CN103171207B - Heat sink material and preparation method thereof - Google Patents
Heat sink material and preparation method thereof Download PDFInfo
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- CN103171207B CN103171207B CN201310070809.7A CN201310070809A CN103171207B CN 103171207 B CN103171207 B CN 103171207B CN 201310070809 A CN201310070809 A CN 201310070809A CN 103171207 B CN103171207 B CN 103171207B
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Abstract
The invention discloses a heat sink material and a preparation method thereof. The heat sink material comprises a graphite substrate. A silicon carbide layer is metallurgically bonded on the top of the graphite substrate. The graphite substrate has a thermal conductivity greater than 150w/(m.K), and is a graphite sheet, or a graphite composite sheet or graphite composite board with graphite as a raw material. According to the invention, graphite is bonded with silicon carbide, such that a graphite-silicon carbide heat sink material with a metallurgically bonded interface is formed. The material has excellent insulation, excellent thermal conductivity, and relatively low expansion coefficient. With a graphite-silicon carbide coating method, the coating forms metallurgical bonding with the graphite substrate, such that material compactness and bonding degree are improved, and material thermal conductivity-heat dissipation performance is further improved.
Description
Technical field
The present invention relates to a kind of heat sink material for LED heat conduction-heat radiation, espespecially a kind of heat sink material and preparation method thereof.
Background technology
Constantly perfect along with semiconductor technology and manufacturing process, luminous flux and the light extraction efficiency of LED improve constantly, and power-type LED has been widely used in daily life and industrial production.But for great power LED, chip power density is large, and large caloric value is had higher requirement to its heat sink material undoubtedly.
The heat radiation of conventional LED chip, its structure as shown in Figure 1, is provided with substrate 3'(and heat sink material in the below of LED chip 1'), the below of substrate 3' is connected with heat abstractor 4' again, the heat of LED chip 1' is transmitted to heat abstractor 4' by substrate 3', then is distributed by heat abstractor 4'.
In system radiating, especially power-type LED, selects suitable substrate, has material impact to its thermal diffusivity and reliability.The baseplate material of great power LED must have high electrical insulation capability, high stability, high heat conductance, the thermal coefficient of expansion close with chip and planarization and higher intensity.
Current conventional substrate material adopts minority can meet the metal or alloy material of high heat conductance substantially.But, in order to ensure electrical insulating property, and chip is fully contacted with substrate, need between chip 1' and substrate 3', apply high molecular polymer deielectric-coating 2', but, the thermal conductivity of this high molecular polymer deielectric-coating 2' is usually very low, define thermal resistance interface, and temperature rising can cause degradation between chip and substrate.In addition, be mechanical bond between this high molecular polymer deielectric-coating 2' and substrate, in conjunction with defective tightness, also have impact on heat conducting performance.
Graphite is a kind of well heat sink material, and its thermal conductivity factor is high, can reach 100w/ (mK) ~ 1000w/ (mK).Because graphite has the crystal structure of hexagonal crystal system and layered distribution, determine graphite and there is special thermal conduction characteristic.This thermal conduction characteristic refers to that graphite bedding angle thermal conductivity factor is tens times perpendicular to bedding angle.Although graphite material has excellent thermal conductivity, it is the good conductor of electricity, and mechanical strength is not enough, and the requirement that some intensity are higher is difficult to realize.On the other hand, carbofrax material has excellent performance, the advantage that with low cost, resistance is large, and its thermal coefficient of expansion is 3.7 × l0
-6/ DEG C, thermal conductivity is 80w/ (mK) ~ 270w/ (mK).Therefore, if graphite and carborundum are combined, then can obtain the heat sink material with excellent insulating properties, thermal conductivity and the lower coefficient of expansion, this case produces therefrom.
Summary of the invention
Not only insulating barrier for conventional substrate heat sink material is combined the technical deficiency part existed with heat conduction-heat dissipating layer, technical problem to be solved by this invention is to provide a kind of and insulate but also can the heat sink material of heat conduction-heat radiation.
