CN104087216B - For the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer - Google Patents
For the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer Download PDFInfo
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- CN104087216B CN104087216B CN201410340705.8A CN201410340705A CN104087216B CN 104087216 B CN104087216 B CN 104087216B CN 201410340705 A CN201410340705 A CN 201410340705A CN 104087216 B CN104087216 B CN 104087216B
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Abstract
For the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, take the acrylic ester monomer of a certain amount of various structures and insulation Graphene, adopt monomer copolymerization grafting synthetic method, insulation Graphene is introduced in acrylic ester monomer polymerization process, obtain the polymer of high molecular, make the composite base-material containing insulation Graphene heat radiation bonding copolymer resins, composite base-material is used for the heat radiation bonding between LED aluminum base plate and scatterer.The thermal conductivity that the present invention is easy to change, not high under having extraordinary bonding intensity and weathering characteristics, high temperature and short wavelength light photograph, there is the new-type encapsulation tackiness agent of low thermal resistance, good heat radiating ability and low mechanical stress, be applicable to heat radiation bonding between high-power LED aluminum substrate and scatterer, greatly can improve the life-span of LED, be the heat radiation tackiness agent of a kind of environmental protection, low consumption, low-temperature curing.
Description
Technical field
The present invention relates to a kind of making method for the tackiness agent that dispels the heat between LED aluminum base plate and scatterer.
Background technology
LED illumination product due to energy conversion efficiency very high, energy consumption only has 10% of incandescent light in theory, compare luminescent lamp, the energy-saving effect of 50% can be reached, thus there is energy-saving and environmental protection and long-life advantage, can be widely used in the lighting fields such as Landscape Lighting, safety lighting, special lighting and normal illumination sources, market potential is huge.
Generally, it is 0.2 ~ 0.3nm/ DEG C that the emission wavelength of LED varies with temperature, and spectral width increases thereupon, affects bright-colored degree.In addition, when forward current flows through pn knot, when heat generation loss makes interface produce temperature rise, at near room temperature, temperature often raises 1 DEG C, the reason that the luminous intensity of LED correspondingly can reduce about 1%, LED heating is because added electric energy is not all converted into luminous energy, but a part transforms into heat energy.The light efficiency of LED only has 100lm/W at present, and its electro-optical efficiency approximately only about 20 ~ 30%, that is the electric energy of about 70% all becomes heat energy.Therefore, the core breakthrough point affecting high-power LED illumination is heat dissipation technology.
All aluminium base is have employed in almost most LED lamp.Below aluminium base, one deck isolator then requires that its insulating property are fine, but also wants heat conductivility fine.But these two performances are contradiction, be all the good heat conductivity of conductor usually, and the heat conductivility of isolator are poor.Not only met thermal conductivity well simultaneously but also good insulating be difficult to accomplish.
Select suitable chip substrate adhesion material, and in mass production processes, ensure that adhesive thickness is as far as possible little, this is very important to the thermal conductance characteristic of guarantee device.Usually select heat-conducting glue, conductivity type silver slurry and tin to starch these 3 kinds of materials to adhere to.Though heat-conducting glue has the packaged material of lower stiffening temperature LED component, there are excellent electrical insulation capability, adherence and dielectric properties, but epoxy resin has water absorbability, easily aging, poor heat resistance, high temperature and short wavelength light according to lower easy to change, and have certain toxicity before curing, therefore impact the life-span of LED component.Nowadays many LED dealers find and replace epoxy resin as packaged material, to improve the life-span of LED.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art and the making method for the tackiness agent that dispels the heat between LED aluminum base plate and scatterer that a kind of reliability is high, radiating efficiency is high is provided, make LED aluminum base plate not only meet thermal conductivity well simultaneously but also good insulating, and greatly improve the life-span of LED.
Technical scheme of the present invention is: a kind of making method for the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, take the acrylic ester monomer of a certain amount of various structures and insulation Graphene, adopt monomer copolymerization grafting synthetic method, insulation Graphene is introduced in acrylic ester monomer polymerization process, obtain the polymer of high molecular, make the composite base-material containing insulation Graphene heat radiation bonding copolymer resins, composite base-material is used for the heat radiation bonding between LED aluminum base plate and scatterer.
