CN101812280B - Environment-friendly heat conduction insulating glue used by high-power LEDs and preparation method - Google Patents
Environment-friendly heat conduction insulating glue used by high-power LEDs and preparation method Download PDFInfo
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Abstract
The invention relates to an environment-friendly heat conduction insulating glue used by high-power LEDs, which is characterized by being prepared from the following raw materials in percentage by weight: 50-68 percent of micro-grade high-thermal conductive powder, 18-30 percent of epoxy resin, 4-10 percent of curing agent, 7-15 percent of solvent, 0.6-1.5 percent of accelerator and 1-2 percent of additive; and the micro-grade high-thermal conductive powder is selected from a mixture formed by one or more of micro-grade aluminum powder, palladium powder, platinum powder, gold powder, C powder, AlN powder and SiC powder. The invention also relates to a preparation method of the heat conduction insulating glue. The environment-friendly heat conduction insulating glue used by high-power LEDs is obtained by optimizing the matching ratio and the modification of the raw materials and improving and simplifying the preparation process. Besides high resistivity, the heat conduction insulating glue also has high thermal conductivity, higher working temperature, strong viscosity, high cutting strength and fine performance index.
Description
Technical field
The present invention relates to a kind of thermal conductive insulation glue, particularly a kind of thermal conductive insulation glue of environment-friendly type great power LED use; The invention still further relates to a kind of preparation method of this thermal conductive insulation glue.
Background technology
21 century is flourish century of information industry, and electron device and electronics be striding forward to the target of microminiaturization constantly.But because the needs of large-scale integrated circuit and electron device microminiaturization, the number of electronic devices on the unit chip area and the density of electronic circuit are more and more higher, and the chip temperature that thereupon produces rising has caused great impact to its performance and life-span.Therefore, heat conduction, heat dissipation problem just become the bottleneck of fixed electron industry development, have caused people's extensive concern.The guardian technique problem that must face.
Particularly for the great power LED industry, because the operating power of chip is very large, if can't effectively reduce its packaging thermal resistance, will wait the great destruction of generation to luminous efficiency and the stability of LED so.Have data to show, for general electronic devices and components, when its temperature is higher than 8 ℃ of its work allowable temperature, working life will reduce by 50%.If be 10 years for the general work temperature in the working life of 150 ℃ electronic devices and components, if work long hours so in the time of 300 ℃, its life-span will drop sharply to 15 days.If with traditional, prepare isolated body with the technology of insulative dielectric material, it is poor heat conductivility to occur, the shortcomings such as mechanical property reduction, and because scattering property is poor, cause the operating power of device can only arrive 40% of nominal operation power, greatly reduced working efficiency and also caused significantly waste for the energy.So in the encapsulation process of great power LED, should use in a large number the insulation paste with excellent heat conductivity performance, with work-ing life and the working efficiency of Effective Raise electronic devices and components, and strengthen simultaneously its reliability.
So in order to solve the critical problem of the production technology of needed thermal conductive insulation glue in the domestic LED industry, for promote domestic LED industry fast, sustainably scientific development, the thermal conductive insulation glue of developing excellent property has great importance.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, and the thermal conductive insulation glue of the environment-friendly type great power LED use of a kind of advantages of simple of filling a prescription, excellent property is provided.
Another technical problem to be solved by this invention has provided a kind of preparation method of the thermal conductive insulation glue of above-described environment-friendly type great power LED use.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is the thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, and be characterized in: it is made by the raw material of following weight percent:
Micron order high thermal conductivity powder 50-68%;
Resins, epoxy 18-30%;
Solidifying agent 4-10%;
Solvent 7-15%;
Promotor 0.6-1.5%;
Additive 1-2%;
Described micron order high thermal conductivity powder is selected from: the mixture of one or more compositions in micron order silver powder, palladium powder, platinum powder, bronze, C powder, AlN powder, the SiC powder.
