CN107227130A - A kind of high-power LED encapsulation conductive silver glue - Google Patents
A kind of high-power LED encapsulation conductive silver glue Download PDFInfo
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- CN107227130A CN107227130A CN201710459698.7A CN201710459698A CN107227130A CN 107227130 A CN107227130 A CN 107227130A CN 201710459698 A CN201710459698 A CN 201710459698A CN 107227130 A CN107227130 A CN 107227130A
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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
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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
- 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
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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
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- 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
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- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- 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
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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
- C08L2205/02—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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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of controllable high-power LED encapsulation conductive silver glues：（1）Prepare silver powder：Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；Wheat stalk is taken, amount of water is 10 times of wheat stalk, 80 DEG C of holding heating extraction 56 hours, and normal temperature is saved backup after filter residue；1 times of weight sweet orange peel extract solution is taken, 1 times of weight pomelo peel extract solution, 0.5 0.8 times of weight wheat stalk extract solutions are mixed with the 0.3mM of 15 18 times of weight silver nitrate solution, the pH value of regulation silver nitrate solution is 9.0,65 DEG C of 20 25min of reaction；Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；(2) matrix polymer is configured；（3）Prepare conducting resinl.
Description
Technical field
The invention belongs to electronic material preparation field, it is related to a kind of high-power LED encapsulation conductive silver glue of excellent performance.
Background technology
Semiconductor solid-state luminescent device LED is light emitting diode, be Developing the swiftest and the most violent energy-conserving and environment-protective show and
Lighting source, LED illumination application is just progressively permeated from LED backlight to general lighting field.Progressively from outdoor lighting to interior
Illumination spread.For encapsulation, how as many as possible in limited cost-range its key technology is after all
The light that sends of extraction chip, while reducing packaging thermal resistance, improve reliability.
The producer of current domestic production LED conductive silver glues is still few, and single-component solvent-free room temperature storage heat radiating type is led
Electric elargol is the developing direction of current LED packages conductive silver glue.Especially there are good heat conduction and heat dispersion, Ke Yiman
High reliability request of the sufficient great power LED to conductive silver glue.
The preparation method of some LED encapsulation conductive silver glues, such as Chinese patent application has been disclosed in prior art
201210304705.3 disclose a kind of preparation method of silver-plated copper powder/epoxide resin conductive adhesive, the conducting resinl electric conductivity of preparation
Can be good, working life is up to more than 3 months；Next improves the electric conductivity of conducting resinl；After silver salt redox reaction, promote
The aldehyde radical entered on agent molecule chain also acts the effect of stable conducting resinl contact resistance, improves the ageing-resistant performance of conducting resinl,
But thermal conductivity factor is outstanding not enough in practical operation, also inadequate high-temp resisting high-humidity resisting.And for example Chinese patent application
201510169776.0 are disclosed a kind of thermal conductivity factor height, shear strength greatly, and the LED encapsulation of the function admirable of high-temp resisting high-humidity resisting is used
Conductive silver glue, it is applicable to high-power LED encapsulation.But find that its process control needs is high in practical operation, heat conductivility
Not good enough, high-temperature shelf property is not good enough.
The present invention is intended to provide a kind of production stage is simple, heat conduction is good, shear strength is big, the function admirable of high-temp resisting high-humidity resisting
LED encapsulation conductive silver glues, it is applicable to high-power LED encapsulation.
The content of the invention
The present invention is intended to provide a kind of production stage is simple and environmentally-friendly, thermal conductivity factor is high, shear strength is big, high-temp resisting high-humidity resisting
The LED encapsulation conductive silver glues of function admirable, it is applicable to high-power LED encapsulation.
Multiple additives are usually contained in conductive silver glue system.
(1) accelerator：To the system that solidification temperature is high, curing rate is slow, solidification temperature, control can be reduced by adding accelerator
Solidification rate processed.Including imidazoles and its salt, phosphorus-containing compound, guanidine derivatives, organic urea etc..
(2) diluent：Regulation system viscosity, improving operability, (non-activated thinner volatilizees in solidification, activity dilution
Agent then has larger reactivity to curing agent).
