CN109486461A - A kind of high stability LED encapsulation conductive silver glue and preparation method thereof - Google Patents
A kind of high stability LED encapsulation conductive silver glue and preparation method thereof Download PDFInfo
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- CN109486461A CN109486461A CN201811344115.7A CN201811344115A CN109486461A CN 109486461 A CN109486461 A CN 109486461A CN 201811344115 A CN201811344115 A CN 201811344115A CN 109486461 A CN109486461 A CN 109486461A
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- epoxy resin
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- conductive silver
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- 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
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- 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
A kind of high stability LED encapsulation conductive silver glue, it is characterised in that be made of the matrix resin of 5 ~ 40%wt and the silver powder filler of 60 ~ 95%wt；Described matrix resin contains 70 ~ 95%wt of macromolecule prepolymer, 1 ~ 10%wt of coupling agent, 1 ~ 20%wt of reactive diluent, 1 ~ 10%wt of non-activated thinner；The macromolecule prepolymer is the prepolymer of epoxy resin and amine curing agent, and wherein epoxy resin is the combination of one or both of glycidyl amine type epoxy resin and bisphenol A type epoxy resin.The present invention also provides a kind of preparation methods of above-mentioned high stability LED encapsulation conductive silver glue.LED encapsulation of the invention epoxy conductive silver glue has high stability, high reliability, and electric conductivity is high, adhesion strength is big, thermal conductivity is good, excellent combination property.
Description
Technical field
The present invention relates to LED encapsulation materials, and in particular to a kind of high stability LED encapsulation conductive silver glue and its preparation side
Method.
Background technique
With the increasingly raising of China's economic level and scientific and technological strength, China has become important LED production and encapsulation base
Ground.The a part of LED die bond as packaging technology, wherein the performance of die bond material is to the quality of LED and the extensive batch of LED
Formula encapsulation has highly important influence.A kind of composite material of the conducting resinl as environment-friendly type not only has excellent conduction, leads
It is hot, moreover it is possible to excellent adhesive property be provided, thus be often used as the die bond material of LED.
Conducting resinl composition mainly includes matrix resin, conductive filler, auxiliary agent etc..Wherein, matrix resin primarily serves bonding
The effect of conductive filler, fixed wafer is broadly divided into epoxy resin, phenolic resin, organic siliconresin, polyurethane etc..Epoxy
Resin due to having many advantages, such as compared with high bond strength, corrosion resistance is strong and storage stability is good, be widely used as the base of conducting resinl
Body resin.Conductive filler mainly has copper powder, silver powder, bronze, metal oxide, graphite etc., wherein silver powder due to Low ESR,
The advantages that chemical stability is good, relative low price, is widely used as conductive filler.Therefore, epoxy conductive silver glue is by pass
Note and the good die bond material of Market reaction.
Currently, the conductive adhesive for LED encapsulation of domestic production is primarily present that stability is poor, market is not achieved in partial properties index
It is required that the problems such as and only occupy the market of sub-fraction, the haze moment that external product monopolizes domestic conducting resinl shrouds in motherland
Overhead.Therefore, a kind of high stability, high reliability, the conducting resinl haveing excellent performance are developed, as core science and technology is in country
Importance and urgency.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of high stability LED encapsulation conductive silver glue and its preparation sides
Method, this LED encapsulation epoxy conductive silver glue have many advantages, such as that high stability, high reliability, adhesion strength are big.The technology of use
Scheme is as follows:
A kind of high stability LED encapsulation conductive silver glue, it is characterised in that by the matrix resin and 60 ~ 95% wt of 5 ~ 40% wt
Silver powder filler composition；Described matrix resin contain 70 ~ 95%wt of macromolecule prepolymer, 1 ~ 10% wt of coupling agent, reactive diluent 1 ~
20% wt, 1 ~ 10% wt of non-activated thinner；The macromolecule prepolymer is the prepolymer of epoxy resin and amine curing agent,
Middle epoxy resin is the combination of one or both of glycidyl amine type epoxy resin and bisphenol A type epoxy resin.
