CN111995963A - Single-component silver-based conductive adhesive and preparation method thereof - Google Patents

Single-component silver-based conductive adhesive and preparation method thereof Download PDF

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CN111995963A
CN111995963A CN202010913558.4A CN202010913558A CN111995963A CN 111995963 A CN111995963 A CN 111995963A CN 202010913558 A CN202010913558 A CN 202010913558A CN 111995963 A CN111995963 A CN 111995963A
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silver
conductive adhesive
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component silver
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陈华
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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
    • 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
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • 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
    • 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
    • C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
    • C09J171/02—Polyalkylene oxides
    • 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
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • 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
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/04—Antistatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The invention relates to a single-component silver-based conductive adhesive which is composed of 25-66% of silver nano conductive particles, 8-10% of a dispersing agent, 10-15% of a coagulant, 3-5% of a curing agent, 20-35% of a plasticizer, 1-20% of a prepolymer and 1-2% of lead-cesium bromide quantum dots, wherein the percentage is mass percentage, the shear strength and the conductivity of the single-component silver-based conductive adhesive are effectively improved, and the single-component silver-based conductive adhesive is simple in preparation method, simple in operation, low in cost, strong in repeatability and high in market commercialization potential.

Description

Single-component silver-based conductive adhesive and preparation method thereof
Technical Field
The invention belongs to the field of conductive adhesives, and particularly relates to a single-component silver-based conductive adhesive, in particular to a preparation method of the single-component silver-based conductive adhesive.
Background
With the development of electronic products in the direction of miniaturization and high integration, the requirements of the packaging technology of electronic components and the manufacturing technology of printed circuit boards on interconnection materials are more severe, and the traditional materials cannot meet the requirements of environment and technology.
The electronic conductive adhesive is an adhesive with certain conductive performance after being cured or dried, and becomes an ideal substitute of the traditional Sn/Pb solder as a new electronic material and has higher competitiveness. In the electronic packaging technology, the conductive adhesive has the advantages of environmental friendliness, low operation temperature and high resolution ratio instead of Sn/Pb solder; printed circuit board manufacturing technologyIn the process, the conductive rubber plug hole replaces the traditional electroplating technology, has the advantages of environmental friendliness and simple process flow, can even realize the interconnection conductive bonding of any layer, is used as a new special process and is increasingly widely applied, and the conductive adhesive becomes an indispensable new material in the electronic industry. The conductive adhesive has many advantages, such as being capable of being cured at lower temperature even room temperature, and avoiding material deformation and component damage caused by high temperature during welding; the stress concentration of riveting and the loss, leakage and the like of electromagnetic signals can be avoided. The volume resistivity of the conductive colloid used in some high-end fields in the domestic market is generally 10-2～10-4Omega cm, the conductive adhesive of partial high-temperature curing can reach 10-5 omega cm, but the application range is limited, because the heating can cause the problems of deformation, thermal aging and the like of electronic components, and the performance of the electronic components is influenced.
The silver has excellent conductivity and heat conductivity, and the conductivity can reach 6.3 multiplied by 107S/m, and the thermal conductivity reaches 429W/(m.K). Silver is not easy to be oxidized in air, and the oxidized product still has conductivity; at the same time, silver is less expensive than gold or platinum, and therefore silver is one of the most common and desirable conductive fillers. The conductive adhesive taking silver powder as conductive filler in China has various types. Patent application CN109243669A discloses a solar front silver paste with good thixotropy prepared by utilizing glass alkalinity and a preparation method thereof, wherein the solar front silver paste is composed of a conductive phase, inorganic phase alkaline glass powder and an organic phase; patent application CN109448886A discloses a preparation method of conductive silver paste, which comprises diluting, curing agent and binder. The ratio of the spherical silver powder to the flake silver powder is 1: 1, but the adhesion is to be improved.
Disclosure of Invention
The invention provides a single-component silver-based conductive adhesive with high cohesiveness, high tensile strength and low resistivity and a preparation method thereof, aiming at the problems of low cohesiveness, low tensile strength and high resistivity of the existing single-component conductive substrate.
