CN107739587A - A kind of LED crystal-bonding adhesives of graphene-containing and preparation method thereof - Google Patents
A kind of LED crystal-bonding adhesives of graphene-containing and preparation method thereof Download PDFInfo
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- CN107739587A CN107739587A CN201710842232.5A CN201710842232A CN107739587A CN 107739587 A CN107739587 A CN 107739587A CN 201710842232 A CN201710842232 A CN 201710842232A CN 107739587 A CN107739587 A CN 107739587A
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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
- 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
- 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
- C08K3/04—Carbon
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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
- C08K3/28—Nitrogen-containing compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of LED crystal-bonding adhesives of graphene-containing, including following component by weight：40 60 parts of modified graphene, 15 35 parts of AlN powder, 15 25 parts of epoxy resin, 15 parts of diluent, 0.5 1 parts of coupling agent, 0.5 5 parts of curing agent.The invention also discloses the preparation method of the LED crystal-bonding adhesives of above-mentioned graphene-containing.The LED crystal-bonding adhesives of the present invention, heat resistance and good heat conductivity, can effectively improve the reliability and service life of LED.
Description
Technical field
The present invention relates to LED heat boundary material field, and in particular to a kind of LED crystal-bonding adhesives of graphene-containing and its preparation
Method.
Background technology
It is well known that LED semiconductor die packages use into light source and as light fixture, if can not effectively process chip collection
Poly- heat, thing followed fuel factor will cause light source junction temperature to raise, lifetime, and directly reduce chip outgoing
Photon, reduce light extraction efficiency.Moreover, the rise of temperature can also make the emission spectrum of chip that red shift occur, and make quality of colour
Decline, especially even more serious to the white light LED part based on blue LED excited yellow fluorescent material, the wherein conversion of fluorescent material
Efficiency can also reduce as temperature raises.Meanwhile in the course of the work because the repetition of chip is generated heat, power model can be continuous
The effect of thermal cycling loads is undergone, because the thermal coefficient of expansion (CTE) of different materials mismatches, interlayer thermal stress can be produced, and
Warpage, stripping, crackle can occur over time, or even produce failure and dead lamp, this is also to cause LED light source finally to lose
One main cause of effect.Therefore, because temperature rise and the party of caused various fuel factor collection seriously affects the LED light source longevity
The performance of life and light fixture.
LED crystal-bonding adhesives are used widely because of can effectively drop the interface resistance between chip and support, wherein elargol
It is exactly crystal-bonding adhesive the most commonly used in market with insulating cement.Crystal-bonding adhesive is for filling LED chip and support as heat-conducting medium
Between space material, by heat energy by crystal-bonding adhesive, support, three big passage of heat of heat-conducting silicone grease, and radiator, allow thermal source to produce
Raw heat energy is constantly dispersed into air by radiator radiation and convection, and LED chip heat source temperature is maintained at one can be with
The level of steady operation, extend LED service life, prevent LED because passage of heat is obstructed and caused by life problems.
The content of the invention
It is an object of the invention to provide a kind of LED crystal-bonding adhesives of graphene-containing, LED crystal-bonding adhesives of the invention, heat resistance
Energy and good heat conductivity, can effectively improve the reliability and service life of LED.
To realize above-mentioned technical purpose and the technique effect, the present invention is achieved through the following technical solutions：
A kind of LED crystal-bonding adhesives of graphene-containing, including following component by weight：Modified graphene 40-60 parts,
AlN powder 15-35 parts, epoxy resin 15-25 parts, diluent 1-5 parts, coupling agent 0.5-1 parts, curing agent 0.5-5 parts.
Further, the modified graphene is prepared through following steps：Titanate coupling agent TMC-TTS is dilute
Release in DMF, then graphene is added in coupling agent dilution, in 4000-6000r/min rotating speeds
Under be sufficiently mixed 20-30min, be then dried in vacuo 5-6h at 70-80 DEG C, obtain the modified graphene.
Further, the epoxy resin is bisphenol-f type, bisphenol A-type, aliphatic epoxy resin, aliphatic glycidyl
One or more blends in ether type epoxy resins.
Further, the diluent is that butyl glycidyl ether, BDDE, ethylene glycol two contract
One or more in water glycerin ether, polypropylene glycol diglycidyl ether, C12-14 fatty glycidyl ethers.
Further, the coupling agent is Silane coupling agent KH550, silane coupler KH560, silane coupler KH570
Or aluminate coupling agent.
Further, the curing agent is amine curing agent, acid anhydride type curing agent or aromatics curing agent.