Reactive diluent and non-activated thinner are applied in combination the present invention, and the viscosity of conductive silver glue and thixotropy can be made to protect
It holds in a more stable section, keeps its die bond workability strong.The curing agent that the present invention uses is the lower aromatic amine of activity
Curing agent is conducive to control curing rate in OK range.Conductive silver glue of the invention is free of curing accelerator, in this way may be used
Conductive silver glue made of making has longer stability and validity period.
It is preferred that the mass percent of epoxy resin is 60 ~ 80% in above-mentioned macromolecule prepolymer, the quality hundred of amine curing agent
Score is 20 ~ 40%.
It is preferred that the mass percent of macromolecule prepolymer is 80 ~ 90% in above-mentioned matrix resin.
It is preferred that the mass percent of coupling agent is 1 ~ 5% in above-mentioned matrix resin.
It is preferred that the mass percent of reactive diluent is 5 ~ 10% in above-mentioned matrix resin.
It is preferred that the mass percent of non-activated thinner is 1 ~ 10% in above-mentioned matrix resin.
It is preferred that the mass percent of matrix resin is 10 ~ 30%, silver powder in above-mentioned high stability LED encapsulation conductive silver glue
Packing quality percentage is 70 ~ 90%.
It is preferred that above-mentioned glycidyl amine type epoxy resin is 4,4 '-diaminodiphenylmethane epoxy resin (AG-80) and right
The combination of one or both of amino-phenol epoxy resin (AFG-90).
It is preferred that above-mentioned bisphenol A type epoxy resin is in bisphenol A type epoxy resin E-54 and bisphenol A type epoxy resin E-44
The combination of one or both.
It is preferred that above-mentioned amine curing agent is one in diaminodiphenyl-methane (DDM) and diaminodiphenylsulfone (DDS)
The combination of kind or both.
It is preferred that above-mentioned coupling agent is in silane resin acceptor kh-550, silane coupling agent KH-560 and silane coupling agent KH-590
One kind or in which a variety of combinations.
It is preferred that above-mentioned reactive diluent is phenyl glycidyl ether (PGE), butanediol diglycidyl ether, trihydroxy methyl
One of propane triglycidyl ether and T 55 or in which a variety of combinations.
It is preferred that above-mentioned non-activated thinner is diethyl phthalate, 2-Butoxyethyl acetate and ethylene carbonate
One of or in which a variety of combinations.
It is preferred that above-mentioned silver powder filler be the flake silver powder that average grain diameter is 10 μm, the flake silver powder that average grain diameter is 3 μm and
Average grain diameter is one of spherical silver powder of 300nm or in which a variety of combinations.Use flake silver powder and the spherical silver powder of nanometer
Collectively as conductive filler, conducting resinl thixotropy can be made more preferable, be more suitable for the extensive die bond encapsulation of LED.Three of the above inhomogeneity
The silver powder of type, which is arranged in pairs or groups, to be used, and can make conductive gumminess and thixotropic index in suitable range, and nano-silver powder can prevent from settling.
The present invention also provides a kind of preparation methods of above-mentioned high stability LED encapsulation conductive silver glue, it is characterised in that packet
Include following step:
(1) it is equipped with epoxy resin and amine curing agent, then makes epoxy resin and amine curing agent that pre-polymerization occur, obtains macromolecule
Prepolymer；
(2) it is equipped with macromolecule prepolymer, coupling agent, reactive diluent and non-activated thinner in proportion, then by coupling agent, work
Property diluent and non-activated thinner be added in macromolecule prepolymer, and stir to be uniformly mixed, obtain matrix resin；
(3) it is equipped with silver powder filler and matrix resin in proportion, then silver powder filler is added in matrix resin, and stirs to mixed
It closes uniformly, obtains high stability LED encapsulation conductive silver glue.
In preferred steps (1), make epoxy resin and amine curing agent that pre-polymerization occur at 80 ~ 105 DEG C.
In preferred steps (1), the proportion of epoxy resin and amine curing agent are as follows: the mass percent of epoxy resin be 60 ~
80%wt, amine curing agent mass percent be 20 ~ 40% wt(sum of the two be 100% wt).
In step (2), be used to prepare the raw material of matrix resin proportion be 70 ~ 95%wt of macromolecule prepolymer, coupling agent 1 ~
10% wt, 1 ~ 20% wt of reactive diluent, these four raw material summations of 1 ~ 10% wt(of non-activated thinner are 100% wt).
