CN111925746A - High-heat-resistance conductive silver adhesive and preparation method thereof - Google Patents
High-heat-resistance conductive silver adhesive and preparation method thereof Download PDFInfo
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- CN111925746A CN111925746A CN202010854345.9A CN202010854345A CN111925746A CN 111925746 A CN111925746 A CN 111925746A CN 202010854345 A CN202010854345 A CN 202010854345A CN 111925746 A CN111925746 A CN 111925746A
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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
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J177/00—Adhesives based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Adhesives based on derivatives of such polymers
- C09J177/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
-
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention relates to a high heat-resistant conductive silver adhesive which is characterized by comprising the following components in parts by weight: 50-70 parts of silver powder mixture, 30-50 parts of aramid 1313 (meta-aramid) polymer stock solution and 0.5-1.0 part of coupling agent; the silver powder mixture comprises: 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder; the aramid 1313 (meta-aramid) polymer stock solution comprises: aramid 1313 (meta-aramid) resin and dimethylacetamide solvent; the coupling agent is one or a mixture of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent. The heat resistance of the high heat-resistant conductive silver adhesive is greatly improved, and the heat-resistant temperature of the common conductive adhesive is increased from about 150 ℃ to more than 200 ℃ when the common conductive adhesive is used for a long time.
Description
Technical Field
The invention relates to a high-heat-resistance conductive silver adhesive and a preparation method thereof, belonging to the technical field of conductive materials.
Background
The conductive silver paste generally bonds conductive particles together by the adhesive action of the matrix resin to form a conductive path, so as to realize the conductive connection of the adhered materials. Conductive silver paste has been widely used in packaging and bonding of electronic components and assemblies such as Liquid Crystal Displays (LCDs), Light Emitting Diodes (LEDs), Integrated Circuit (IC) chips, Printed Circuit Board Assemblies (PCBA), dot matrix blocks, ceramic capacitors, membrane switches, smart cards, radio frequency identification, etc., and has a tendency to gradually replace conventional soldering.
Along with the increasing power of electronic products, the current density is stronger and higher, the heat dissipation requirements of components are higher, the conductive silver adhesive not only provides good conductive performance and heat dissipation performance, but also needs excellent heat resistance, the heat resistance of the current epoxy resin, silica gel modified epoxy resin and the like is about 150 ℃, and the higher temperature requirements need resins and formulas with better heat resistance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the high heat-resistant conductive silver adhesive and the preparation method thereof, the heat resistance of the high heat-resistant conductive silver adhesive is greatly improved, the heat resistance temperature is increased to more than 200 ℃ from about 150 ℃ when the common conductive adhesive is used for a long time, and the volume resistivity is 5 x 10-4omega.CM or less.
The technical scheme for solving the technical problems is as follows: the high-heat-resistance conductive silver adhesive comprises the following components in parts by weight: 50-70 parts of silver powder mixture, 30-50 parts of aramid 1313 (meta-aramid) polymer stock solution and 0.5-1.0 part of coupling agent;
the silver powder mixture comprises: 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder; the aramid 1313 (meta-aramid) polymer stock solution comprises: aramid 1313 (meta-aramid) resin and dimethylacetamide solvent; the coupling agent is one or a mixture of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent.
Preferably, the weight ratio of the 0.5-1 micron granular silver powder to the 1-5 micron branch-packed silver powder to the 3-10 micron flaky silver powder is 3:1: 3.
Preferably, the aramid 1313 (meta-aramid) polymer stock solution comprises, by weight: 10-30 parts of aramid 1313 (meta-aramid) resin and 70-90 parts of dimethylacetamide solvent.
The invention also discloses a preparation method of the high heat-resistant conductive silver adhesive, which comprises the following steps:
(1) selecting 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder to be mixed to obtain a silver powder mixture;
(2) adding the silver powder mixture obtained in the step (1) into aramid 1313 (meta-aramid) polymer stock solution, and adding a coupling agent to obtain a silver colloid mixture, wherein the silver powder mixture accounts for 50-70 parts by weight, the aramid 1313 (meta-aramid) polymer stock solution accounts for 30-50 parts by weight, and the coupling agent accounts for 0.5-1.0 part by weight;
the aramid 1313 (meta-aramid) polymer stock solution comprises: aramid 1313 (meta-aramid) resin and dimethylacetamide solvent; the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent;
(3) and (3) a curing process: and (3) baking the silver colloid mixture obtained in the step (2) at 120-180 ℃ for 1 hour, and then baking at 280-380 ℃ for 30 minutes to obtain the high heat-resistant conductive silver colloid.