The invention also discloses the preparation method of the LED crystal-bonding adhesives of above-mentioned graphene-containing, comprise the following steps：
1) each component is weighed by the formula of the LED crystal-bonding adhesives of above-mentioned graphene-containing；
2) the AlN powder weighed is taken, is added in DMF, stirs, then ultrasonic vibration processing
30-60min；Then after absolute ethyl alcohol washs, 1-2h is dried in vacuo at 40-60 DEG C again for centrifugal filtration, obtained powder；
3) the AlN powder after step 2) of learning from else's experience processing, is stirred together with modified graphene, epoxy resin and other additives
Mix, until then mixture is carried out vacuumizing degassing process to mixture, produced of the present invention solid in the paste body shape of flowing
Brilliant glue.
The beneficial effects of the invention are as follows:
The crystal-bonding adhesive of the graphene-containing of the present invention, using the excellent graphene of thermal conductivity and AlN powder as crystal-bonding adhesive
Packing material, and graphene is modified, and AlN powder is pre-processed so that graphene and AlN powder are in epoxy
It is well dispersed in resin matrix, and graphene and AlN powder properties are sufficiently stable, greatly improve the capacity of heat transmission of crystal-bonding adhesive；
Secondly, the heat resistance and good insulation preformance of graphene and AlN powder, the service life of crystal-bonding adhesive is improved.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, described in detail below with presently preferred embodiments of the present invention as after.The tool of the present invention
Body embodiment is shown in detail by following examples.
Embodiment
Below in conjunction with following examples of the present invention, technical scheme is clearly and completely described, shown
So, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on the reality in the present invention
Example is applied, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, is all belonged to
In the scope of protection of the invention.
Embodiment 1
A kind of LED crystal-bonding adhesives of graphene-containing, it is formulated and corresponding constituent content is as shown in table 1.Wherein, asphalt mixtures modified by epoxy resin
Fat is bisphenol f type epoxy resin, and diluent is butyl glycidyl ether, and coupling agent is Silane coupling agent KH550, the curing agent
For fatty amine；
Modified graphene is prepared through following steps：5g titanate coupling agents TMC-TTS is diluted in 50mL's
In DMF, then 10g graphenes are added in coupling agent dilution, under 4000r/min rotating speeds fully
30min is mixed, then 6h is dried in vacuo at 80 DEG C, obtains modified graphene.
The crystal-bonding adhesive is prepared through following steps：
1) each component is weighed according to the formula of embodiment 1 in table 1；
2) the AlN powder weighed is taken, is added in 50mL DMF, magnetic agitation 1h is equal to being formed
One solution, then ultrasonic vibration processing 60min；Then solution is added to centrifugal filtration in centrifuge, obtained AlN powder is again
After absolute ethyl alcohol washs, 2h is dried in vacuo at 60 DEG C, the AlN powder pre-processed, its average grain diameter is 20-50 μm；
3) by the AlN powder of pretreatment, stirring is added to together with modified graphene, epoxy resin and other additives
Stirred in machine, until then mixture carries out vacuumizing degassing process to mixture, produce institute of the present invention in the paste body shape of flowing
The crystal-bonding adhesive stated.
Embodiment 2
A kind of LED crystal-bonding adhesives of graphene-containing, it is formulated and corresponding constituent content is as shown in table 1.Wherein, asphalt mixtures modified by epoxy resin
Fat is aliphatic epoxy resin, and diluent is BDDE, and coupling agent is silane coupler KH560, institute
It is phthalic anhydride to state curing agent；
Modified graphene is prepared through following steps：5g titanate coupling agents TMC-TTS is diluted in 50mL's
In DMF, then 10g graphenes are added in coupling agent dilution, under 5000r/min rotating speeds fully
20min is mixed, then 5h is dried in vacuo at 70 DEG C, obtains modified graphene.
The crystal-bonding adhesive is prepared through following steps：
1) each component is weighed according to the formula of embodiment 2 in table 1；
2) the AlN powder weighed is taken, is added in 50mL DMF, magnetic agitation 1h is equal to being formed
One solution, then ultrasonic vibration processing 40min；Then solution is added to centrifugal filtration in centrifuge, obtained AlN powder is again
After absolute ethyl alcohol washs, 1h is dried in vacuo at 60 DEG C, the AlN powder pre-processed, its average grain diameter is 20-50 μm；
3) by the AlN powder of pretreatment, stirring is added to together with modified graphene, epoxy resin and other additives
Stirred in machine, until then mixture carries out vacuumizing degassing process to mixture, produce institute of the present invention in the paste body shape of flowing
The crystal-bonding adhesive stated.
