CN102352213A - Organic silicon heat conduction bonding agent adopting high-power light emitting diode (LED) for illumination and preparation method thereof - Google Patents
Organic silicon heat conduction bonding agent adopting high-power light emitting diode (LED) for illumination and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an organic silicon heat conduction bonding agent adopting a high-power light emitting diode (LED) for illumination and a preparation method thereof. The organic silicon heat conduction bonding agent consists of polydimethylsiloxane with trimethoxy silane oxygen at the tail end, alkoxy silane cross linking agents, titanate catalysts, adhesion promoters, micrometer level mixed heat conducting materials with different grain diameters, nanometer level heat conduction materials and the like. The preparation method of the bonding agent comprises the following steps that: the nanometer level heat conduction materials carry out lyophobic treatment, then, the polydimethylsiloxane with trimethoxy silane oxygen at the tail end, the micrometer level mixed heat conducting materials with different grain diameters and the nanometer level heat conduction materials after the lyophobic treatment are added into a high-speed dispersing stirring machine and are stirred and dewatered for 1 to 3 hours in vacuum, the alkoxy silane cross linking agents, the titanate catalysts and the adhesion promoters are added after the materials are cooled, the materials are output after the vacuum stirring for 60 minutes, and the single ingredients are sealed and packed. The organic silicon heat conduction bonding agent has the advantages that the heat conduction material filling parts are few, the heat conduction factor is high, the elasticity after the solidification is excellent, no corrosion is caused on light emitting diode (LED) electronic elements and aluminum base plates, and the like.
Description
Technical field
The invention belongs to self cure heat-conducting silicon rubber technical field, be specifically related to a kind of thermally conductive material fill umber less and thermal conductivity is high, solidify back elasticity excellent, LED electronic devices and components and aluminium base are not had corrosive silicone adhesive.The present invention is widely used in that the heat conduction of electronic devices and components is adhesively fixed in the high-power LED illumination product.
Background technology
As the 4th generation lighting engineering; The LED illumination application of green energy conservation expands to the function illumination of street lamp, indoor lamp gradually from the Landscape Lighting that shows, develop the color; Wherein the power of led light source, LED driving also all constantly increases; Heat dissipation problem is constantly outstanding, especially the light source of high-power LED illumination and drive the heat dissipation problem important bottleneck in its life-span especially.
High-power LED illumination product; As the light source and the aluminium base heat conduction that are used for LED bulb lamp, the LED shot-light of interior lighting fix, drive the heat conduction of module components and parts is fixed and and shell, radiator element between fixing once trial of heat conduction adopt heat-conducting silicone grease or thermal conductive silicon film as insulated heat-conducting medium; Also need adopt extra part to fix simultaneously, have potential conduction hidden danger; The irregularly shaped thermal conductive silicon film that more makes of some component is difficult to effectively fill the gap, and the air in the gap greatly reduces radiating effect; Therefore have that heat conduction, heat-conductive bonding agent bonding, insulation function are just more and more to be applied to a plurality of component assemblings of high-power LED illumination product.
Patent CN10139775A has announced the thermal conductivity flexible material that uses in the power type LED lamp; Need in the time of 100 ℃-150 ℃, just can sinter thermally conductive material into after the nanometer silver fusing; And the control chip of high-power LED illumination product; Components and parts such as electric capacity can't stand the baking of temperature more than 100 ℃; The limitation of same temperature limitation also appears among patent CN101139513A and the WO2005030874; The addition curing heat-conductive bonding agent that two patents in back are announced also need be heated to 100 ℃-150 ℃, and the platinum catalyst component also very easily receives aluminium base in the heat-conductive bonding agent; Components and parts; Sulfur-bearings such as soldering flux; Ammonia; Thereby the phosphorus substance poisoning and deactivation can not crosslinking curing.
So patent CN100374490C has announced that the heat-conductive bonding agent of self-vulcanizing is to solve the technological deficiency of heating cure heat-conductive bonding agent; Its thermally conductive material is still continued to use highly-filled alumina material commonly used in the past; Promptly fill the aluminum oxide umber and reach more than 9 times of base polymer dimethyl polysiloxane; This increases the difficulty of suitability for industrialized production greatly; Simultaneous altitude is filled alumina material and is caused the heat-conductive bonding agent extrusion performance to descend easily and solidify the back hardness is too high lacking flexibility the problems such as electronic devices and components of the big and fragile bonding portion of internal stress.
Summary of the invention
The heat-conductive bonding agent that the objective of the invention is to overcome prior art causes defectives such as the increase of production difficulty, extrusion performance and flexibility decrease because of highly-filled alumina packing; Provide a kind of thermally conductive material filling umber less; But still maintenance high thermal conductivity coefficient; LED electronic devices and components and aluminium base are not had corrodibility, and being exposed to simultaneously then can be rapidly by the organosilicon heat-conductive bonding agent that is used for high-power LED illumination of airborne moisture-curable in the air.