Another technical problem to be solved by this invention is to provide that a kind of technique is simple, the preparation method of the heat sink material of low cost.
For solving the problems of the technologies described above, technical solution of the present invention is:
A kind of heat sink material, comprise graphite matrix, be combined with one deck silicon carbide layer at the top of this graphite matrix in metallurgical binding mode, this graphite matrix is that thermal conductivity factor is greater than the graphite sheet of 150w/ (mK) or take graphite as graphite composite sheet or the graphite composite plate material of raw material.
The preparation method of described heat sink material, comprises the following steps:
(1) batching slurrying: pulping raw material comprises silicon carbide micro-powder 30 ~ 60%, silica flour 20 ~ 60% and carbon source 10 ~ 20% in mass ratio; Wherein said carbon source comprises two parts, and a part is from one or more combinations in graphite powder, carbon black, petroleum coke, and this part addition is 8 ~ 15%, and another part is from organic bond, and addition is 2 ~ 5%; Above-mentioned organic bond is added appropriate water to saturated in described ratio, and 50 ~ 80 DEG C of heating water baths, obtain clear solution; Other raw materials weighed up in proportion are mixed with above-mentioned solution, stirs and obtain mixed slurry;
(2) graphite matrix decontamination and activation process: graphite matrix is placed in deoil liquid or industrial alcohol or acetone of alkalescence and cleans, then adopt chemical activation liquid to the graphite matrix activation process 5 ~ 15min after washing after deoiling, to increase the contact area of coating and matrix material; Finally, to graphite matrix Ultrasonic Cleaning 10 ~ 20min;
(3) apply: mixed slurry obtained for step (1) is uniformly coated on graphite matrix that step (2) process on the surface, with 60 ~ 120 DEG C of maintenances 1 ~ 10 hour in baking oven, obtains graphite-silicon carbide compound base substrate;
(4) reaction-sintered: above-mentioned dried graphite-silicon carbide compound base substrate is placed in sintering furnace, under inert gas or the protection of flowing hydrogen atmosphere, is warming up to 1300 ~ 1500 DEG C of sintering with 2 ~ 20 DEG C of speed per minute, is incubated 1 ~ 4 hour; After Temperature fall, goods are taken out in blow-on, obtain described heat sink material.
Comprise step (5) further: described goods are placed in insulation process in 1 ~ 2 hour under the sintering furnace inert gas shielding of 2000 ~ 2500 DEG C or vacuum, the more complete densification of coat of silicon carbide of the heat sink material of gained after cooling.
Comprise step (6) post processing further: required to be processed into required shape, thickness according to encapsulation by the graphite-coat of silicon carbide heat sink material of step (4) or step (5) gained, and effects on surface carries out polishing.
In described step (1), described organic bond is one or more combinations in CMC, methylcellulose, polyvinyl alcohol.
In described step (1), described silicon carbide micro-powder is the powder constituent of 0.1 ~ 10 μm primarily of granularity; Chemical composition requires: SiC content is greater than 98%.
In described step (1), described silica flour adopts purity to be greater than 99%, granularity is 0.1 ~ 10 μm of object industrial silica fume.
In described step (2), described chemical activation liquid is acid solution; As can be salpeter solution or 30 ~ 40% sulfuric acid solutions of 20 ~ 30%.
After adopting such scheme, because graphite and carborundum combine by the present invention, form the heat sink material with metallurgical bonding interface of graphite-carborundum, and this material have excellent insulating properties, thermal conductivity and the lower coefficient of expansion.
And the present invention adopts graphite-coat of silicon carbide method, silicon melts and reacts Formed SiClx with material with carbon element (comprising graphite matrix), makes coating and graphite matrix form metallurgical binding.Coat of silicon carbide is very little on the impact of the heat conductivility of graphite sheet, even do not affect.The processing method finally adopting high temperature to sinter again improves density and the conjugation of material, thus improves the heat conductivility of material further.