The technical scheme of the invention is as follows:
the single-component silver-based conductive adhesive is characterized by comprising 25-66% of silver nano conductive particles, 8-10% of a dispersing agent, 10-15% of a coagulant, 3-5% of a curing agent, 20-35% of a plasticizer, 1-20% of a prepolymer and 1-2% of lead cesium bromide quantum dots, wherein the mass percentage of the single-component silver-based conductive adhesive is mass percentage.
Preferably, the coagulant is composed of more than two of coconut oil acid glycol amide, methylene diacrylamide, -caprolactam alkyl, alcohol amide, lauramidopropyl betaine and polyacrylamide in any proportion, the acylation effect of the coagulant is remarkable, the conductive channel of the coagulant is increased, excessive energy loss in the process of electron transmission is reduced, particularly, the composite amide agent taking alcohol amide as a main body has the most remarkable effect, has very low surface energy and reduces the sheet resistance value;
preferably, the raw material for synthesizing the lead cesium bromide quantum dots is 8-13% of GeO25 to 13% of B2O312-18% of PbO and 8-15% of Cs2CO310-22% of PbBr2And 31-57% of NaBr, wherein the percentage is mass percentage; and performing secondary high-temperature treatment on the raw materials to obtain the lead cesium bromide quantum dots, wherein the first treatment temperature is 600-800 ℃, and the second treatment temperature is 100-350 ℃.
Preferably, the prepolymer is composed of more than two of urea-formaldehyde resin, fluorine-containing resin, organic silicon resin, hydroxypropyl cellulose methyl ether alkoxy pyrrolidone, polyvinyl pyrrolinone, acetone, silicone and silicone alcohol in any proportion, the dispersing agent is composed of more than two of ethanol, propylene glycol, isopropanol, glycerol, methanol, propanol, D-sorbitol, dimethyl methanol and butanediol in any proportion, the dielectric constant of the prepolymer is greatly reduced due to the existence of silicon base, the oxidation resistance of the prepolymer is greatly enhanced, the dispersing agent is composed of more than two of ethanol, propylene glycol, isopropanol, glycerol, methanol, propanol, D-sorbitol, dimethyl methanol and butanediol in any proportion, the dispersibility of the prepolymer can be enhanced by an alcohol organic solvent, the low-temperature resistant effect can be achieved, and the dispersing agent of a main organic matter in the alcohol is added, the silver-based conductive silver adhesive has good conductivity at low temperature.
Preferably, the curing agent is a multifunctional group branched chain formed by more than two of fatty alcohol-polyoxyethylene ether sulfate, fatty alcohol-polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester and fatty alcohol-ethylene oxide condensation compound in any proportion, so that the multifunctional group branched chain has good ductility, and the adhesive property of the conductive silver adhesive can be remarkably enhanced.
Preferably, the plasticizer is composed of more than two of polyoxyethylene alkyl phenyl ether, dodecyl phenol polyoxyethylene ether, alkyl polyoxyethylene sodium sulfate, polyethylene glycol phenyl ether, octyl phenol polyoxyethylene ether and polypropoxy butyl ether sulfuric acid in any proportion.
The preparation method comprises the following steps:
1) dispersing silver particles in ethanol, performing ultrasonic treatment for 1-2 hours, and then washing and drying at the drying temperature of 60-80 ℃; then taking a grinding vessel to grind for 1-3 h;
2) calcining the product obtained in the step 1) at high temperature in an inert environment, wherein the calcining temperature is 100-300 ℃ and the time is 10-12 hours, and crushing to obtain silver nano conductive particles for later use;
3) dispersing 1-20% of prepolymer, 3-5% of curing agent, 20-35% of plasticizer, 10-15% of coagulant and 1-2% of lead cesium bromide quantum dots in 8-10% of dispersant by mass percent, and ultrasonically stirring for 5-10 minutes to obtain a prepolymer product;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percentage of 25-66%, and grinding for 1-30 minutes;
5) and (3) coating the product obtained in the step (4), and storing in a sealed and air-isolated manner to obtain the single-component silver conductive adhesive, wherein the drying temperature is 30-45 ℃.
Preferably, the particle size of the silver nano conductive particles is 10-50 nm.
Preferably, the lead cesium bromide quantum dots are prepared by using GeO2、B2O3、PbO、Cs2CO3、PbBr2And NaBr, mixing uniformly, melting at 600-800 ℃, stirring while cooling to room temperature, annealing and calcining at 100-300 ℃ for 2-4h, and grinding to obtain the lead-cesium bromide quantum dots.