(3) coupling agent：Conductive silver glue shear strength after the bonding force during die bond and solidification is pointed out, is improved using resistance to
Long property, including zirconate, titanate esters, organic complex, silanes etc..
The pattern and granule size of super fine silver powder are strictly influenceed by production technology.Generally, in solution
Single step synthetic reaction, faster reaction rate can generate more nucleus in nucleation stage, and the generation of more nucleus result in single
The relatively small and whole nucleation stage of final growth size of particle is relative to be shortened, and typically favors generation size smaller and uniform
The nano-particle of distribution.Comparatively speaking, slower reaction then advantageously reduces the formation of defect in crystal growth, thus based on anti-
Influence of the speed to the nano-particles size of generation is answered, can be big to regulate and control the size of particle by the control to reaction rate
It is small.
Prior art also discloses that by plant extraction liquid to prepare the technique of nano silver particles, but be not directed to also into
One step high-power LED encapsulation angle set out research super fine silver powder research.Someone is by using two kinds or two or more plants
Thing extract solution, finds under sweet orange bark extract and Lotus Leafextract collective effect, can reach certain synergy, can produce
Particle diameter is small, narrow distribution range, and form is in the nano silver particles of regular cube shape.
Stalk, Gu claims ligusticumic, and also known as straw is careless, refers to remaining after the ripe threshing of the gramineae farm crops such as paddy rice, wheat, corn
Cauline leaf part, the stalk of wherein paddy rice is commonly referred to as straw, rice ligusticumic, and the stalk of wheat is then referred to as straw.Before industrialization,
Utilization of the peasant to stalk is multifarious, enriches very much.Such as in southern china, rice straw is dried storage by people, can be used as bavin
Fire, weaves the household wares such as seat cushion, mattress, broom, and place mat domestic animal circle, pasture, heap make compost returning to the field, or even for making makeshift house
The roof in room etc., is seldom directly slatterned.China is in the late two decades due to coal, electricity, the popularizing of natural gas, various industrial products
It is abundant, rural area reduced to the demand of stalk, and a large amount of stalks are processed into for a serious social concern, although law is prohibited
Only, but many local peasants still direct burning straw in the fields, trigger air pollution, fire, aircraft can not Normal Take-Off And Landing
Etc. consequence.The inventors discovered that, wheat stalk has special effect to the pattern particle diameter for controlling Nano Silver.
The present invention is prepared from the environmental protection of super fine silver powder to start with, and has prepared the super of suitable production LED encapsulation conductive silver glues
Thin silver powder, and it has further been discovered that in specific silver powder particle diameter, form, with reference to specific epoxy resin, curing agent, accelerator
Under the other compositions such as coupling agent, it easy can prepare that thermal conductivity factor is high, shear strength is big at low cost, high-temp resisting high-humidity resisting
The LED encapsulation conductive silver glues of function admirable, it is applicable to high-power LED encapsulation.Especially, in a preferred embodiment
In, the present invention prepares the solid type Nano Silver of rule, and it especially has excellent performance.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of high-power LED encapsulation conductive silver glue, it is prepared via a method which to obtain：
(1) silver powder is prepared：
Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Wheat stalk is taken, amount of water is 10 times of wheat stalk, 80 DEG C of holding heating extraction 5-6 hours, normal temperature after filter residue
Save backup；
1 times of weight sweet orange peel extract solution is taken, 1 times of weight pomelo peel extract solution, 0.5-0.8 times of weight wheat stalk is extracted
Liquid, is mixed with the 0.3mM of 15-18 times of weight silver nitrate solution, and the pH value of regulation silver nitrate solution is 9.0,65 DEG C of reactions
20-25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea two
5-8 parts of phenylmethane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 2- ethyls -0.7 part of 4-methylimidazole；
Aforementioned proportion raw material is mixed, matrix polymer is stirred and be uniformly dispersed and to obtain；
(3) conducting resinl is prepared：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation is with leading
Electric elargol.
The present invention is advantageous in that：
(1) present invention is raw material using biological waste, and natural environmental-protective cost is low.
(2) preparation method for the LED encapsulation conductive silver glues that the present invention is provided is simple, it is only necessary to which one-step method can just be prepared
Required silver powder, it is with low cost, there are very much market prospects.