In the thermal conductive insulation glue that above-described environment-friendly type great power LED uses:
1, described Resins, epoxy can be the disclosed any Resins, epoxy that is suitable for doing thermal conductive insulation glue in the prior art, a kind of in preferred tetraglycidel ether epoxy resin, glycidyl ester, novolac epoxy, modification tetraglycidel ether epoxy resin, modification glycidyl ester or the Modified phenolic epoxy resin, perhaps multiple mixture by any ratio composition applicatory.
2, described solidifying agent can be the disclosed any solidifying agent that is suitable for doing thermal conductive insulation glue in the prior art, the mixture that one or more in preferred anhydrides, boron amide, hydrazides, Dyhard RU 100 or the modification Dyhard RU 100 form in any ratio applicatory.
3, described solvent can be the disclosed any solvent that is suitable for doing thermal conductive insulation glue in the prior art, the mixture that one or more in preferred 2-Butoxyethyl acetate, butylacetate, propylene-glycol ethyl ether, 1-Methoxy-2-propyl acetate, propylene glycol monomethyl ether or the acetone form in any ratio applicatory.
4, described promotor can be the disclosed any promotor that is suitable for doing thermal conductive insulation glue in the prior art, the mixture that one or more in preferred organic urea, imidazoles, phenol or the tertiary amine class form in any ratio applicatory.
5, described additive can be one or more mixtures that form in any ratio applicatory in disclosed defoamer, dispersion agent, coupling agent and the thixotropic agent that is suitable for doing thermal conductive insulation glue in the prior art; The mixture that described additive preferably is comprised of defoamer, dispersion agent, coupling agent and thixotropic agent; And in mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent is preferably 0.5-1: 1-2: 1-1.5: 0.5-2.
The thermal conductive insulation glue that environment-friendly type great power LED of the present invention uses can be according to preparation method's preparation of thermal conductive insulation glue conventional in the prior art.Preferably by preparing with the below.It is as follows that it possesses step: in temperature be under 25 ℃-28 ℃ the constant temperature, humidity is to be not more than under 60% the constant humidity condition to carry out following operation: take by weighing Resins, epoxy, solvent, solidifying agent, promotor and additive by described proportioning raw materials first, stir to such an extent that matrix is for subsequent use after the mixing; Then take by weighing micron order high thermal conductivity powder by described proportioning raw materials, and put into three-roller behind the above-mentioned matrix mix and blend and mix, and get final product.
The particle diameter of thermal conductive insulation glue of the present invention is 3-10 μ m, and viscosity is about the 30000-60000 centipoise, and the resistivity of thermal conductive insulation glue is at 1-3x10 after solidifying
14Ω cm, thermal conductivity is at 20-24w/km, and shearing resistance is at 5-9x10
13Pa, maximum operation (service) temperature can arrive 280 ℃.So the heat dispersion that this thermal conductive insulation glue can the Effective Raise great power LED, thereby for the working efficiency that improves great power LED with reliable guarantee is provided work-ing life.
The present invention by use diameter at the high thermal conductivity powder of micron dimension as thermal conducting agent, selectivity adds defoamer, dispersion agent, coupling agent and thixotropic agent etc. simultaneously, has obtained the thermal conductive insulation glue that chi directly is uniformly dispersed, solidification value is low and set time is short.And the present invention is conducted electricity insulation paste use 2-Butoxyethyl acetate, butylacetate, propylene-glycol ethyl ether, 1-Methoxy-2-propyl acetate, propylene glycol monomethyl ether or acetone etc. as solvent; and avoid using in the past the virose toluene of tool, dimethylbenzene and phenylcarbinol equal solvent in the technology of preparing; adequately protected environment and the producer's health meets the requirement of national green environmental protection.