In step (3), the proportion of matrix resin and silver powder filler are as follows: 5 ~ 40% wt of matrix resin, silver powder filler 60 ~ 95%
Wt(sum of the two is 100% wt).10 ~ 30% wt of preferred substrate resin, 70 ~ 90% wt of silver powder filler.
In preferred steps (3), silver powder filler and matrix resin are uniformly mixed in vacuum mixer.
Conductive silver glue of the invention mainly has the advantage that
(1) it has good stability: being placed at room temperature for 10 days, viscosity and thixotropic index variation are respectively less than 5%；0 DEG C or less stable storing phase
More than 1 year；
(2) electric conductivity is high: volume resistivity is less than 2.0 × 10-5Ω·cm；
(3) adhesion strength is big: being greater than 30MPa with the adhesion strength of silver coating；
(4) thermal conductivity is good: thermal conductivity is higher than 15W/mK；
(5) high reliablity: high temperature, high humidity and hyperbaric environment (121 DEG C, the steam of 2 atm.s of the conductive silver glue by 300 hours
Environment, i.e. PCT) after, conductive silver glue does not change the adhesion strength and volume resistivity of silver coating；By 500 bouts -65 ~
After 150 DEG C of cooling thermal impact, conductive silver glue is to the adhesion strength and volume resistivity of silver coating also without variation；At 260 DEG C
Under high temperature, conductive silver glue is greater than 7MPa to silver coating adhesion strength.
In brief, LED encapsulation of the invention epoxy conductive silver glue has a high stability, high reliability, electric conductivity is high,
Adhesion strength is big, thermal conductivity is good, excellent combination property.
Specific embodiment
Embodiment 1
In the present embodiment, the preparation method of high stability LED encapsulation conductive silver glue includes the following steps:
(1) it is equipped with epoxy resin and amine curing agent, then makes epoxy resin and amine curing agent that pre-polymerization occur at 80 ~ 85 DEG C
(epoxy resin can be uniformly mixed with amine curing agent, under agitation control the temperature of the mixture of the two 80 ~ 85
DEG C, heat preservation is cooled to room temperature after 1.5 hours), obtain macromolecule prepolymer；
In this step (1), the proportion of epoxy resin and amine curing agent are as follows: the mass percent of epoxy resin is 60%wt, amine
The mass percent of curing agent is 40% wt；Epoxy resin be bisphenol A type epoxy resin E-54, mutual-amino phenol epoxy resin and
4,4 '-diaminodiphenylmethane epoxy resin combination (wherein mutual-amino phenol epoxy resin accounts for the 1/2 of epoxy resin total amount,
Bisphenol A type epoxy resin E-54,4,4 '-diaminodiphenylmethane epoxy resin respectively account for the 1/4 of epoxy resin total amount)；Amine is solid
Agent is diaminodiphenyl-methane；
(2) it is equipped with macromolecule prepolymer, coupling agent, reactive diluent and non-activated thinner in proportion, then by coupling agent, work
Property diluent and non-activated thinner be added in macromolecule prepolymer, and stir to be uniformly mixed, obtain matrix resin；
In this step (2), the proportion for being used to prepare the raw material of matrix resin is macromolecule prepolymer 80%wt, 5% wt of coupling agent
(being silane coupling agent KH-560), 10% wt(of reactive diluent are phenyl glycidyl ether), 5% wt of non-activated thinner
(being 2-Butoxyethyl acetate)；
(3) it is equipped with silver powder filler and matrix resin in proportion, then silver powder filler is added in matrix resin, and stirs to mixed
It closes and uniformly (is uniformly mixed silver powder filler and matrix resin in vacuum mixer, vacuum mixer can also be simultaneously to therein
Material carries out deaeration), obtain high stability LED encapsulation conductive silver glue.
In this step (3), the proportion of matrix resin and silver powder filler are as follows: 30% wt of matrix resin, 70% wt of silver powder filler.
Silver powder filler is the flake silver powder that average grain diameter is 3 μm.
High stability LED encapsulation conductive silver glue obtained is by the matrix resin of 30% wt and the silver powder filler group of 70% wt
At.Described matrix resin contains macromolecule prepolymer 80%wt, 5% wt of coupling agent, 10% wt of reactive diluent, inactive diluents
5% wt of agent.