Another object of the present invention is to be provided for the preparation method of the organosilicon heat-conductive bonding agent of high-power LED illumination.
For reaching above purpose, the present invention can realize through following scheme:
A kind of organosilicon heat-conductive bonding agent that is used for high-power LED illumination is characterized in that (by weight) composed of the following components:
Further, described micron order different-grain diameter blended thermally conductive material median size is the 1-30 micron.。
Further, described micron order different-grain diameter blended thermally conductive material is at least a in micron order different-grain diameter blended ball-aluminium oxide, zinc oxide, the aluminium nitride.
Further, described nano level thermally conductive material is the nano level aluminium nitride through hydrophobic treatment, and median size is 40 nanometers, specific surface area 50m
2/ g plays the thixotropic agent effect simultaneously.
Further, the polydimethylsiloxane structural formula of described terminal trimethoxy silica does
m = 20 ~ 100,25 ℃ viscosity of 0.5Pa.s ~ 10Pa.s.
Further, described alkoxy silane cross linked dose is at least a in methyltrimethoxy silane, vinyltrimethoxy silane, the phenyltrimethoxysila,e.
Further, described titanate ester catalyzer is one or both in tetra-n-butyl titanate, tetraisopropoxy titanium, two (methyl aceto acetate) metatitanic acid diisobutyl ester.
Further; Described tackifier are the organoalkoxysilane that contains amido, epoxy group(ing) or isocyanato; Like γ-An Bingjisanyiyangjiguiwan, γ-glycidyl ether oxygen base propyl trimethoxy silicane, 1,3, one or both in 5-three (the trimethoxy silicon propyl group) polymeric polyisocyanate
A kind of preparation method who is used for the organosilicon heat-conductive bonding agent of high-power LED illumination may further comprise the steps:
Step 1: nano level thermally conductive material hydrophobic treatment: 100 parts of nano level thermally conductive materials, hexamethyldisilazane 2-6 part, in the high speed dispersion stirrer in 100 ℃-120 ℃ of temperature stirring reaction 2-5 hour;
Step 2: count by weight; Polydimethylsiloxane, 200-500 part micron order different-grain diameter blended thermally conductive material, 5-20 part of 100 parts of terminal trimethoxy silica are added in the high speed dispersion stirrer through the nano level thermally conductive material that hydrophobic treatment is crossed; 110 ℃-130 ℃ following vacuum stirring dehydrations 1-3 hour; Add alkoxy silane cross linked dose of 2-8 part after the cooling again; 0.6-2 part titanate ester catalyzer and 2-6 part tackifier, vacuum stirring are discharging sealing single-component package after 60 minutes.
Owing to adopted technique scheme, the present invention to have following advantage:
1, adopt nano level aluminium nitride that micron order different-grain diameter blended thermally conductive material and hydrophobic treatment cross as thermally conductive material; And the ratio combination according to the closest packing distribution curve is used; Nano level aluminium nitride body thermal conductivity is very high simultaneously; Thereby realize that the thermally conductive material of filling less umber just can reach good heat-conducting, and have excellent resilience after solidifying.
2, nano aluminum nitride and the base polymer consistency crossed of hydrophobic treatment is better; Tackiness agent extrusion performance and mobile the maintenance well; Simultaneously also play thixotropic transformation, prevent after the tackiness agent long storage time micron order different-grain diameter blended thermally conductive material separate and subside to take place.
3, the tackiness agent of room temperature fast-curing is convenient to the high-power LED illumination product streamline and is produced installation fast, has also avoided being subjected to simultaneously sulfur-bearing, ammonia, phosphorus substance poisoning and deactivations such as aluminium base, components and parts, soldering flux
4, the polydimethylsiloxane with terminal trimethoxy silica is the organosilicon base polymer of tackiness agent, and not retrogradation of material in the preparation process does not have the viscosity peak, has stopped the storage unstable that free hydroxyl causes in the conventional adhesive simultaneously.
5, adopt the neutral dealcoholizing-type tackiness agent of alkoxyl group linking agent and titanate ester Preparation of Catalyst, be fit to being adhesively fixed of high-power LED illumination product electronic devices and components, avoided of the infringement of ketoxime removing type tackiness agent metallic substance.
Embodiment
Below through the embodiment description concrete to the present invention; Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; Can not be interpreted as the restriction to protection domain of the present invention, the person skilled in the art in this field can make nonessential improvement and adjustment according to the present invention.