Preferably, the weight ratio of the 0.5-1 micron granular silver powder to the 1-5 micron branch-packed silver powder to the 3-10 micron flaky silver powder is 3:1: 3.
Preferably, the aramid 1313 (meta-aramid) polymer stock solution comprises: 10-30 parts of aramid 1313 (meta-aramid) resin and 70-90 parts of dimethylacetamide solvent.
The invention has the beneficial effects that:
(1) compared with the prior art, the aramid 1313 (meta-aramid) resin which is a matrix resin with good heat resistance is selected, the heat resistance of the whole system is greatly improved, the heat resistance temperature of the common conductive adhesive is improved to be more than 200 ℃ from about 150 ℃ (the long-term use temperature), namely the aramid 1313 (meta-aramid) resin can be used for a long time at the temperature of 200 ℃, the conventional use of the aramid 1313 (meta-aramid) resin is used in weaving, and the aramid 1313 (meta-aramid) resin is pioneering in conductive silver adhesive;
(2) the silver powder is integrated according to the types, and the silver powder is mutually matched in a granular shape, a flaky shape and a dendritic shape and is mutually filled, so that the silver powder is favorably linked, the resistance is effectively reduced, and the volume resistivity can reach 2 x 10-4Ω·CM；
(3) According to the invention, the silver powder is uniformly dispersed in the resin system by using the effective surfactant, and is not agglomerated and layered in the mixing and curing processes, so that the uniformity of resistance is effectively ensured, and the condition of large local resistance is avoided.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
A preparation method of high heat-resistant conductive silver adhesive comprises the following steps:
(1) selecting 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder to be mixed to obtain a silver powder mixture; the weight ratio of the 0.5-1 micron granular silver powder, the 1-5 micron branch-packed silver powder and the 3-10 micron flaky silver powder is 3:1: 3.
(2) Adding the silver powder mixture obtained in the step (1) into an aramid 1313 (meta-aramid) polymer stock solution, and adding a coupling agent to obtain a silver colloid mixture, wherein the silver powder mixture comprises 50 parts by weight, the aramid 1313 (meta-aramid) polymer stock solution comprises 50 parts by weight, and the coupling agent comprises 0.5 part by weight;
the aramid 1313 (meta-aramid) polymer stock solution comprises: 30 parts of aramid 1313 (m-aramid) resin and 70 parts of dimethylacetamide solvent; the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent;
(3) and (3) a curing process: and (3) baking the silver colloid mixture obtained in the step (2) at 120-180 ℃ for 1 hour, and then baking at 280-380 ℃ for 30 minutes to obtain the high heat-resistant conductive silver colloid.
Example 2
A preparation method of high heat-resistant conductive silver adhesive comprises the following steps:
(1) selecting 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder to be mixed to obtain a silver powder mixture; the weight ratio of the 0.5-1 micron granular silver powder, the 1-5 micron branch-packed silver powder and the 3-10 micron flaky silver powder is 3:1: 3.
(2) Adding the silver powder mixture obtained in the step (1) into aramid 1313 (meta-aramid) polymer stock solution, and adding a coupling agent to obtain a silver colloid mixture, wherein the silver powder mixture comprises 70 parts by weight, the aramid 1313 (meta-aramid) polymer stock solution comprises 30 parts by weight, and the coupling agent comprises 0.8 part by weight;
the aramid 1313 (meta-aramid) polymer stock solution comprises: 10 parts of aramid 1313 (m-aramid) resin and 90 parts of dimethylacetamide solvent; the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent;
(3) and (3) a curing process: and (3) baking the silver colloid mixture obtained in the step (2) at 120-180 ℃ for 1 hour, and then baking at 280-380 ℃ for 30 minutes to obtain the high heat-resistant conductive silver colloid.
Example 3
A preparation method of high heat-resistant conductive silver adhesive comprises the following steps:
(1) selecting 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder to be mixed to obtain a silver powder mixture; the weight ratio of the 0.5-1 micron granular silver powder, the 1-5 micron branch-packed silver powder and the 3-10 micron flaky silver powder is 3:1: 3.