Preferably, in the step 4), the dispersant is subjected to ultrasonic treatment for 10-30 minutes in advance.
Compared with other products, the invention has the following advantages:
the prepolymer, the plasticizer, the curing agent and the curing agent can form a silane coupling effect to enhance the bonding strength of the prepolymer;
the organic silicon resin in the prepolymer can form a layer of silicon-silver oxide film on the surface of the conductive colloid, so that the conductivity of the conductive colloid is enhanced, the heat conduction is accelerated, and the service life of the conductive colloid is prolonged;
the calcined silver nanoparticles have better dispersibility, can be uniformly dispersed in a sol phase primarily synthesized by the calcined silver nanoparticles, and the uniformity of a dried product is greatly improved;
the particle size of the silver nanoparticles after calcination and grinding is more uniform, the resistivity of the silver nanoparticles is effectively reduced, and the conductivity of the silver nanoparticles is effectively improved;
the drying temperature is controlled within the range of 30-45 ℃, and the low-temperature slow drying is adopted, so that the flexibility and the bonding degree of the product are effectively improved.
Drawings
FIG. 1 is a comparative scanning electron microscope image of the single-component silver-based conductive adhesive and the common conductive adhesive disclosed by the invention;
FIG. 2 is a graph showing the comparison of the bonding strength between a single-component silver-based conductive adhesive and a common conductive adhesive;
fig. 3 is a graph showing the comparison of the conductivity of the single-component silver-based conductive adhesive and the conductivity of the common conductive adhesive.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are described in detail as follows:
example 1
The preparation method of the single-component silver-based conductive adhesive comprises the following steps:
1) dispersing 20mg of silver nanoparticles in ethanol, performing ultrasonic treatment for 1h, and then washing and drying at the drying temperature of 60 ℃; then taking a grinding dish to grind for 3 hours;
2) calcining the product obtained in the step 1) at high temperature in an inert environment, wherein the calcining temperature is 200 ℃ for 12 hours, and crushing to obtain silver nano conductive particles for later use;
3) dispersing 0% of lead cesium bromide quantum dots, 5% of fatty alcohol-polyoxyethylene ether, 35% of octyl phenol-polyoxyethylene ether and 15% of dimethyl methanol in a dispersing agent according to mass percentage, and ultrasonically stirring for 10 minutes to obtain a prepolymer product;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percent of 25, and grinding for 30 minutes;
5) and (4) coating the product obtained in the step (4), and preserving in a sealed and air-isolated manner to obtain the single-component silver conductive adhesive.
And (4) taking the conductive silver adhesive to perform four-probe resistance test, and counting the conductivity of the conductive silver adhesive.
The prepared conductive silver adhesive is tested by a scanning electron microscope, as shown in fig. 1(a) common conductive silver adhesive and (b) the conductive silver adhesive prepared in the patent, the smoothness of (b) is greatly improved, and the conductive silver adhesive has better ductility and composite performance.
Example 2
The preparation method of the single-component silver-based conductive adhesive comprises the following steps:
1) dispersing 20mg of silver nanoparticles in a dispersing agent, carrying out ultrasonic treatment for 1h, and then washing and drying at the drying temperature of 80 ℃; then taking a grinding dish to grind for 3 hours;
2) calcining the product obtained in the step 1) at high temperature for 10 hours at 100 ℃;
3) taking the following components in percentage by mass: 1% of urea-formaldehyde resin, 3% of polyoxyethylene sorbitan fatty acid, 35% of octyl phenol polyoxyethylene ether and 15% of dimethyl methanol are dispersed in a dispersing agent, and ultrasonic stirring is carried out for 10 minutes;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percent of 25, and grinding for 30 minutes;
5) and (4) coating the product obtained in the step (4), and preserving in a sealed and air-isolated manner to obtain the final product, namely the single-component silver conductive silver adhesive.
Uniformly coating the product obtained in the step 5) on one end of a LY12CZ aluminum alloy test piece joint which is polished and lapped by No. 1 abrasive cloth and cleaned by acetone, gluing, and feeding into an electrothermal blowing drying oven at the temperature of (25 +/-3) DEG C for curing. And (5) carrying out a tensile test of a tensile machine, wherein the test temperature is 175 ℃, and the shearing force is 9.3 MPa.