(3) LED encapsulation produced by the present invention is big with conductive silver glue shear strength, high temperature resistant storage, the property of high-temp resisting high-humidity resisting
The excellent LED encapsulation conductive silver glues of energy, are highly suitable for high-power LED encapsulation.
Brief description of the drawings
Fig. 1 is the typical nanoscale silver figure of Examples 1 and 2.
Fig. 2 is the typical nanoscale silver figure of embodiment 3.
Embodiment
Embodiment 1：
A kind of high-power LED encapsulation conductive silver glue, it is prepared via a method which to obtain：
(1) silver powder is prepared：
Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Wheat stalk is taken, amount of water is 10 times of wheat stalk, 80 DEG C of holding heating extraction 5-6 hours, normal temperature after filter residue
Save backup；
1 times of weight sweet orange peel extract solution is taken, 1 times of weight pomelo peel extract solution, 0.5-0.8 times of weight wheat stalk is extracted
Liquid, is mixed with the 0.3mM of 15-18 times of weight silver nitrate solution, and the pH value of regulation silver nitrate solution is 9.0,65 DEG C of reactions
20-25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea two
5-8 parts of phenylmethane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 2- ethyls -0.7 part of 4-methylimidazole；
Aforementioned proportion raw material is mixed, matrix polymer is stirred and be uniformly dispersed and to obtain；
(3) conducting resinl is prepared：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation is with leading
Electric elargol.
The present embodiment prepares morphology controllable, and regular spherical, the extra small Nano Silver of particle diameter, typical shape appearance figure is as shown in Figure 1.
Embodiment 2：
A kind of high-power LED encapsulation conductive silver glue, it is prepared via a method which to obtain：
(1) silver powder is prepared：
Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Wheat stalk is taken, amount of water is 10 times of wheat stalk, 80 DEG C of holding heating extraction 5-6 hours, normal temperature after filter residue
Save backup；
1 times of weight sweet orange peel extract solution is taken, 1 times of weight pomelo peel extract solution, 0.5-0.8 times of weight wheat stalk is extracted
Liquid, is mixed with the 0.3mM of 15-18 times of weight silver nitrate solution, and the pH value of regulation silver nitrate solution is 9.0,65 DEG C of reactions
20-25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea two
5-8 parts of phenylmethane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 2- ethyls -0.7 part of 4-methylimidazole；
Aforementioned proportion raw material is mixed, matrix polymer is stirred and be uniformly dispersed and to obtain；
(3) conducting resinl is prepared：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation is with leading
Electric elargol.
The present embodiment prepares morphology controllable, and regular spherical, the extra small Nano Silver of particle diameter, typical shape appearance figure is as shown in Figure 1.
Embodiment 3：
A kind of high-power LED encapsulation conductive silver glue, it is prepared via a method which to obtain：
(1) silver powder is prepared：
Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Wheat stalk is taken, amount of water is 10 times of wheat stalk, 80 DEG C of holding heating extraction 5-6 hours, normal temperature after filter residue
Save backup；
1 times of weight sweet orange peel extract solution is taken, 1 times of weight pomelo peel extract solution, 0.5-0.8 times of weight wheat stalk is extracted
Liquid, is mixed with the 0.3mM of 15-18 times of weight silver nitrate solution, and the pH value of regulation silver nitrate solution is 9.0,65 DEG C of reactions
20-25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea two
5-8 parts of phenylmethane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 2- ethyls -0.7 part of 4-methylimidazole；
Aforementioned proportion raw material is mixed, matrix polymer is stirred and be uniformly dispersed and to obtain；
(3) conducting resinl is prepared：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation is with leading
Electric elargol.
The present embodiment prepares morphology controllable, complicated solid type, the less Nano Silver of particle diameter, typical shape appearance figure such as Fig. 2 institutes
Show.