Embodiment 2
In the present embodiment, the preparation method of high stability LED encapsulation conductive silver glue includes the following steps:
(1) it is equipped with epoxy resin and amine curing agent, then occurs at 100 ~ 105 DEG C epoxy resin and amine curing agent pre-
It is poly- (epoxy resin to be uniformly mixed with amine curing agent, under agitation control the temperature of the mixture of the two 100
~ 105 DEG C, heat preservation is cooled to room temperature after 1.5 hours), obtain macromolecule prepolymer；
In this step (1), the proportion of epoxy resin and amine curing agent are as follows: the mass percent of epoxy resin is 70%wt, amine
The mass percent of curing agent is 30% wt；Epoxy resin is bisphenol A type epoxy resin E-44 and 4,4 '-diaminodiphenylmethane
The combination of epoxy resin (bisphenol A type epoxy resin E-44 and 4,4 '-diaminodiphenylmethane epoxy resin respectively accounts for half)；Amine
Curing agent is diaminodiphenylsulfone；
(2) it is equipped with macromolecule prepolymer, coupling agent, reactive diluent and non-activated thinner in proportion, then by coupling agent, work
Property diluent and non-activated thinner be added in macromolecule prepolymer, and stir to be uniformly mixed, obtain matrix resin；
In this step (2), the proportion for being used to prepare the raw material of matrix resin is macromolecule prepolymer 83%wt, 1% wt of coupling agent
(being silane coupling agent KH-560), 6% wt(of reactive diluent wherein butanediol diglycidyl ether and trimethylolpropane tris
Glycidol ether respectively accounts for half), wherein ethylene carbonate and diethyl phthalate respectively account for 10% wt(of non-activated thinner
Half)；
(3) it is equipped with silver powder filler and matrix resin in proportion, then silver powder filler is added in matrix resin, and stirs to mixed
It closes and uniformly (is uniformly mixed silver powder filler and matrix resin in vacuum mixer, vacuum mixer can also be simultaneously to therein
Material carries out deaeration), obtain high stability LED encapsulation conductive silver glue.
In this step (3), the proportion of matrix resin and silver powder filler are as follows: 25% wt of matrix resin, 75% wt of silver powder filler
(wherein 12.5% wt is the flake silver powder that average grain diameter is 10 μm, remaining 62.5% wt is the sheet silver that average grain diameter is 3 μm
Powder).
High stability LED encapsulation conductive silver glue obtained is by the matrix resin of 20% wt and the silver powder filler group of 80% wt
At.Described matrix resin contains macromolecule prepolymer 83%wt, 1% wt of coupling agent, 6% wt of reactive diluent, non-activated thinner
10% wt。
Embodiment 3
In the present embodiment, the preparation method of high stability LED encapsulation conductive silver glue includes the following steps:
(1) it is equipped with epoxy resin and amine curing agent, then makes epoxy resin and amine curing agent that pre-polymerization occur at 80 ~ 83 DEG C
(epoxy resin can be uniformly mixed with amine curing agent, under agitation control the temperature of the mixture of the two 80 ~ 83
DEG C, heat preservation is cooled to room temperature after 1.5 hours), obtain macromolecule prepolymer；
In this step (1), the proportion of epoxy resin and amine curing agent are as follows: the mass percent of epoxy resin is 74%wt, amine
The mass percent of curing agent is 26% wt；Epoxy resin is bisphenol A type epoxy resin E-54, bisphenol A type epoxy resin E-44
(wherein 4,4 '-diaminodiphenylmethane epoxy resin account for epoxy resin for combination with 4,4 '-diaminodiphenylmethane epoxy resin
The 1/2 of total amount, bisphenol A type epoxy resin E-54, bisphenol A type epoxy resin E-44 respectively account for the 1/4 of epoxy resin total amount)；Amine
Curing agent is diaminodiphenyl-methane；
(2) it is equipped with macromolecule prepolymer, coupling agent, reactive diluent and non-activated thinner in proportion, then by coupling agent, work
Property diluent and non-activated thinner be added in macromolecule prepolymer, and stir to be uniformly mixed, obtain matrix resin；
In this step (2), the proportion for being used to prepare the raw material of matrix resin is macromolecule prepolymer 87%wt, 2% wt of coupling agent
Wherein 3% wt is T 55, remaining 2% wt by (being silane coupling agent KH-590), 5% wt(of reactive diluent
For phenyl glycidyl ether), 6% wt(of non-activated thinner be 2-Butoxyethyl acetate)；
(3) it is equipped with silver powder filler and matrix resin in proportion, then silver powder filler is added in matrix resin, and stirs to mixed
It closes and uniformly (is uniformly mixed silver powder filler and matrix resin in vacuum mixer, vacuum mixer can also be simultaneously to therein
Material carries out deaeration), obtain high stability LED encapsulation conductive silver glue.