Further, the acrylic ester monomer of described various structures forms by more than three in methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl acrylate, Octyl acrylate, butyl methacrylate, vinylformic acid, N hydroxymethyl acrylamide, acrylamide monomer kind.
Further, described insulation Graphene is single-layer sheet or multilayer tablet, and the thickness of described single-layer sheet is 0.33nm, and length is 3 ~ 5um.
Further, the composition of described insulation Graphene heat radiation bonding copolymer resins and the per-cent accounting for monomer total amount are: the monomer total amounts of more than three kinds compositions in described methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl acrylate, Octyl acrylate, butyl methacrylate, vinylformic acid, N hydroxymethyl acrylamide, acrylamide monomer are 100%, initiator 0.25 ~ 0.55%(preferably 0.30 ~ 0.45%), ethanol 200 ~ 650%(preferably 300 ~ 450%), insulation Graphene 5 ~ 320%(preferably 180 ~ 280%).
Further, the insulation Graphene heat radiation bonding copolymer resins that described employing monomer copolymerization grafting synthetic method is made, comprises the following steps:
A. taking ethanol total amount 3/4 for dissolving N hydroxymethyl acrylamide and acrylamide compound monomer, being added in ethanol while stirring and fully dissolving; Add the insulation Graphene of whole consumption 50% subsequently while stirring, dispersed and fully stir 1.5 hours;
B. take all the other monomers and the insulation Graphene of residue 50% consumption is added in mix monomer while stirring, dissolving in 3/5 of initiator total amount wherein, dispersed and fully stir 2.5 hours;
C. step a is mixed with each half of two kinds of solution of step b, be added in copolymerization device, agitator is started in heating, condensing reflux system, when solution temperature to be mixed reaches 75 DEG C ~ 85 DEG C appearance backflows, start timing, under the condition maintaining reflux temperature, two of remaining step a and step b kinds of solution are distinguished section at one time to drip, the period added in 50 ~ 60 minutes;
D. continuing reaction was appended in copolymerization device by remaining 1/4 ethanol and residue 1/5 initiator mixed solution after 3 ~ 5 hours, and the period added in 10 ~ 15 minutes;
E. continue reaction after 1.5 ~ 2.5 hours, stop heated and stirred, when being cooled to 30 DEG C ~ 40 DEG C, discharging can obtain insulation Graphene heat radiation bonding copolymer resins.
Further, the composition and ratio of described composite base-material is: insulation Graphene heat radiation bonding copolymer resins 15 ~ 50%(preferably 30 ~ 40%), vinyl acetic monomer 10 ~ 60%(preferably 18 ~ 30%), ethanol 15 ~ 35%(preferably 20 ~ 30%), butanols 10 ~ 25%(preferably 12 ~ 20%), amido phenolic resin 2 ~ 10%(preferably 5 ~ 8%).
Further, the bake out temperature of described composite base-material is 60 DEG C ~ 120 DEG C (preferably 80 DEG C ~ 100 DEG C), and drying time is 5 ~ 20 minutes (preferably 12 ~ 18 minutes).