And the present invention improves and simplification preparation technology by optimizing raw material ratio and modification, and having obtained can be for the environment-friendly type thermal conductive insulation glue of great power LED.Thermal conductive insulation glue of the present invention is on the basis with very high resistivity (1-3x1014 Ω cm), have simultaneously high thermal conductivity (20-24w/km), higher working temperature (280 ℃) and strong viscosity (30000-60000 centipoise) and high shear strength (5-9x1013Pa), its performance index are good.The inventive method is used relatively simple preparation technology and production unit in the high performance thermal conductive insulation glue production process of preparation simultaneously, have simultaneously that cost is low, output is large, efficient is high and the advantage such as reliability is strong, be particularly suitable for encapsulation and heat sink use on the great power LED.
Description of drawings
Fig. 1 is the SEM figure of the thermal conductive insulation glue of the present invention after solidifying.
Fig. 2 is the sticking power distribution plan of 150 ℃ of thermal conductive insulation glues of the present invention behind lower the curing.
Fig. 3 is the sticking power distribution plan of 230 ℃ of thermal conductive insulation glues of the present invention behind lower the curing.
Fig. 4 is the viscosity profile of thermal conductive insulation glue of the present invention.
Fig. 5 is the thermal conductivity distribution plan of thermal conductive insulation glue of the present invention.
Fig. 6 is volt-ampere characteristic (I-V) graphic representation of thermal conductive insulation glue of the present invention under the room temperature.
Embodiment
Referring to accompanying drawing, further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not consist of its Copyright law.
Embodiment 1.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by the raw material of following weight percent:
Micron order high thermal conductivity powder 57.4%;
Resins, epoxy 30%;
Solidifying agent 4%;
Solvent 7%;
Promotor 0.6%;
Additive 1%;
Described micron order high thermal conductivity powder is selected from: a kind of in micron order silver powder, palladium powder, platinum powder, bronze, C powder, AlN powder, the SiC powder.
Its method for making adopts the preparation method of conventional thermal conductive insulation glue.
Embodiment 2.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by the raw material of following weight percent:
Micron order high thermal conductivity powder 53.5%;
Resins, epoxy 18%;
Solvent 15%;
Promotor 1.5%;
Additive 2%;
Described micron order high thermal conductivity powder is selected from: any 2 kinds or 3 kinds of mixtures that form in any proportion in micron order silver powder, palladium powder, platinum powder, bronze, C powder, AlN powder, the SiC powder.
Its preparation method is: in temperature be under 26 ℃ the constant temperature, humidity is to carry out following operation under 52% the constant humidity condition: take by weighing Resins, epoxy, solvent, solidifying agent, promotor and additive by described proportioning raw materials first, stir to such an extent that matrix is for subsequent use after the mixing; Then take by weighing micron order high thermal conductivity powder by described proportioning raw materials, and put into three-roller behind the above-mentioned matrix mix and blend and mix, and get final product.
Embodiment 3.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by the raw material of following weight percent:
Micron order high thermal conductivity powder 50%;
Resins, epoxy 30%;
Solidifying agent 8%;
Solvent 9.8%;
Additive 1.2%;
Described micron order high thermal conductivity powder is selected from: any 4 kinds or 5 kinds of mixtures that form in any proportion in micron order silver powder, palladium powder, platinum powder, bronze, C powder, AlN powder, the SiC powder.
Its preparation method is: in temperature be under 28 ℃ the constant temperature, humidity is to carry out following operation under 60% the constant humidity condition: take by weighing Resins, epoxy, solvent, solidifying agent, promotor and additive by described proportioning raw materials first, stir to such an extent that matrix is for subsequent use after the mixing; Then take by weighing micron order high thermal conductivity powder by described proportioning raw materials, and put into three-roller behind the above-mentioned matrix mix and blend and mix, and get final product.
Embodiment 4.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by the raw material of following weight percent:
Micron order high thermal conductivity powder 68%;
Resins, epoxy 18%;
Solidifying agent 4%;
Solvent 7%;
Promotor 1.2%;
Additive 1.8%;
Described micron order high thermal conductivity powder is selected from: any 6 kinds or the mixture that forms in any proportion in micron order silver powder, palladium powder, platinum powder, bronze, C powder, AlN powder, the SiC powder.