And (3) uniformly coating the product obtained in the step 6) on the surface of a glass slide, and performing four-probe resistance test to obtain the resistivity of 9.4 & 10-5 omega & cm.
Example 3
The preparation method of the single-component silver-based conductive adhesive comprises the following steps:
1) dispersing 50mg of silver nanoparticles in a dispersing agent, carrying out ultrasonic treatment for 2 hours, and then washing and drying, wherein the drying temperature is 60 ℃; then taking a grinding dish to grind for 3 hours;
2) calcining the product obtained in the step 1) at high temperature in an inert environment, wherein the calcining temperature is 100 ℃ for 12 hours, and crushing to obtain silver nano conductive particles for later use;
3) taking the following components in percentage by mass: dispersing 15% of lead cesium bromide quantum dots, 4% of fatty alcohol-polyoxyethylene ether, 25% of polypropoxy butyl ether sulfuric acid and 15% of dimethyl methanol in a dispersing agent, and ultrasonically stirring for 10 minutes;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percent of 25, and grinding for 30 minutes;
5) and (3) coating the product obtained in the step (4), and storing in a sealed and air-isolated manner to obtain the final product, namely the single-component silver conductive silver adhesive, wherein the drying temperature is 45 ℃.
6) Uniformly coating the product obtained in the step 4) on one end of a LY12CZ aluminum alloy test piece joint which is polished and lapped by No. 1 abrasive cloth and cleaned by acetone, gluing, and feeding into an electrothermal blowing drying oven at the temperature of (25 +/-3) DEG C for curing. And (3) carrying out a tensile test of a tensile machine, wherein the test temperature is 175 ℃, and the shearing force is 13.5 MPa.
7) And (3) uniformly coating the product obtained in the step (4) on the surface of a glass slide, and carrying out four-probe resistance test to obtain the resistivity of 8.9 & 10-5 omega & cm.
Example 4
The preparation method of the single-component silver-based conductive adhesive comprises the following steps:
1) dispersing 100mg of silver nanoparticles in a dispersing agent, carrying out ultrasonic treatment for 1h, and then washing and drying, wherein the drying temperature is 60 ℃; then taking the grinding vessel for 2 hours;
2) calcining the product obtained in the step 1) at high temperature in an inert environment, wherein the calcining temperature is 100 ℃ for 12 hours, and crushing to obtain silver nano conductive particles for later use;
3) taking the following components in percentage by mass: dispersing 10% of lead-cesium bromide quantum dots, 5% of fatty alcohol-polyoxyethylene ether, 35% of octylphenol-polyoxyethylene ether and 15% of isopropyl glycol in a dispersing agent, and ultrasonically stirring for 10 minutes;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percent of 25, and grinding for 30 minutes;
5) uniformly coating the product obtained in the step 4) on one end of a LY12CZ aluminum alloy test piece joint which is polished and lapped by No. 1 abrasive cloth and cleaned by acetone, gluing, and feeding into an electrothermal blowing drying oven at the temperature of (25 +/-3) DEG C for curing. And (3) carrying out a tensile test of a tensile machine, wherein the test temperature is 175 ℃, and the shearing force is 16.9 MPa.
6) Uniformly coating the product obtained in the step 4) on the surface of a glass slide, and carrying out four-probe resistance test to obtain the resistivity of the glass slide of 6.5-10-5Ω·cm。
Example 5:
the preparation method of the single-component silver-based conductive adhesive comprises the following steps:
1) dispersing 100mg of silver nanoparticles in a dispersing agent, carrying out ultrasonic treatment for 2 hours, and then washing and drying, wherein the drying temperature is 80 ℃; then taking a grinding dish to grind for 3 hours;
2) calcining the product obtained in the step 1) at high temperature in an inert environment, wherein the calcining temperature is 100 ℃ for 12 hours, and crushing to obtain silver nano conductive particles for later use;
3) taking the following components in percentage by mass: dispersing 20% of pre-fluorine-containing resin, 35% of fatty alcohol ethylene oxide, 15% of fatty alcohol ethylene oxide and 15% of propylene alcohol in a dispersing agent, and ultrasonically stirring for 10 minutes;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percent of 25, and grinding for 30 minutes;
5) coating the product obtained in the step 4), and preserving in a sealed and air-isolated manner to obtain the final product, namely the single-component silver conductive silver adhesive; uniformly coating the product obtained in the step 4) on one end of a LY12CZ aluminum alloy test piece joint which is polished and lapped by No. 1 abrasive cloth and cleaned by acetone, gluing, and feeding into an electrothermal blowing drying oven at the temperature of (25 +/-3) DEG C for curing. Performing tensile test of a tensile machine at the test temperature of 175 ℃ to obtain the shearing force of 11.8 MPa;
and (3) uniformly coating the product obtained in the step (4) on the surface of a glass slide, and carrying out four-probe resistance test to obtain the resistivity of 10.2 & 10 & lt-5 & gt omega & cm.