The present invention compared with prior art has following features:
(1) insulation Graphene and multiple acrylic ester monomer composite insulation Graphene heat radiation bonding copolymer resins is adopted to replace to dispel the heat between routine LED aluminum base plate and scatterer and bond, utilize the high thermal conductivity coefficient characteristic of single-layer sheet or multilayer tablet insulation Graphene, carry out modification LED aluminum base plate, make LED aluminum base plate not only meet thermal conductivity well simultaneously but also good insulating;
(2) in whole synthesis route, during monomer copolymerization, copolymer resins is grafted to single-layer sheet or multilayer tablet insulation graphenic surface formation monomer copolymerization polymer and Graphene and forms an interpolymer, it is the core of insulation Graphene heat radiation bonding copolymer resins, by regulating acrylic monomer group and copolymerization conditions, the consumption of suitable single-layer sheet or multilayer tablet insulation Graphene, it has extraordinary bonding intensity and weathering characteristics, high temperature and short wavelength light are not easy to change under shining, high thermal conductivity, there is low thermal resistance, the new-type encapsulation tackiness agent of good heat radiating ability and low mechanical stress, be applicable to heat radiation bonding between high-power LED aluminum substrate and scatterer, greatly can improve the life-span of LED, it is a kind of environmental protection, low consumption, the heat radiation tackiness agent of low-temperature curing.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Making method of the present invention is specifically set forth containing single-layer sheet or multilayer tablet insulation Graphene heat radiation bonding copolymer resins below by way of preparation 100kg:
Embodiment 1
One. the composition ratio of insulation Graphene heat radiation bonding copolymer resins
Methyl methacrylate 18.5%
Butyl acrylate 21.5%
β-dimethyl-aminoethylmethacrylate 9.5%
Vinylformic acid 42.0%
Octyl acrylate 3.0%
N hydroxymethyl acrylamide 4.0%
Acrylamide 1.5%
Monomer total amount 100%
Initiator 0.45% (accounting for monomer total amount)
Ethanol 300% (accounting for monomer total amount)
Single-layer sheet insulation Graphene (thickness 0.33nm, length 3um) 280% (accounting for monomer total amount)
Two. copolymerization technique
A. taking ethanol total amount 3/4 for dissolving N hydroxymethyl acrylamide and acrylamide compound monomer, being added in ethanol while stirring and fully dissolving; Add the insulation Graphene of whole consumption 50% subsequently while stirring, dispersed and fully stir 1.5 hours;
B. take all the other monomers and the insulation Graphene of residue 50% consumption is added in mix monomer while stirring, dissolving in 3/5 of initiator total amount wherein, dispersed and fully stir 2.5 hours;
C. step a is mixed with each half of two kinds of solution of step b, be added in copolymerization device, agitator is started in heating, condensing reflux system, when solution temperature to be mixed reaches 75 DEG C ~ 85 DEG C appearance backflows, start timing, under the condition maintaining reflux temperature, two of remaining step a and step b kinds of solution are distinguished section at one time to drip, the period added in 50 ~ 60 minutes;
D. continuing reaction was appended in copolymerization device by remaining 1/4 ethanol and residue 1/5 initiator mixed solution after 3 ~ 5 hours, and the period added in 10 ~ 15 minutes;
E. continue reaction after 1.5 ~ 2.5 hours, stop heated and stirred, when being cooled to 30 DEG C ~ 40 DEG C, discharging can obtain insulation Graphene heat radiation bonding copolymer resins.
Embodiment 2
One. the composition ratio of insulation Graphene heat radiation bonding copolymer resins
Methyl methacrylate 18.5%
Butyl acrylate 21.5%
β-dimethyl-aminoethylmethacrylate 6.5%
Vinylformic acid 42.0%
Octyl acrylate 1.5%
N hydroxymethyl acrylamide 7.5%
Acrylamide 2.5%
Monomer total amount 100%
Initiator 0.45% (accounting for monomer total amount)
Ethanol 300% (accounting for monomer total amount)
Multilayer tablet insulation Graphene (thickness 3nm, length 5um) 320% (accounting for monomer total amount)
Two. copolymerization technique
A. taking ethanol total amount 3/4 for dissolving N hydroxymethyl acrylamide and acrylamide compound monomer, being added in ethanol while stirring and fully dissolving; Add the insulation Graphene of whole consumption 50% subsequently while stirring, dispersed and fully stir 1.5 hours;
B. take all the other monomers and the insulation Graphene of residue 50% consumption is added in mix monomer while stirring, dissolving in 3/5 of initiator total amount wherein, dispersed and fully stir 2.5 hours;
C. step a is mixed with each half of two kinds of solution of step b, be added in copolymerization device, agitator is started in heating, condensing reflux system, when solution temperature to be mixed reaches 75 DEG C ~ 85 DEG C appearance backflows, start timing, under the condition maintaining reflux temperature, two of remaining step a and step b kinds of solution are distinguished section at one time to drip, the period added in 50 ~ 60 minutes;
D. continuing reaction was appended in copolymerization device by remaining 1/4 ethanol and residue 1/5 initiator mixed solution after 3 ~ 5 hours, and the period added in 10 ~ 15 minutes;
E. continue reaction after 1.5 ~ 2.5 hours, stop heated and stirred, when being cooled to 30 DEG C ~ 40 DEG C, discharging can obtain insulation Graphene heat radiation bonding copolymer resins.