In this step (3), the proportion of matrix resin and silver powder filler are as follows: 15% wt of matrix resin, 85% wt of silver powder filler
(wherein 52% wt is the flake silver powder that average grain diameter is 10 μm, remaining 33% wt is the spherical silver powder that average grain diameter is 300nm).
High stability LED encapsulation conductive silver glue obtained is by the matrix resin of 15% wt and the silver powder filler group of 85% wt
At.Described matrix resin contains macromolecule prepolymer 87%wt, 2% wt of coupling agent, 5% wt of reactive diluent, non-activated thinner
6% wt。
Embodiment 4
In the present embodiment, the preparation method of high stability LED encapsulation conductive silver glue includes the following steps:
(1) it is equipped with epoxy resin and amine curing agent, then makes epoxy resin and amine curing agent that pre-polymerization occur at 90 ~ 95 DEG C
(epoxy resin can be uniformly mixed with amine curing agent, under agitation control the temperature of the mixture of the two 90 ~ 95
DEG C, it is cooling after heat preservation 1.5 hours), obtain macromolecule prepolymer；
In this step (1), the proportion of epoxy resin and amine curing agent are as follows: the mass percent of epoxy resin is 80%wt, amine
The mass percent of curing agent is 20% wt；Epoxy resin is bisphenol A type epoxy resin E-44 and 4,4 '-diaminodiphenylmethane
(bisphenol A type epoxy resin E-44 accounts for the 3/4 of weight epoxy, 4,4 '-diaminodiphenylmethane epoxies for the combination of epoxy resin
Resin accounts for the 1/4 of weight epoxy)；Amine curing agent is diaminodiphenyl-methane；
(2) it is equipped with macromolecule prepolymer, coupling agent, reactive diluent and non-activated thinner in proportion, then by coupling agent, work
Property diluent and non-activated thinner be added in macromolecule prepolymer, and stir to be uniformly mixed, obtain matrix resin；
In this step (2), the proportion for being used to prepare the raw material of matrix resin is macromolecule prepolymer 81%wt, 2% wt of coupling agent
Wherein 4% wt is phenyl glycidyl ether by (being silane resin acceptor kh-550), 7% wt(of reactive diluent, remaining 3% wt is
Trihydroxymethylpropanyltri diglycidyl ether), wherein 9% wt is diethyl phthalate to 10% wt(of non-activated thinner, remaining
1% wt is 2-Butoxyethyl acetate)；
(3) it is equipped with silver powder filler and matrix resin in proportion, then silver powder filler is added in matrix resin, and stirs to mixed
It closes and uniformly (is uniformly mixed silver powder filler and matrix resin in vacuum mixer, vacuum mixer can also be simultaneously to therein
Material carries out deaeration), obtain high stability LED encapsulation conductive silver glue.
In this step (3), the proportion of matrix resin and silver powder filler are as follows: 10% wt of matrix resin, 90% wt of silver powder filler
(wherein 63% wt is the flake silver powder that average grain diameter is 10 μm, and in addition 18% wt is the flake silver powder that average grain diameter is 3 μm,
9% wt of remaininging is the spherical silver powder that average grain diameter is 300nm).