(2) Adding the silver powder mixture obtained in the step (1) into an aramid 1313 (meta-aramid) polymer stock solution, and adding a coupling agent to obtain a silver colloid mixture, wherein the silver powder mixture comprises 60 parts by weight, the aramid 1313 (meta-aramid) polymer stock solution comprises 40 parts by weight, and the coupling agent comprises 1.0 part by weight;
the aramid 1313 (meta-aramid) polymer stock solution comprises: 20 parts of aramid 1313 (m-aramid) resin and 80 parts of dimethylacetamide solvent; the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent;
(3) and (3) a curing process: and (3) baking the silver colloid mixture obtained in the step (2) at 120-180 ℃ for 1 hour, and then baking at 280-380 ℃ for 30 minutes to obtain the high heat-resistant conductive silver colloid.
The conductive silver pastes obtained in examples 1 to 3 and the commercially available common conductive silver paste were subjected to a performance test using a measurement method known in the art, and the test data are as follows in table 1:
table 1 conductive silver paste property test data
| Heat resistance temperature (. degree. C.) | Volume resistivity (omega CM) | |
| Conductive silver paste of example 1 | 239 | 2*10-4 |
| Conductive silver paste of example 2 | 230 | 1.7*10-4 |
| Conductive silver paste of example 3 | 221 | 1.9*10-4 |
| Common conductive silver adhesive on market | 155 | 5.5*10-4 |
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. The high-heat-resistance conductive silver adhesive is characterized by comprising the following components in parts by weight: 50-70 parts of silver powder mixture, 30-50 parts of aramid 1313 (meta-aramid) polymer stock solution and 0.5-1.0 part of coupling agent;
the silver powder mixture comprises: 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder; the aramid 1313 (meta-aramid) polymer stock solution comprises: aramid 1313 (meta-aramid) resin and dimethylacetamide solvent; the coupling agent is one or a mixture of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent.
2. The highly heat-resistant conductive silver paste according to claim 1, wherein the weight ratio of the 0.5-1 micron granular silver powder, the 1-5 micron branch-packed silver powder and the 3-10 micron plate-like silver powder is 3:1: 3.
3. The high-heat-resistance conductive silver adhesive as claimed in claim 1, wherein the aramid 1313 (meta-aramid) polymer stock solution comprises, in parts by weight: 10-30 parts of aramid 1313 (meta-aramid) resin and 70-90 parts of dimethylacetamide solvent.
4. A method for preparing the high heat-resistant conductive silver paste according to any one of claims 1 to 3, wherein the method comprises the following steps:
(1) selecting 0.5-1 micron granular silver powder, 1-5 micron branch-packed silver powder and 3-10 micron flaky silver powder to be mixed to obtain a silver powder mixture;
(2) adding the silver powder mixture obtained in the step (1) into aramid 1313 (meta-aramid) polymer stock solution, and adding a coupling agent to obtain a silver colloid mixture, wherein the silver powder mixture accounts for 50-70 parts by weight, the aramid 1313 (meta-aramid) polymer stock solution accounts for 30-50 parts by weight, and the coupling agent accounts for 0.5-1.0 part by weight;
the aramid 1313 (meta-aramid) polymer stock solution comprises: aramid 1313 (meta-aramid) resin and dimethylacetamide solvent; the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and titanate coupling agent;
(3) and (3) a curing process: and (3) baking the silver colloid mixture obtained in the step (2) at 120-180 ℃ for 1 hour, and then baking at 280-380 ℃ for 30 minutes to obtain the high heat-resistant conductive silver colloid.
5. The method for preparing high heat-resistant conductive silver paste according to claim 4, wherein the weight ratio of the 0.5-1 micron granular silver powder, the 1-5 micron branch-packed silver powder and the 3-10 micron plate-like silver powder is 3:1: 3.
6. The method for preparing the high-heat-resistance conductive silver adhesive according to claim 4, wherein the aramid 1313 (meta-aramid) polymer stock solution comprises: 10-30 parts of aramid 1313 (meta-aramid) resin and 70-90 parts of dimethylacetamide solvent.
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| CN202010854345.9A CN111925746A (en) | 2020-08-24 | 2020-08-24 | High-heat-resistance conductive silver adhesive and preparation method thereof |
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2020
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