Embodiment 3
A kind of LED crystal-bonding adhesives of graphene-containing, it is formulated and corresponding constituent content is as shown in table 1.Wherein, asphalt mixtures modified by epoxy resin
Fat is bisphenol A type epoxy resin, and diluent is polypropylene glycol diglycidyl ether, and coupling agent is coupled for silane coupler Aluminate
Agent, the curing agent are diethyl toluene diamine；
Modified graphene is prepared through following steps：5g titanate coupling agents TMC-TTS is diluted in 50mL's
In DMF, then 10g graphenes are added in coupling agent dilution, under 6000r/min rotating speeds fully
20min is mixed, then 5h is dried in vacuo at 80 DEG C, obtains modified graphene.
The crystal-bonding adhesive is prepared through following steps：
1) each component is weighed according to the formula of embodiment 3 in table 1；
2) the AlN powder weighed is taken, is added in 50mL DMF, magnetic agitation 1h is equal to being formed
One solution, then ultrasonic vibration processing 60min；Then solution is added to centrifugal filtration in centrifuge, obtained AlN powder is again
After absolute ethyl alcohol washs, 1h is dried in vacuo at 50 DEG C, the AlN powder pre-processed, its average grain diameter is 20-50 μm；
3) by the AlN powder of pretreatment, stirring is added to together with modified graphene, epoxy resin and other additives
Stirred in machine, until then mixture carries out vacuumizing degassing process to mixture, produce institute of the present invention in the paste body shape of flowing
The crystal-bonding adhesive stated.
Comparative example 1
A kind of LED crystal-bonding adhesives, it is formulated and corresponding constituent content is as shown in table 1.Wherein, epoxy resin is bisphenol-f type
Epoxy resin, diluent are butyl glycidyl ether, and coupling agent is Silane coupling agent KH550, and the curing agent is fatty amine；
The crystal-bonding adhesive is prepared through following steps：
1) each component is weighed according to the formula of comparative example 1 in table 1；
2) the Ag powder weighed is taken, is added in 50mL DMF, magnetic agitation 1h is homogeneous to being formed
Solution, then ultrasonic vibration processing 60min；Then solution is added to centrifugal filtration in centrifuge, obtained Ag powder is again through nothing
After water-ethanol washing, 2h is dried in vacuo at 60 DEG C, the Ag powder pre-processed；
3) by the Ag powder of pretreatment, it is added in mixer and stirs together with epoxy resin and other additives, until
Then mixture carries out vacuumizing degassing process to mixture, produces crystal-bonding adhesive of the present invention in the paste body shape of flowing.
Comparative example 2
A kind of LED crystal-bonding adhesives of graphene-containing, it is formulated and corresponding constituent content is as shown in table 1.Wherein, asphalt mixtures modified by epoxy resin
Fat is bisphenol f type epoxy resin, and diluent is butyl glycidyl ether, and coupling agent is Silane coupling agent KH550, the curing agent
For fatty amine；
Modified graphene is prepared through following steps：5g titanate coupling agents TMC-TTS is diluted in 50mL's
In DMF, then 10g graphenes are added in coupling agent dilution, under 4000r/min rotating speeds fully
30min is mixed, then 6h is dried in vacuo at 80 DEG C, obtains modified graphene.
The crystal-bonding adhesive is prepared through following steps：
1) each component is weighed according to the formula of comparative example 2 in table 1；
2) modified graphene is added in mixer together with epoxy resin and other additives and stirred, until mixing
Then thing carries out vacuumizing degassing process to mixture, produces crystal-bonding adhesive of the present invention in the paste body shape of flowing.
The formula table of the crystal-bonding adhesive of the embodiment of table 1 and comparative example
Performance detection：
The crystal-bonding adhesive that Example 1-3 and comparative example 1-2 are prepared, according to ATM-0052 standard detection crystal-bonding adhesive
Shear strength, it is as shown in table 2 according to the thermal conductivity factor of ASTM D5470 standard testing crystal-bonding adhesive, acquired results.
The shear strength and thermal conductivity factor of the embodiment of table 2 and comparative example
Table 2 is referred to, crystal-bonding adhesive prepared by embodiment 1-3, its shear strength is up to more than 15MPa, higher than comparative example 1
With comparative example 2.Thermal conductivity factor is all higher than 100W/MK, hence it is evident that higher than comparative example 1 (using traditional Ag powder as packing material)
With the sample of comparative example 2 (using graphene as packing material).The encapsulation of great power LED electronics device in being adapted to.Comparative example 2
In merely using graphene as packing material, but graphene is dispersed poor, easy reunion, especially in too high levels
In the case of, it is scattered uneven in the epoxy, it have impact on the overall thermal conductivity factor of crystal-bonding adhesive and shear strength.The present invention is in ring
Reduce the dosage of graphene in epoxy resin-based body, introduce the AlN powder of certain content, AlN powder has well heat-resisting
Property and high heat conductance, after pretreatment, dispersiveness is better than graphene, thus be favorably improved crystal-bonding adhesive thermal conductivity factor and
Shear strength.
