CN101812280A - 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, the thermal conductive insulation glue that particularly a kind of environment-friendly type great power LED uses; 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 influence 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,,, will produce great destruction to the luminous efficiency of LED and stability etc. so if can't reduce its packaging thermal resistance effectively because the operating power of chip is very big.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 is 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 use technology traditional, use insulative dielectric material to prepare isolated body, it is poor heat conductivility to occur, 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 waste significantly for the energy.So in the encapsulation process of great power LED, should use insulation paste in a large number,, and strengthen its reliability simultaneously with the work-ing life and the working efficiency of effective raising electronic devices and components with excellent heat conductivity performance.
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, scientific development sustainably, 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 at 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 following raw materials by 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 Resins, epoxy, 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 are formed 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 are formed 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 are formed in any ratio applicatory.
5, described additive can be one or more mixtures of forming 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 made up 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 earlier, stir to such an extent that matrix is standby after the mixing; Take by weighing micron order high thermal conductivity powder by described proportioning raw materials then, mix with above-mentioned matrix and put into three-roller after stirring and mix, promptly.
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 solidifying the back thermal conductive insulation glue is at 1-3x10
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 this thermal conductive insulation glue can effectively improve the heat dispersion of 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; have toxic toluene, dimethylbenzene and phenylcarbinol equal solvent in the technology of preparing and avoid using in the past; the adequately protected environment and the producer's health meets national requirements of 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 use.Thermal conductive insulation glue of the present invention is on the basis with very high resistivity (1-3x1014 Ω cm), have high thermal conductivity (20-24w/km), higher working temperature (280 ℃) and strong viscosity (30000-60000 centipoise) and high shear strength (5-9x1013Pa) simultaneously, its performance index are good.The inventive method is used simple relatively 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 big, efficient is high and advantage such as good reliability, 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 the thermal conductive insulation glue of the present invention after solidifying under 150 ℃.
Fig. 3 is the sticking power distribution plan of the thermal conductive insulation glue of the present invention after solidifying under 230 ℃.
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
Following with reference 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 constitute restriction to its right.
Embodiment 1.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by following raw materials by 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 following raw materials by 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: press the mixture that arbitrary proportion is formed for any 2 kinds or 3 kinds 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 earlier, stir to such an extent that matrix is standby after the mixing; Take by weighing micron order high thermal conductivity powder by described proportioning raw materials then, mix with above-mentioned matrix and put into three-roller after stirring and mix, promptly.
Embodiment 3.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by following raw materials by weight percent:
Micron order high thermal conductivity powder 50%;
Resins, epoxy 30%;
Solidifying agent 8%;
Solvent 9.8%;
Promotor 1%;
Additive 1.2%;
Described micron order high thermal conductivity powder is selected from: press the mixture that arbitrary proportion is formed for any 4 kinds or 5 kinds 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 earlier, stir to such an extent that matrix is standby after the mixing; Take by weighing micron order high thermal conductivity powder by described proportioning raw materials then, mix with above-mentioned matrix and put into three-roller after stirring and mix, promptly.
Embodiment 4.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by following raw materials by 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: in micron order silver powder, palladium powder, platinum powder, bronze, C powder, AlN powder, the SiC powder any 6 kinds or press the mixture that arbitrary proportion is formed.
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 earlier, stir to such an extent that matrix is standby after the mixing; Take by weighing micron order high thermal conductivity powder by described proportioning raw materials then, mix with above-mentioned matrix and put into three-roller after stirring and mix, promptly.
Embodiment 5.The thermal conductive insulation glue that a kind of environment-friendly type great power LED uses, it is made by following raw materials by 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: press the mixture that arbitrary proportion is formed 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 earlier, stir to such an extent that matrix is standby after the mixing; Take by weighing micron order high thermal conductivity powder by described proportioning raw materials then, mix with above-mentioned matrix and put into three-roller after stirring and mix, promptly.
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 Resins, epoxy.
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 of forming 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 of being made up of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent was 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 of being made up of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent was 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 of being made up of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent was 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 following raw materials by 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 are formed by weight 1: 1: 1;
Described Resins, epoxy is tetraglycidel ether epoxy resin;
Described solidifying agent is an acid anhydrides;
Described solvent is a 2-Butoxyethyl acetate;
Described promotor is organic urea;
Described additive is the mixture of being made up of defoamer, dispersion agent, coupling agent and thixotropic agent; In the mixture, the weight ratio of defoamer, dispersion agent, coupling agent and thixotropic agent was 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 earlier, stir to such an extent that matrix is standby after the mixing; Take by weighing micron order high thermal conductivity powder by described proportioning raw materials then, mix with above-mentioned matrix and put into three-roller after stirring and mix, promptly.
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.
By doing the composition that the EDX that solidifies the back thermal conductive insulation glue can spectrogram can obviously determine the prepared environment-friendly type thermal conductive insulation glue that goes out.Wherein main component is C, O element, and they come from 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 the prepared product that goes out is highly purified thermal conductive insulation glue among the present invention.
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 1.5x10 respectively
13Pa and 9x10
12Pa.Though a little decline appears in the sticking power through 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.Show 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 (8)
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 following raw materials by 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.
2. the thermal conductive insulation glue that environment-friendly type great power LED according to claim 1 uses, it is characterized in that: 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 Resins, epoxy.
3. the thermal conductive insulation glue that environment-friendly type great power LED according to claim 1 uses, it is characterized in that: 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.
4. the thermal conductive insulation glue that environment-friendly type great power LED according to claim 1 uses, it is characterized in that: 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.
5. the thermal conductive insulation glue that environment-friendly type great power LED according to claim 1 uses, it is characterized in that: described promotor is selected from the mixture of one or more compositions in organic urea, imidazoles, phenol or the tertiary amine class.
6. the thermal conductive insulation glue that environment-friendly type great power LED according to claim 1 uses is characterized in that: described additive is selected from one or more above mixtures of forming in defoamer, dispersion agent, coupling agent and the thixotropic agent.
7. the thermal conductive insulation glue that environment-friendly type great power LED according to claim 1 uses is characterized in that: the mixture of described additive for being made up 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 0.5-1: 1-2: 1-1.5: 0.5-2.
8. the preparation method of a thermal conductive insulation glue that uses as the described environment-friendly type great power LED of claim 1-7, 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 earlier, stir to such an extent that matrix is standby after the mixing; Take by weighing micron order high thermal conductivity powder by described proportioning raw materials then, mix with above-mentioned matrix and put into three-roller after stirring and mix, promptly.
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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. |