Embodiment 3
Dispel the heat between aluminium base and scatterer the composition and ratio of tackiness agent:
Adopt the insulation Graphene heat radiation bonding copolymer resins obtained by embodiment 1, that is:
Single-layer sheet insulation Graphene heat radiation bonding copolymer resins 30%
Vinyl acetic monomer 20%
Ethanol 35%
Butanols 10%
Amido phenolic resin 5%
Above-mentioned heat radiation tackiness agent is mainly used in contacting use with connecting between LED aluminum base plate with scatterer in LED lamp.Bake out temperature is 75 DEG C, and drying time is 8 minutes; Thermal resistance can accomplish 0.003 DEG C/W.
Embodiment 4
Dispel the heat between aluminium base and scatterer the composition and ratio of tackiness agent:
Adopt the insulation Graphene heat radiation bonding copolymer resins obtained by embodiment 2, that is:
Multilayer tablet insulation Graphene heat radiation bonding copolymer resins 42%
Vinyl acetic monomer 18%
Ethanol 25%
Butanols 10%
Amido phenolic resin 5%
Above-mentioned heat radiation tackiness agent is mainly used in contacting use with connecting between LED aluminum base plate with scatterer in LED lamp.Bake out temperature is 75 DEG C, and drying time is 8 minutes; Thermal resistance can accomplish 0.005 DEG C/W.
These are only the preferred embodiments of the present invention, be not limited to the present invention, obviously, those skilled in the art can carry out various change, modification and do not depart from the spirit and scope of the present invention to the present invention.If belong within the scope of the claims in the present invention and equivalent technologies thereof these amendments of the present invention and modification, all belong to protection scope of the present invention.
Claims (6)
1. the making method for the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, it is characterized in that: take the acrylic ester monomer of a certain amount of various structures and insulation Graphene, adopt monomer copolymerization grafting synthetic method, insulation Graphene is introduced in acrylic ester monomer polymerization process, obtain the polymer of high molecular, make the composite base-material containing insulation Graphene heat radiation bonding copolymer resins, composite base-material is used for the heat radiation bonding between LED aluminum base plate and scatterer;
The acrylic ester monomer of described various structures forms by more than three in methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl acrylate, Octyl acrylate, butyl methacrylate, vinylformic acid, N hydroxymethyl acrylamide, acrylamide monomer kind;
The composition of described insulation Graphene heat radiation bonding copolymer resins and the per-cent accounting for monomer total amount are: the monomer total amounts of more than three kinds compositions in described methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl acrylate, Octyl acrylate, butyl methacrylate, vinylformic acid, N hydroxymethyl acrylamide, acrylamide monomer are 100%, initiator 0.25 ~ 0.55%, ethanol 200 ~ 650%, insulation Graphene 5 ~ 320%;
The insulation Graphene heat radiation bonding copolymer resins that described employing monomer copolymerization grafting synthetic method is made, comprises the following steps:
A. taking ethanol total amount 3/4 for dissolving N hydroxymethyl acrylamide and acrylamide compound monomer, being added in ethanol while stirring and fully dissolving; Add the insulation Graphene of whole consumption 50% subsequently while stirring, dispersed and fully stir 1.5 hours;
B. take all the other monomers and the insulation Graphene of residue 50% consumption is added in mix monomer while stirring, dissolving in 3/5 of initiator total amount wherein, dispersed and fully stir 2.5 hours;
C. step a is mixed with each half of two kinds of solution of step b, be added in copolymerization device, agitator is started in heating, condensing reflux system, when solution temperature to be mixed reaches 75 DEG C ~ 85 DEG C appearance backflows, start timing, under the condition maintaining reflux temperature, two of remaining step a and step b kinds of solution are distinguished section at one time to drip, the period added in 50 ~ 60 minutes;
D. continuing reaction was appended in copolymerization device by remaining 1/4 ethanol and remaining initiator mixed solution after 3 ~ 5 hours, and the period added in 10 ~ 15 minutes;
E. continue reaction after 1.5 ~ 2.5 hours, stop heated and stirred, when being cooled to 30 DEG C ~ 40 DEG C, discharging can obtain insulation Graphene heat radiation bonding copolymer resins.