The crystal-bonding adhesive of the graphene-containing of the present invention, has good thermal conductivity factor, heat resistance and service life, can replace passing
The crystal-bonding adhesive of system.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (7)
1. the LED crystal-bonding adhesives of a kind of graphene-containing, it is characterised in that including following component by weight：Modified graphene
40-60 parts, AlN powder 15-35 parts, epoxy resin 15-25 parts, diluent 1-5 parts, coupling agent 0.5-1 parts, curing agent 0.5-5
Part.
2. the LED crystal-bonding adhesives of graphene-containing as claimed in claim 1, it is characterised in that the modified graphene is through as follows
What step was prepared：Titanate coupling agent TMC-TTS is diluted in DMF, then added graphene
Into coupling agent dilution, 20-30min is sufficiently mixed under 4000-6000r/min rotating speeds, then vacuum is done at 70-80 DEG C
Dry 5-6h, obtain the modified graphene.
3. the LED crystal-bonding adhesives of graphene-containing as claimed in claim 1, it is characterised in that the epoxy resin be bisphenol-f type,
One or more blends in bisphenol A-type, aliphatic epoxy resin, aliphatic glycidyl ether based epoxy resin.
4. the LED crystal-bonding adhesives of graphene-containing as claimed in claim 1, it is characterised in that the diluent is that butyl shrink is sweet
Oily ether, 1,4- butanediol diglycidyl ethers, ethylene glycol diglycidylether, polypropylene glycol diglycidyl ether, C12-14 fat
One or more in fat glycidol ether.
5. the LED crystal-bonding adhesives of graphene-containing as claimed in claim 1, it is characterised in that the coupling agent is silane coupler
KH550, silane coupler KH560, silane coupler KH570 or aluminate coupling agent.
6. the LED crystal-bonding adhesives of graphene-containing as claimed in claim 1, it is characterised in that the curing agent be amine curing agent,
Acid anhydride type curing agent or aromatics curing agent.
7. the preparation method of the LED crystal-bonding adhesives of a kind of graphene-containing, it is characterised in that comprise the following steps：
1) each component is weighed by the formula of the LED crystal-bonding adhesives of any one of claim 1-6 graphene-containing；
2) the AlN powder weighed is taken, is added in DMF, stirs, then ultrasonic vibration processing 30-
60min；Then after absolute ethyl alcohol washs, 1-2h is dried in vacuo at 40-60 DEG C again for centrifugal filtration, obtained powder；
3) the AlN powder after step 2) of learning from else's experience processing, is stirred together with modified graphene, epoxy resin and other additives,
Until then mixture carries out vacuumizing degassing process to mixture, produces die bond of the present invention in the paste body shape of flowing
Glue.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710842232.5A CN107739587A (en) | 2017-09-18 | 2017-09-18 | A kind of LED crystal-bonding adhesives of graphene-containing and preparation method thereof |
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| CN201710842232.5A CN107739587A (en) | 2017-09-18 | 2017-09-18 | A kind of LED crystal-bonding adhesives of graphene-containing and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135659A (en) * | 2018-08-08 | 2019-01-04 | 无锡帝科电子材料股份有限公司 | A kind of LED crystal-bonding adhesive and production method |
| CN112322149A (en) * | 2020-09-22 | 2021-02-05 | 广东杰果新材料有限公司 | Glue for red light LED lamp and preparation method thereof |
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| CN107142062A (en) * | 2017-05-25 | 2017-09-08 | 钱龙风 | A kind of high-efficiency heat conduction glue |
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| CN104017537A (en) * | 2014-06-26 | 2014-09-03 | 轻工业部南京电光源材料科学研究所 | Heat-conducting adhesive for LED (light-emitting diode) lamp packaging and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109135659A (en) * | 2018-08-08 | 2019-01-04 | 无锡帝科电子材料股份有限公司 | A kind of LED crystal-bonding adhesive and production method |
| CN112322149A (en) * | 2020-09-22 | 2021-02-05 | 广东杰果新材料有限公司 | Glue for red light LED lamp and preparation method thereof |
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