Embodiment 1
In parts by weight, with 100 parts of median size 40 nano aluminum nitrides, 4 parts of hexamethyldisilazanes in 110 ℃ of stirring reactions of temperature 3 hours, use as nano heat-conductive material after the hydrophobic treatment in the high speed dispersion stirrer.
Viscosity is 100 parts of the polydimethylsiloxanes of the terminal trimethoxy silica of 1Pa.S when getting 25 ℃; Median size is 200 parts of 10 microns ball-aluminium oxides; Median size is 100 parts of 1 micron ball-aluminium oxides; 40 nano aluminum nitrides that hydrophobic treatment is crossed add in the high speed dispersion stirrer for 15 parts; 120 ℃ of following vacuum stirring dehydrations 2 hours; Add 5 parts of methyltrimethoxy silanes after the cooling again; 0.5 part of tetra-n-butyl titanate; 0.5 part of two (methyl aceto acetate) metatitanic acid diisobutyl ester; 2 parts of γ-An Bingjisanyiyangjiguiwans; 1; 3; 2 parts of 5-three (trimethoxy silicon propyl group) polymeric polyisocyanates; Vacuum stirring is discharging sealing single-component package after 60 minutes, and the product performance test result sees for details shown in the table 1.
Embodiment 2
In parts by weight, with 100 parts of median size 40 nano aluminum nitrides, 2 parts of hexamethyldisilazanes in 100 ℃ of stirring reactions of temperature 5 hours, use as nano heat-conductive material after the hydrophobic treatment in the high speed dispersion stirrer.
Viscosity is 100 parts of the polydimethylsiloxanes of the terminal trimethoxy silica of 10Pa.S when getting 25 ℃; Median size is 130 parts of 30 microns aluminium nitride; Median size is 70 parts of 5 microns aluminium nitride; 40 nano aluminum nitrides that hydrophobic treatment is crossed add in the high speed dispersion stirrer for 20 parts; 110 ℃ of following vacuum stirring dehydrations 3 hours; Add 2 parts of vinyltrimethoxy silanes after the cooling again; 0.3 part of tetraisopropoxy titanium; 0.3 part of two (methyl aceto acetate) metatitanic acid diisobutyl ester; 1 part of γ-glycidyl ether oxygen base propyl trimethoxy silicane; 1; 3; 1 part of 5-three (trimethoxy silicon propyl group) polymeric polyisocyanate; Vacuum stirring is discharging sealing single-component package after 60 minutes, and the product performance test result sees for details shown in the table 1.
Embodiment 3
In parts by weight, with 100 parts of median size 40 nano aluminum nitrides, 6 parts of hexamethyldisilazanes in 120 ℃ of stirring reactions of temperature 2 hours, use as nano heat-conductive material after the hydrophobic treatment in the high speed dispersion stirrer.
Viscosity is 100 parts of the polydimethylsiloxanes of the terminal trimethoxy silica of 0.5Pa.S when getting 25 ℃; Median size is 340 parts in 20 microns zinc oxide; Median size is 160 parts of 2 micrometer aluminas; 40 nano aluminum nitrides that hydrophobic treatment is crossed add in the high speed dispersion stirrer for 5 parts; 130 ℃ of following vacuum stirring dehydrations 1 hour; Add 5 parts of phenyltrimethoxysila,e after the cooling again; 3 parts of methyltrimethoxy silanes; 2 parts of tetraisopropoxy titaniums; 6 parts of γ-An Bingjisanyiyangjiguiwans; Vacuum stirring is discharging sealing single-component package after 60 minutes, and the product performance test result sees for details shown in the table 1.
Table 1 organosilicon heat-conductive bonding agent The performance test results
Claims (9)
1. organosilicon heat-conductive bonding agent that is used for high-power LED illumination is characterized in that (by weight) composed of the following components:
100 parts of the polydimethylsiloxanes of terminal trimethoxy silica;
Alkoxy silane cross linked dose of 2-8 part;
Titanate ester catalyzer 0.6-2 part;
Tackifier 2-6 part;
Micron order different-grain diameter blended thermally conductive material 200-500 part;
Nano level thermally conductive material 5-20 part.
2. the organosilicon heat-conductive bonding agent that is used for high-power LED illumination according to claim 1 is characterized in that described micron order different-grain diameter blended thermally conductive material median size is the 1-30 micron.
3. the organosilicon heat-conductive bonding agent that is used for high-power LED illumination according to claim 2 is characterized in that described micron order different-grain diameter blended thermally conductive material is at least a in micron order different-grain diameter blended ball-aluminium oxide, zinc oxide, the aluminium nitride.
4. according to claim 1, the 2 or 3 described organosilicon heat-conductive bonding agents that are used for high-power LED illumination, it is characterized in that described nano level thermally conductive material is the nano level aluminium nitride through hydrophobic treatment, median size is 40 nanometers, specific surface area 50m
2/ g plays the thixotropic agent effect simultaneously.