2. according to claim 1 for the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, it is characterized in that: described insulation Graphene is single-layer sheet or multilayer tablet, the thickness of described single-layer sheet is 0.33nm, and length is 3 ~ 5um.
3. according to claim 2 for the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, it is characterized in that: the composition and ratio of described composite base-material is: insulation Graphene heat radiation bonding copolymer resins 15 ~ 50%, vinyl acetic monomer 10 ~ 60%, ethanol 15 ~ 35%, butanols 10 ~ 25%, amido phenolic resin 2 ~ 10%.
4. according to claim 3 for the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, it is characterized in that: the composition and ratio of described composite base-material is: insulation Graphene heat radiation bonding copolymer resins 30 ~ 40%, vinyl acetic monomer 18 ~ 30%, ethanol 20 ~ 30%, butanols 12 ~ 20%, amido phenolic resin 5 ~ 8%.
5. according to claim 3 or 4 for the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, it is characterized in that: the bake out temperature of described composite base-material is 60 DEG C ~ 120 DEG C, and drying time is 5 ~ 20 minutes.
6. according to claim 5 for the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer, it is characterized in that: the bake out temperature of described composite base-material is 80 DEG C ~ 100 DEG C, and drying time is 12 ~ 18 minutes.
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| CN104848065A (en) * | 2015-05-15 | 2015-08-19 | 东莞市闻誉实业有限公司 | Led lamp |
| CN106129240B (en) * | 2016-08-05 | 2019-04-16 | 江苏新宝玛光电制造有限公司 | High-power LED chip and its COB packaging method based on graphene material |
| CN106366983B (en) * | 2016-09-06 | 2019-02-19 | 哈尔滨工业大学无锡新材料研究院 | Acrylate is electromagnetically shielded pressure sensitive adhesive and preparation method thereof |
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| CN103450830A (en) * | 2013-09-02 | 2013-12-18 | 西北工业大学 | Preparation of high-performance magnetic conductive pressure-sensitive adhesive |
| CN103554346A (en) * | 2013-10-14 | 2014-02-05 | 陕西科技大学 | Method for preparing pigment printing binder from oxidized graphene modified polyacrylate |
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| KR101075265B1 (en) * | 2009-04-24 | 2011-10-19 | 충주대학교 산학협력단 | Thermally conductive adhesive composition containing carbon fiber and adhesive sheet fabricated using thereof |
| KR101225497B1 (en) * | 2009-11-05 | 2013-01-23 | (주)덕산테코피아 | Conductive paste and the manufacturing method thereof and the electric device comprising thereof |
| KR101378352B1 (en) * | 2012-11-15 | 2014-03-28 | 충남대학교산학협력단 | Photo-curing psa composition comprising modified graphene and manufacturing thereof |
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| CN103450830A (en) * | 2013-09-02 | 2013-12-18 | 西北工业大学 | Preparation of high-performance magnetic conductive pressure-sensitive adhesive |
| CN103554346A (en) * | 2013-10-14 | 2014-02-05 | 陕西科技大学 | Method for preparing pigment printing binder from oxidized graphene modified polyacrylate |
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| Preparation and properties of UV curable acrylic PSA by vinyl bonded graphene oxide;Beili Pang et al.;《Applied Surface Science》;20130901;第4108-4111页 * |
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