Embodiment 4：
Verify the effect of wheat stalk：
A kind of high-power LED encapsulation conductive silver glue, it is prepared via a method which to obtain：
(1) silver powder is prepared：
Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Take 1 times of weight sweet orange peel extract solution, 1 times of weight pomelo peel extract solution, the nitric acid with 0.3 mM of 15-18 times of weight
Silver-colored solution mixing, the pH value of regulation silver nitrate solution is 9.0,65 DEG C of reaction 20-25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea two
5-8 parts of phenylmethane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 2- ethyls -0.7 part of 4-methylimidazole；
Aforementioned proportion raw material is mixed, matrix polymer is stirred and be uniformly dispersed and to obtain；
(3) conducting resinl is prepared：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation is with leading
Electric elargol.
Embodiment 5：
Wheat stalk is substituted with maize straw：
A kind of high-power LED encapsulation conductive silver glue, it is prepared via a method which to obtain：
(1) silver powder is prepared：
Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Maize straw is taken, amount of water is 10 times of maize straw, 80 DEG C of holding heating extraction 5-6 hours, normal temperature after filter residue
Save backup；
1 times of weight sweet orange peel extract solution is taken, 1 times of weight pomelo peel extract solution, 0.5-0.8 times of weight maize straw is extracted
Liquid, is mixed with the 0.3mM of 15-18 times of weight silver nitrate solution, and the pH value of regulation silver nitrate solution is 9.0,65 DEG C of reactions
20-25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea two
5-8 parts of phenylmethane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 2- ethyls -0.7 part of 4-methylimidazole；
Aforementioned proportion raw material is mixed, matrix polymer is stirred and be uniformly dispersed and to obtain；
(3) conducting resinl is prepared：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation is with leading
Electric elargol.
Embodiment 6：
The inventors discovered that, the ratio of three kinds of plant extracts is also extremely important, and ratio is not right, also can prepare Chu Lai the present invention
Silver powder.
Record comparative example demonstration：
A kind of high-power LED encapsulation conductive silver glue, it is prepared via a method which to obtain：
(1) silver powder is prepared：
Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Wheat stalk is taken, amount of water is 10 times of wheat stalk, 80 DEG C of holding heating extraction 5-6 hours, normal temperature after filter residue
Save backup；
Take 2 times of weight sweet orange peel extract solutions, 1 times of weight pomelo peel extract solution, 1 times of weight wheat stalk extract solution, with 15-
The 0.3mM of 18 times of weight silver nitrate solution mixing, the pH value of regulation silver nitrate solution is 9.0,65 DEG C of reaction 20-25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea two
5-8 parts of phenylmethane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 2- ethyls -0.7 part of 4-methylimidazole；
Aforementioned proportion raw material is mixed, matrix polymer is stirred and be uniformly dispersed and to obtain；
(3) conducting resinl is prepared：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation is with leading
Electric elargol.
The LED encapsulation prepared to embodiment 1-6 is further tested with conductive silver glue.
The silver powder obtained to embodiment 1-6 carries out the sign of form.
Transmission electron microscope (TEM) is characterized, as a result as shown in table 1.
Table 1
It can be seen that, silver powder particle diameter produced by the present invention is small, form rule, is distributed very narrow.
Resistance to heat-storage test：The high-temperature storage performance of conductive silver glue is the heat resistance for simulating LED in actual application
Can, conductive silver glue sample is fabricated to specific insulation test sample and shear strength test sample, sample is store at 150 DEG C
Hide 1000h；
Heat-resisting moisture-proof test：Conductive silver glue sample is fabricated to specific insulation test sample and shear strength test examination
Sample, sample is placed in high-low temperature tester, and 1000h is preserved under the conditions of 85 DEG C and 85%RH, its specific insulation and shearing
Strength Changes.