5. according to claim 1, the 2 or 3 described organosilicon heat-conductive bonding agents that are used for high-power LED illumination, it is characterized in that the polydimethylsiloxane structural formula of described terminal trimethoxy silica does
6. according to claim 1, the 2 or 3 described organosilicon heat-conductive bonding agents that are used for high-power LED illumination, it is characterized in that described alkoxy silane cross linked dose of at least a in methyltrimethoxy silane, vinyltrimethoxy silane, the phenyltrimethoxysila,e.
7. according to claim 1, the 2 or 3 described organosilicon heat-conductive bonding agents that are used for high-power LED illumination, it is characterized in that described titanate ester catalyzer is one or both in tetra-n-butyl titanate, tetraisopropoxy titanium, two (methyl aceto acetate) metatitanic acid diisobutyl ester.
8. according to claim 1, the 2 or 3 described organosilicon heat-conductive bonding agents that are used for high-power LED illumination; It is characterized in that described tackifier are the organoalkoxysilane that contains amido, epoxy group(ing) or isocyanato; Like γ-An Bingjisanyiyangjiguiwan, γ-glycidyl ether oxygen base propyl trimethoxy silicane, 1; 3, one or both in 5-three (the trimethoxy silicon propyl group) polymeric polyisocyanate.
9. one kind prepares the described method that is used for the organosilicon heat-conductive bonding agent of high-power LED illumination of claim 1, it is characterized in that may further comprise the steps:
Step 1: nano level thermally conductive material hydrophobic treatment: 100 parts of nano level thermally conductive materials, hexamethyldisilazane 2-6 part, in the high speed dispersion stirrer in 100 ℃-120 ℃ of temperature stirring reaction 2-5 hour;
Step 2: count by weight; Polydimethylsiloxane, 200-500 part micron order different-grain diameter blended thermally conductive material, 5-20 part of 100 parts of terminal trimethoxy silica are added in the high speed dispersion stirrer through the nano level thermally conductive material that hydrophobic treatment is crossed; 110 ℃-130 ℃ following vacuum stirring dehydrations 1-3 hour; Add alkoxy silane cross linked dose of 2-8 part after the cooling again; 0.6-2 part titanate ester catalyzer and 2-6 part tackifier, vacuum stirring are discharging sealing single-component package after 60 minutes.
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CN103013122A (en) * | 2012-12-11 | 2013-04-03 | 江苏大学 | Preparation method of micro-nanometer mixed stuffing/liquid silicon rubber heat-conductive composite material |
CN103215010A (en) * | 2013-04-28 | 2013-07-24 | 深圳市新亚新材料有限公司 | Single-component dealcoholized heat-conducting flame retardant fixing glue and preparation method thereof |
CN103756575A (en) * | 2013-11-27 | 2014-04-30 | 常熟市富邦胶带有限责任公司 | Heat-conductive double-faced adhesive tape and preparation technology thereof |
CN104497558A (en) * | 2014-11-28 | 2015-04-08 | 广东银禧科技股份有限公司 | Novel heat conduction nylon composite material and preparation method thereof |
CN105086918A (en) * | 2015-08-07 | 2015-11-25 | 苏州晶雷光电照明科技有限公司 | Efficient heat conduction glue for LEDs |
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CN103215010A (en) * | 2013-04-28 | 2013-07-24 | 深圳市新亚新材料有限公司 | Single-component dealcoholized heat-conducting flame retardant fixing glue and preparation method thereof |
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CN103756575A (en) * | 2013-11-27 | 2014-04-30 | 常熟市富邦胶带有限责任公司 | Heat-conductive double-faced adhesive tape and preparation technology thereof |
CN104497558A (en) * | 2014-11-28 | 2015-04-08 | 广东银禧科技股份有限公司 | Novel heat conduction nylon composite material and preparation method thereof |
CN105086918A (en) * | 2015-08-07 | 2015-11-25 | 苏州晶雷光电照明科技有限公司 | Efficient heat conduction glue for LEDs |
CN105524590A (en) * | 2016-02-18 | 2016-04-27 | 广州市白云化工实业有限公司 | Single-component RTV (room temperature vulcanization) silicone sealing material for LED lamp and preparation method of single-component RTV silicone sealing material |
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CN106753205B (en) * | 2017-01-11 | 2020-05-22 | 湖南博翔新材料有限公司 | Epoxy modified organic silicon pouring sealant with low viscosity and high heat conductivity and application thereof |
CN107828386A (en) * | 2017-10-11 | 2018-03-23 | 上海阿莱德实业股份有限公司 | One kind has vulcanized by moisture shaping one pack system high heat conduction calking boundary material and preparation method thereof |
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Application publication date: 20120215 |