Example 6:
the preparation method of the single-component silver-based conductive adhesive comprises the following steps:
1) dispersing a certain amount of 100mg of silver nanoparticles in a dispersing agent, carrying out ultrasonic treatment for 2 hours, and then washing and drying at the drying temperature of 80 ℃; then taking a grinding dish to grind for 3 hours;
2) calcining the product obtained in the step 1) at high temperature in an inert environment, wherein the calcining temperature is 150 ℃ for 12 hours, and crushing to obtain silver nano conductive particles for later use;
3) taking the following components in percentage by mass: dispersing 20% of lead-cesium bromide quantum dots, 5% of fatty alcohol ethylene oxide, 35% of fatty alcohol ethylene oxide and 15% of propylene alcohol in a dispersing agent, and ultrasonically stirring for 10 minutes;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percent of 25, and grinding for 30 minutes;
5) coating the product obtained in the step 4), and storing in a closed and air-isolated manner to obtain the final product, namely the single-component silver conductive silver adhesive, wherein the drying temperature is 45 ℃;
uniformly coating the product obtained in the step 4) on one end of a LY12CZ aluminum alloy test piece joint which is polished and lapped by No. 1 abrasive cloth and cleaned by acetone, gluing, and feeding into an electrothermal blowing drying oven at the temperature of (25 +/-3) DEG C for curing. And (3) carrying out a tensile test of a tensile machine, wherein the test temperature is 175 ℃, and the shearing force is 11.7 MPa.
And (3) uniformly coating the product obtained in the step (4) on the surface of a glass slide, and carrying out four-probe resistance test to obtain the resistivity of 7.3 & 10-5 omega & cm.
The bonding strength and the bonding strength of the prepared conductive silver adhesive are compared with those of the common silver adhesive, the fact that the conductivity and the bonding strength of the conductive silver adhesive added with the lead cesium bromide quantum dots are obviously improved can be found, the silver nanoparticles are calcined, the particle roughness of the conductive silver adhesive can be well improved by adding the lead cesium bromide quantum dot prepolymer, the conductivity of the conductive silver adhesive is increased, and the conductive silver adhesive has potential research and development values.
The foregoing detailed description is exemplary only, and is not intended to limit the scope of the patent, as defined by the appended claims; any equivalent alterations or modifications made according to this patent are intended to fall within the scope of this patent.

Claims (10)

1. The single-component silver-based conductive adhesive is characterized by comprising 25-66% of silver nano conductive particles, 8-10% of a dispersing agent, 10-15% of a coagulant, 3-5% of a curing agent, 20-35% of a plasticizer, 1-20% of a prepolymer and 1-2% of lead cesium bromide quantum dots, wherein the mass percentage of the single-component silver-based conductive adhesive is mass percentage.
2. The single-component silver-based conductive adhesive according to claim 1, wherein the coagulant is composed of more than two of cocamidoglycol, methylene bisacrylamide, -caprolactam, alkanolamide, lauramidopropyl betaine and polyacrylamide in any proportion.
3. The single-component silver-based conductive adhesive as claimed in claim 1, wherein the raw material for synthesizing the lead-cesium bromide quantum dots is 8-13% of GeO25 to 13% of B2O312-18% of PbO and 8-15% of Cs2CO310-22% of PbBr2And 31-57% of NaBr, wherein the percentage is mass percentage; and performing secondary high-temperature treatment on the raw materials to obtain the lead cesium bromide quantum dots, wherein the first treatment temperature is 600-800 ℃, and the second treatment temperature is 100-350 ℃.