Its preparation method is: in temperature be under 27 ℃ the constant temperature, humidity is to carry out following operation under 50% the constant humidity condition: take by weighing Resins, epoxy, solvent, solidifying agent, promotor and additive by described proportioning raw materials first, stir to such an extent that matrix is for subsequent use after the mixing; Then take by weighing micron order high thermal conductivity powder by described proportioning raw materials, and put into three-roller behind the above-mentioned matrix mix and blend and mix, and get final product.
Embodiment 5.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by the raw material of following weight percent:
Micron order high thermal conductivity powder 60%;
Resins, epoxy 19%;
Solidifying agent 8%;
Solvent 11%;
Promotor 0.7%;
Additive 1.3%;
Described micron order high thermal conductivity powder is selected from: the mixture that forms in any proportion in micron order silver powder, palladium powder, platinum powder, bronze, C powder, AlN powder and the SiC powder.
Its preparation method is: in temperature be under 25 ℃ the constant temperature, humidity is to carry out following operation under 55% the constant humidity condition: take by weighing Resins, epoxy, solvent, solidifying agent, promotor and additive by described proportioning raw materials first, stir to such an extent that matrix is for subsequent use after the mixing; Then take by weighing micron order high thermal conductivity powder by described proportioning raw materials, and put into three-roller behind the above-mentioned matrix mix and blend and mix, and get final product.
Embodiment 6.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-5: described Resins, epoxy is selected from the mixture of one or more compositions in tetraglycidel ether epoxy resin, glycidyl ester, novolac epoxy, modification tetraglycidel ether epoxy resin, modification glycidyl ester or the Modified phenolic epoxy resin.
Embodiment 7.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-6: described solidifying agent is selected from the mixture of one or more compositions in acid anhydrides, boron amide, hydrazides, Dyhard RU 100 or the modification Dyhard RU 100.
Embodiment 8.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-7: described solvent is selected from the mixture of one or more compositions in 2-Butoxyethyl acetate, butylacetate, propylene-glycol ethyl ether, 1-Methoxy-2-propyl acetate, propylene glycol monomethyl ether or the acetone.
Embodiment 9.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-8: described promotor is selected from the mixture of one or more compositions in organic urea, imidazoles, phenol or the tertiary amine class.
Embodiment 10.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-9: described additive is selected from one or more above mixtures that form in defoamer, dispersion agent, coupling agent and the thixotropic agent.
Embodiment 11.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-9: described additive is the mixture that is comprised of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent is followed successively by 0.5: 2: 1: 0.5.
Embodiment 12.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-9: described additive is the mixture that is comprised of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent is followed successively by 1: 1: 1: 1.
Embodiment 13.In the thermal conductive insulation glue that any one described environment-friendly type great power LED uses among the embodiment 1-9: described additive is the mixture that is comprised of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent is followed successively by 1: 2: 1.5: 2.
Embodiment 14.With reference to Fig. 1-6.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by the raw material of following weight percent:
Micron order high thermal conductivity powder 58%;
Resins, epoxy 20%;
Solidifying agent 8.3%;
Solvent 11%;
Promotor 1.2%;
Additive 1.5%;
Described micron order high thermal conductivity powder is for getting the mixture that micron order bronze, C powder and SiC powder form by weight 1: 1: 1;
Described Resins, epoxy is tetraglycidel ether epoxy resin;
Described solidifying agent is acid anhydrides;
Described solvent is 2-Butoxyethyl acetate;
Described promotor is organic urea;
Described additive is the mixture that is comprised of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent is followed successively by 0.8: 1.5: 1.2: 1.2.
Its preparation method is: in temperature be under 26 ℃ the constant temperature, humidity is to carry out following operation under 50% the constant humidity condition: take by weighing Resins, epoxy, solvent, solidifying agent, promotor and additive by described proportioning raw materials first, stir to such an extent that matrix is for subsequent use after the mixing; Then take by weighing micron order high thermal conductivity powder by described proportioning raw materials, and put into three-roller behind the above-mentioned matrix mix and blend and mix, and get final product.