High stability LED encapsulation conductive silver glue obtained is by the matrix resin of 10% wt and the silver powder filler group of 90% wt
At.Described matrix resin contains macromolecule prepolymer 81%wt, 2% wt of coupling agent, 7% wt of reactive diluent, non-activated thinner
10% wt。
Respectively by conductive silver glue made from embodiment 1 ~ 4 and commercial product (using the optimal product of performance currently on the market)
It is toasted 2 hours at 170 DEG C, sample is made, is tested respectively:
Adhesion strength is testing conductive elargol bonding plating silver plate and 1.1mm*Destructive thrust after 1.2mm silicon chip；Volume electricity
Resistance rate is to be tested after preparing sample according to the length of sheet glass, width and thickness using four foot sonde methods；Thermal conductivity be by
According to coefficient of conductivity tester QTM-500 test；Cooling thermal impact experiment is that sample is placed in cooling thermal impact 500 at -65 ~ 150 DEG C
Adhesion strength, volume resistivity and thermal conductivity are tested after bout；High temperature, high humidity, high pressure (PCT) senile experiment are to be placed in sample
121 DEG C, the lower 168 hours test sample adhesion strengths of water vapour environment of 2atm..
The stability test result and the performance test results of embodiment 1 ~ 4 and commercial product are as shown in table one, table two:
Table one: stability test result
a: 0.5 min-1;B: sample is stored at room temperature;C: 0 DEG C of sample saves；D:0.5/5 min-1
Table two: conductive silver glue the performance test results
As shown in Table 1, the conductive silver glue stability of embodiment 1 ~ 4 is better than commercial product, can meet the extensive batch type of LED
Encapsulation requirement, be greatly improved LED encapsulation factory packaging efficiency.
As shown in Table 2, for adhesion strength, embodiment 1 ~ 4 is better than commercial product, and passes through cooling thermal impact or PCT
Afterwards, adhesion strength has no significant change, and especially at 260 DEG C, the adhesion strength of embodiment 1 ~ 4 is significantly better than commercial product.
In terms of volume resistivity, embodiment 1 ~ 3 is noticeably greater than commercial product, and after cooling thermal impact or PCT, volume resistivity
It changes greatly, and the volume resistivity of embodiment 4 is suitable in commercial product, cold-resistant thermal shock and PCT are significantly better than commercially available production
Product.In terms of thermal conductivity, embodiment 1 ~ 3 is slightly worse than commercial product, and embodiment 4 is suitable with commercial product.
To sum up, embodiment 1-4, which has, is significantly better than the comprehensive performance of commercial product, especially stability, reliability and
It is excellent in terms of adhesion strength.
Claims (10)
1. a kind of high stability LED encapsulation conductive silver glue, it is characterised in that by the matrix resin and 60 ~ 95% wt of 5 ~ 40% wt
Silver powder filler composition；Described matrix resin contains 70 ~ 95%wt of macromolecule prepolymer, 1 ~ 10% wt of coupling agent, reactive diluent
1 ~ 20% wt, 1 ~ 10% wt of non-activated thinner；The macromolecule prepolymer is the prepolymer of epoxy resin and amine curing agent,
Wherein epoxy resin is the combination of one or both of glycidyl amine type epoxy resin and bisphenol A type epoxy resin.
2. high stability LED encapsulation conductive silver glue according to claim 1, it is characterized in that: the macromolecule prepolymer
The mass percent of middle epoxy resin is 60 ~ 80%, and the mass percent of amine curing agent is 20 ~ 40%.
3. high stability LED encapsulation conductive silver glue according to claim 1 or 2, it is characterized in that: the glycidyl amine
Type epoxy resin is the group of one or both of 4,4 '-diaminodiphenylmethane epoxy resin and mutual-amino phenol epoxy resin
It closes.
4. high stability LED encapsulation conductive silver glue according to claim 1 or 2, it is characterized in that: the bisphenol-A type ring
Oxygen resin is the combination of one or both of bisphenol A type epoxy resin E-54 and bisphenol A type epoxy resin E-44.
5. high stability LED encapsulation conductive silver glue according to claim 1 or 2, it is characterized in that: the amine curing agent
For the combination of one or both of diaminodiphenyl-methane and diaminodiphenylsulfone.
6. high stability LED encapsulation conductive silver glue according to claim 1 or 2, it is characterized in that: the coupling agent is silicon
One of alkane coupling agent KH-550, silane coupling agent KH-560 and silane coupling agent KH-590 or in which a variety of combinations.