Embodiment 1-6 experimental result and the resistance to heat-storage of the present embodiment, heat-resisting moisture-proof test result is as shown in table 2：-5
Table 2
As can be seen here, conductive silver glue heat conductivility produced by the present invention is very good, good heat dissipation, and especially embodiment 3 is vertical
Build Nano Silver thermal conductivity factor is very high, rapid heat dissipation, it is adaptable to high-power encapsulation；In addition, volume resistance is small, shear strength is big,
Resistance to heat-storage, heat-resisting moisture-proof, performance is very excellent.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (3)
1. a kind of preparation method of high-power LED encapsulation conductive silver glue, its step is as follows：
（1）Prepare silver powder：
Fresh sweet orange peel is taken to be squeezed into juice, 4 DEG C save backup；
Fresh grapefruit skin is taken to be squeezed into juice, 4 DEG C save backup；
Wheat stalk is taken, is added water, 80 DEG C of holding heating extraction 5-6 hours, normal temperature is saved backup after filter residue；
Sweet orange peel extract solution is taken, pomelo peel extract solution, wheat stalk extract solution is mixed with 0.3mM silver nitrate solution, adjusted
It is 9.0,65 DEG C of reaction 20-25min to save the pH values of silver nitrate solution；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally；
(2) matrix polymer is configured：
Configured according to following parts by weight：60-80 parts of bisphenol F epoxy resin, 0.4 part of phenyl silicone, diaminourea hexichol first
5-8 parts of alkane, 5-6 parts of diaminodiphenyl ether, 6 parts of phenyl vinyl MQ silicone resin, 0.7 part of 2-ethyl-4-methylimidazole；Will be above-mentioned
Ratio raw material is mixed, and stirs and be uniformly dispersed and to obtain matrix polymer；
（3）Prepare conducting resinl：
Configured according to following parts by weight：22 parts of matrix polymer, 80-90 parts of silver powder, mixing composition LED encapsulation conductive silvers
Glue.
2. the preparation method of the LED encapsulation conductive silver glues described in claim 1, it is characterised in that：
Step（1）For：Fresh sweet orange peel is taken, amount of water is 4 times of sweet orange peel weight and is squeezed into juice, and 4 DEG C save backup；
Fresh grapefruit skin is taken, amount of water is 3 times of shaddock weight and is squeezed into juice, and 4 DEG C save backup；
Wheat stalk is taken, amount of water is 10 times of wheat stalk, 80 DEG C of holding heating extraction 5-6 hours, normal temperature preservation after filter residue
It is standby；
Take 1 times of weight sweet orange peel extract solution, 1 times of weight pomelo peel extract solution, 0.5-0.8 times of weight wheat stalk extract solution, with
The 0.3mM of 15-18 times of weight silver nitrate solution mixing, the pH values of regulation silver nitrate solution are 9.0,65 DEG C of reaction 20-
25min；
Centrifuged after reaction, add ethanol, acetone cyclic washing product, sample dries naturally.
3. the conductive silver glue that the preparation method described in claim 1-2 is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710459698.7A CN107227130B (en) | 2017-06-16 | 2017-06-16 | A kind of high-power LED encapsulation conductive silver glue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710459698.7A CN107227130B (en) | 2017-06-16 | 2017-06-16 | A kind of high-power LED encapsulation conductive silver glue |
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| Publication Number | Publication Date |
|---|---|
| CN107227130A true CN107227130A (en) | 2017-10-03 |
| CN107227130B CN107227130B (en) | 2019-03-12 |
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ID=59936107
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| CN201710459698.7A Active CN107227130B (en) | 2017-06-16 | 2017-06-16 | A kind of high-power LED encapsulation conductive silver glue |
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| CN113265210A (en) * | 2021-05-17 | 2021-08-17 | 北京中天鹏宇科技发展有限公司 | Adhesive with high electric and heat conductivity and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104889418A (en) * | 2015-05-18 | 2015-09-09 | 湖州品创孵化器有限公司 | Biological synthesis method of cubic nanometer silver particles |
| CN104893634A (en) * | 2015-04-10 | 2015-09-09 | 浙江安吉成新照明电器有限公司 | Conductive silver adhesive with excellent performance used for LED packaging |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104893634A (en) * | 2015-04-10 | 2015-09-09 | 浙江安吉成新照明电器有限公司 | Conductive silver adhesive with excellent performance used for LED packaging |
| CN104889418A (en) * | 2015-05-18 | 2015-09-09 | 湖州品创孵化器有限公司 | Biological synthesis method of cubic nanometer silver particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113265210A (en) * | 2021-05-17 | 2021-08-17 | 北京中天鹏宇科技发展有限公司 | Adhesive with high electric and heat conductivity and preparation method thereof |
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