organic carrier is 3%, the mass percent of the organic solvent is 17%, and the balance is nano-silver and nano-tin.
S5: coating the composite soldering paste on a substrate by adopting a screen printing method;
s6: attaching the chip to the coating composite soldering paste;
s7: and sintering the substrate under the controlled pressure and temperature, and cooling to obtain the sintered connecting device, wherein the sintering pressure is 9MPa, the sintering temperature is 215 ℃, and the sintering time is 27 min.
According to the invention, the metal tin particles are added in the nano silver paste in a non-agglomerated dispersed manner, and the nano silver sintering is assisted by the metal tin, so that the thermal property, the electrical property and the mechanical property reliability of the silver sintering paste can be effectively improved, the silver sintering paste can be applied to a high-temperature environment, the shrinkage of the structure of a sintered body during secondary sintering can be effectively reduced, the connection strength can be improved, the heat conductivity can be improved, and the service life can be prolonged.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (6)
1. A liquid metal tin auxiliary nano silver sintering process is characterized in that: the method specifically comprises the following operation steps:
s1: preparing nano silver particles by using a silver nitrate solution, a sodium borohydride solution and polyvinylpyrrolidone, and calculating the silver nitrate solution and the sodium borohydride solution according to the mass fraction ratio: 1:3.2-4.3, preparing nano silver particles, adding polyvinylpyrrolidone into the mixture for dispersion, filtering out powder after reacting for 5-10 minutes, drying, ionizing by using current with voltage of 300-350V to prepare silver ions, adding the silver ions into 5-6mol/L salt solution, neutralizing the silver ions, filtering and drying again for later use;
s2: preparing nano silver soldering paste, namely mixing the prepared nano silver particles with an organic solvent to prepare the nano silver soldering paste;
s3: preparing nano tin-nano silver composite soldering paste, wherein the mass ratio of nano tin to the total mass of the nano tin-nano silver composite soldering paste is 0.5-2.5%, adding the metal tin into the prepared nano silver slurry, adding an organic solvent, and stirring to obtain a liquid mixture;
s4: dissolving an organic carrier into an organic solvent, mixing the organic carrier with the solution obtained in the step S3, fully stirring, and performing ultrasonic dispersion to obtain the nano tin nano silver composite soldering paste;
s5: coating the composite soldering paste on a substrate by adopting a screen printing method;
s6: attaching the chip to the coating composite soldering paste;
s7: and controlling the pressure and the temperature to sinter the substrate, and cooling to obtain the sintered connecting device.
2. The liquid metallic tin-assisted nano-silver sintering process of claim 1, wherein: the grain range of the nano silver particles prepared in the step S1 is 40-80 nm.
3. The liquid metallic tin-assisted nano-silver sintering process of claim 1, wherein: the organic solvent in the steps S2 and S3 is any combination of ethanol, ethylene glycol and propylene glycol.
4. The liquid metallic tin-assisted nano-silver sintering process of claim 1, wherein: in the step S4, the organic carrier is ethyl cellulose, polyvinyl alcohol, terpineol and the like, and the mass percentage of the organic carrier is 1-5%.
5. The liquid metallic tin-assisted nano-silver sintering process of claim 1, wherein: in the step S4, the mass percent of the organic solvent is 10-20%, and the balance is nano silver and nano tin.
6. The liquid metallic tin-assisted nano-silver sintering process of claim 1, wherein: in step S7, the sintering pressure is 8-10MPa, the sintering temperature is 195-220 ℃, and the sintering time is 25-30 min.
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CN113206018A (en) * | 2021-04-23 | 2021-08-03 | 天津工业大学 | Low-temperature large-area uniform sintering method for nano-silver soldering paste |
CN113284645A (en) * | 2021-04-25 | 2021-08-20 | 广州汉源新材料股份有限公司 | Nano silver paste and preparation method thereof |
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CN115026458A (en) * | 2022-06-17 | 2022-09-09 | 温州宏丰电工合金股份有限公司 | Ag-based alloy powder slurry, Ag-based alloy active solder and preparation method thereof |
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