7. high stability LED encapsulation conductive silver glue according to claim 1 or 2, it is characterized in that: the reactive diluent
For phenyl glycidyl ether, butanediol diglycidyl ether, trihydroxymethylpropanyltri diglycidyl ether and glycerol three-glycidyl
One of ether or in which a variety of combinations.
8. high stability LED encapsulation conductive silver glue according to claim 1 or 2, it is characterized in that: the inactive diluents
Agent is one of diethyl phthalate, 2-Butoxyethyl acetate and ethylene carbonate or in which a variety of combinations.
9. high stability LED encapsulation conductive silver glue according to claim 1 or 2, it is characterized in that: the silver powder filler is
Flake silver powder, the flake silver powder that average grain diameter is 3 μm and the average grain diameter that average grain diameter is 10 μm are in the spherical silver powder of 300nm
One kind or in which a variety of combinations.
10. the preparation method that conductive silver glue is used in high stability LED encapsulation of any of claims 1 or 2, it is characterised in that including under
State step:
(1) it is equipped with epoxy resin and amine curing agent, then makes epoxy resin and amine curing agent that pre-polymerization occur, obtains macromolecule
Prepolymer；
(2) it is equipped with macromolecule prepolymer, coupling agent, reactive diluent and non-activated thinner in proportion, then by coupling agent, work
Property diluent and non-activated thinner be added in macromolecule prepolymer, and stir to be uniformly mixed, obtain matrix resin；
(3) it is equipped with silver powder filler and matrix resin in proportion, then silver powder filler is added in matrix resin, and stirs to mixed
It closes uniformly, obtains high stability LED encapsulation conductive silver glue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811344115.7A CN109486461A (en) | 2018-11-13 | 2018-11-13 | A kind of high stability LED encapsulation conductive silver glue and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811344115.7A CN109486461A (en) | 2018-11-13 | 2018-11-13 | A kind of high stability LED encapsulation conductive silver glue and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
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Cited By (6)
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| CN110117474A (en) * | 2019-04-12 | 2019-08-13 | 江苏矽时代材料科技有限公司 | A kind of conduction high-thermal-conductivity epoxy resin composition and preparation method thereof |
| CN110689993A (en) * | 2019-09-03 | 2020-01-14 | 北京氦舶科技有限责任公司 | Low-temperature curing conductive silver paste for electronic packaging and preparation method thereof |
| CN112951953A (en) * | 2019-12-11 | 2021-06-11 | 深圳市聚飞光电股份有限公司 | LED printing method |
| CN113563837A (en) * | 2021-09-26 | 2021-10-29 | 西安宏星电子浆料科技股份有限公司 | HJT conductive silver colloid composition, preparation method thereof and HJT solar cell |
| CN115216228A (en) * | 2022-07-28 | 2022-10-21 | 南方科技大学 | Method for improving heat conductivity of conductive silver adhesive, conductive silver adhesive and application thereof |
| CN115678473A (en) * | 2022-11-09 | 2023-02-03 | 宁夏中色新材料有限公司 | Single-component silver conductive adhesive suitable for normal-temperature storage and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110117474A (en) * | 2019-04-12 | 2019-08-13 | 江苏矽时代材料科技有限公司 | A kind of conduction high-thermal-conductivity epoxy resin composition and preparation method thereof |
| CN110689993A (en) * | 2019-09-03 | 2020-01-14 | 北京氦舶科技有限责任公司 | Low-temperature curing conductive silver paste for electronic packaging and preparation method thereof |
| CN112951953A (en) * | 2019-12-11 | 2021-06-11 | 深圳市聚飞光电股份有限公司 | LED printing method |
| CN113563837A (en) * | 2021-09-26 | 2021-10-29 | 西安宏星电子浆料科技股份有限公司 | HJT conductive silver colloid composition, preparation method thereof and HJT solar cell |
| CN115216228A (en) * | 2022-07-28 | 2022-10-21 | 南方科技大学 | Method for improving heat conductivity of conductive silver adhesive, conductive silver adhesive and application thereof |
| CN115678473A (en) * | 2022-11-09 | 2023-02-03 | 宁夏中色新材料有限公司 | Single-component silver conductive adhesive suitable for normal-temperature storage and preparation method thereof |
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