4. The single-component silver-based conductive adhesive as claimed in claim 1, wherein the prepolymer is composed of two or more of urea-formaldehyde resin, fluorine-containing resin, silicone resin, hydroxypropyl cellulose methyl ether alkoxy pyrrolidone, polyvinyl pyrrolinone, acetone, silicone and silicone alcohol in any proportion, and the dispersant is composed of two or more of ethanol, propylene glycol, isopropanol, glycerol, methanol, propanol, D-sorbitol, dimethyl methanol and butanediol in any proportion.
5. The single-component silver-based conductive adhesive according to claim 1, characterized in that: the curing agent is composed of more than two of fatty alcohol-polyoxyethylene ether sulfate, fatty alcohol-polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester and fatty alcohol-ethylene oxide condensation compound in any proportion.
6. The single-component silver-based conductive adhesive according to claim 1, wherein the plasticizer is composed of two or more of polyoxyethylene alkyl phenyl ether, dodecylphenol polyoxyethylene ether, alkyl polyoxyethylene sodium sulfate, polyethylene glycol phenyl ether, octylphenol polyoxyethylene ether, and polypropoxy butyl ether sulfuric acid at any ratio.
7. The preparation method of the single-component silver-based conductive adhesive as claimed in claim 1, wherein the preparation method comprises the following steps:
1) dispersing silver particles in ethanol, performing ultrasonic treatment for 1-2 hours, and then washing and drying at the drying temperature of 60-80 ℃; then taking a grinding vessel to grind for 1-3 h;
2) calcining the product obtained in the step 1) at high temperature in an inert environment, wherein the calcining temperature is 100-300 ℃ and the time is 10-12 hours, and crushing to obtain silver nano conductive particles for later use;
3) dispersing 1-20% of prepolymer, 3-5% of curing agent, 20-35% of plasticizer, 10-15% of coagulant and 1-2% of lead cesium bromide quantum dots in 8-10% of dispersant by mass percent, and ultrasonically stirring for 5-10 minutes to obtain a prepolymer product;
4) adding the silver nano conductive particles obtained in the step 2) into the prepolymer obtained in the step 3) according to the mass percentage of 25-66%, and grinding for 1-30 minutes;
5) and (3) coating the product obtained in the step (4), and storing in a sealed and air-isolated manner to obtain the single-component silver conductive adhesive, wherein the drying temperature is 30-45 ℃.
8. The method for preparing the single-component silver-based conductive adhesive as claimed in claim 7, wherein the particle size of the silver nano conductive particles is 10-50 nm.
9. The method for preparing the single-component silver-based conductive adhesive as claimed in claim 7, wherein the lead-cesium bromide quantum dots are prepared by using GeO2、B2O3、PbO、Cs2CO3、PbBr2And NaBr, mixing uniformly, melting at 600-800 ℃, stirring while cooling to room temperature, annealing and calcining at 100-300 ℃ for 2-4h, and grinding to obtain the lead-cesium bromide quantum dots.
10. The method for preparing the single-component silver-based conductive adhesive according to claim 7, wherein the method comprises the following steps: in the step 4), the dispersant is subjected to ultrasonic treatment for 10-30 minutes in advance.
CN202010913558.4A 2020-09-03 2020-09-03 Single-component silver-based conductive adhesive and preparation method thereof Pending CN111995963A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101629057A (en) * 2009-08-22 2010-01-20 漳立冰 Nano conductive adhesive and preparation method thereof
KR101732965B1 (en) * 2016-03-17 2017-05-08 주식회사 에프피 Conductive adhesives solventless type silver paste for high radiation led
CN110093130A (en) * 2018-01-31 2019-08-06 上海宝银电子材料有限公司 A kind of electromagnetic shielding conductive silver glue and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101629057A (en) * 2009-08-22 2010-01-20 漳立冰 Nano conductive adhesive and preparation method thereof
KR101732965B1 (en) * 2016-03-17 2017-05-08 주식회사 에프피 Conductive adhesives solventless type silver paste for high radiation led
CN110093130A (en) * 2018-01-31 2019-08-06 上海宝银电子材料有限公司 A kind of electromagnetic shielding conductive silver glue and preparation method thereof

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