It is transparent thick colloid that present embodiment is prepared thermal conductive insulation glue, the colloid color even, and particle size distribution is even, and the diameter Distribution scope is at 3-10 μ m; The SEM figure of the thermal conductive insulation glue after the curing as shown in Figure 1.
Can obviously determine the composition of prepared environment-friendly type thermal conductive insulation glue by doing the EDX energy spectrogram that solidifies rear thermal conductive insulation glue.Wherein main component is C, O element, and they come from the organism such as Resins, epoxy, and wherein the Au element is to derive from bronze, and the Si element then derives from the SiC powder.In addition, do not have other element in the whole colloid, this shows that product prepared among the present invention is highly purified thermal conductive insulation glue.
In order further to determine the serviceability of present embodiment thermal conductive insulation glue, we have carried out the test analysis of a series of systems to 50 samples.From Fig. 2-3, we can find that the sticking power of the thermal conductive insulation glue sample after 150 ℃ and the 230 ℃ of curing can reach respectively 1.5x10
13Pa and 9x10
12Pa.Although a little decline appears in the sticking power through the thermal conductive insulation glue after 230 ℃ of curing and substrate, still can satisfy the basic demand that LED uses.And the viscosity profile among Fig. 4 shows, the viscosity profile scope of the thermal conductive insulation glue of embodiment is at the 22000-25000 centipoise.Shown in the thermal conductivity distribution plan among Fig. 5, the average thermal conductivity of the thermal conductive insulation glue of embodiment has reached 22w/km.Fig. 6 has provided the current voltage characteristic of sample, and the average resistance that can calculate the thermal conductive insulation glue of embodiment is 2.5x10
14Ω/cm
2, this can satisfy the insulating requirements of great power LED fully.Shown that by above-mentioned data analysis the performance characteristics of the prepared thermal conductive insulation glue of embodiment (specific conductivity, thermal conductivity, viscosity and shearing resistance etc.) performance is very excellent.
Claims (2)
1. the thermal conductive insulation glue that uses of an environment-friendly type great power LED, it is characterized in that: it is made by the raw material of following weight percent:
Described micron order high thermal conductivity powder is for getting the mixture that micron order bronze, C powder and SiC powder form by weight 1: 1: 1;
Described Resins, epoxy is tetraglycidel ether epoxy resin;
Described solidifying agent is acid anhydrides;
Described solvent is 2-Butoxyethyl acetate;
Described promotor is organic urea;
Described additive is the mixture that is comprised of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent is followed successively by 0.8: 1.5: 1.2: 1.2.
2. the preparation method of the thermal conductive insulation glue that uses of an environment-friendly type great power LED as claimed in claim 1, it is characterized in that: in temperature be under 25 ℃-28 ℃ the constant temperature, humidity is to be not more than under 60% the constant humidity condition to carry out following operation: take by weighing Resins, epoxy, solvent, solidifying agent, promotor and additive by described proportioning raw materials first, stir to such an extent that matrix is for subsequent use after the mixing; Then take by weighing micron order high thermal conductivity powder by described proportioning raw materials, and put into three-roller behind the above-mentioned matrix mix and blend and mix, and get final product.
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| CN 201010142958 CN101812280B (en) | 2010-04-09 | 2010-04-09 | Environment-friendly heat conduction insulating glue used by high-power LEDs and preparation method |
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Effective date of registration: 20200721 Address after: No.16, songtiaozhen Hualu, Haizhou District, Lianyungang City, Jiangsu Province 222000 Patentee after: Lianyungang Zhaohua Photoelectric Technology Co., Ltd Address before: 222000 Long Xi deep blue apartment 1, the Yellow River Road, Lianyungang economic and Technological Development Zone, Jiangsu, Lianyungang 810 Patentee before: LIANYUNGANG ZHAOHUA TECHNOLOGY Co.,Ltd. |