The raw material that the present invention adopts and proportioning, scientific and reasonable, the overall thermal conductivity of obtained heat sink material is at more than 150w/ (mK), and SiC layer density reaches 95 ~ 99%, the density of material own is low simultaneously, can meet the requirement of LED heat sink material lightweight, high thermal conductance.And coat of silicon carbide has high-insulativity, can directly LED chip be fitted on coat of silicon carbide, simplify encapsulating structure, reduce costs.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of conventional LED chip radiator structure;
Fig. 2 is the structural representation of heat sink material of the present invention.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Disclosed is a kind of heat sink material, as shown in Figure 1, this heat sink material comprises graphite matrix 1, be combined with one deck silicon carbide layer 2 at the top of this graphite matrix 1 in metallurgical binding mode, the thermal conductivity factor that this graphite matrix 1 is is greater than the graphite sheet of 150w/ (mK) or take graphite as graphite composite sheet or the graphite composite plate material of raw material.Because silicon carbide layer 2 has high-insulativity, therefore, it is possible to directly by team of LED chip 3 side of being fitted in silicon carbide layer 2, simplify encapsulating structure, reduce cost.
Present invention further teaches a kind of preparation method of above-mentioned heat sink material, specific embodiment is as follows.
embodiment one
1. batching slurrying: silicon carbide powder, silica flour, graphite powder and methylcellulose are got powder according to the ratio of mass ratio 37:44:14:5, and wherein particle diameter is 3 μm of silicon carbide powders and 10 μm of silicon carbide powder mass ratios is 2:1.Take out methylcellulose and add a certain amount of water to saturated, heating water bath 60 DEG C, stirs and obtains clear solution.Then silicon carbide powder, silica flour, graphite powder mixing are added in solution and be put into mixer and carry out stirring after 1 hour, take out slurry.
2. graphite matrix decontamination and activation process: adopt acetone to deoil process to graphite matrix at normal temperatures, wash.Then HNO is adopted
3(20%) to the graphite matrix activation 10min after deoiling, after washing, to increase the contact area of coating and matrix material.Finally to graphite matrix Ultrasonic Cleaning 15min.
3. apply: obtained mixed slurry is uniformly coated on the graphite matrix that processed on the surface, thickness is needed to control voluntarily by technique, if anisotropic graphite monocrystalline, the face of selection must be perpendicular to graphite bedding angle.In baking oven, 80 DEG C keep drying for 3 hours.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in ordinary sinter stove, is warming up to 1000 DEG C with 10 DEG C of speed per minute under argon shield, is more then warming up to 1350 DEG C of sintering with 5 DEG C of speed per minute, is incubated 3 hours.Temperature fall is to less than 120 DEG C, and goods are taken out in blow-on.
5. high-temperature process: above-mentioned made graphite-Silicon carbide composite bodies of obtaining and heat sink material can be carried out high-temperature process again, such performance is better.Specific practice is: said products is placed in 2200 DEG C, Ar-sintering stove insulation 1.5 hours, such coat of silicon carbide is finer and close.
6. post processing: the graphite-Silicon carbide composite bodies (heat sink material) of step (4) or step (5) gained also can require to be processed into required shape, thickness according to encapsulation, and effects on surface carries out polishing, LED chip can be made with it like this to combine tightr.
The sample that this method obtains, SiC layer density reaches 98%, and overall thermal conductivity is 225w/ (mK).
embodiment two
1. batching slurrying: silicon carbide powder, silica flour, carbon black and polyvinyl alcohol are got powder according to the ratio of mass ratio 50:33:13:4, and wherein silicon carbide powder particle diameter is 0.5 μm.Take out polyvinyl alcohol and add a certain amount of water to saturated, heating water bath 80 DEG C, stirs and obtains clear solution.Then silicon carbide powder, silica flour, carbon black mixing are added in solution and be put into mixer and carry out stirring after 0.5 hour, take out slurry.
2. graphite matrix decontamination and activation process: adopt alcohol to deoil process to graphite matrix at normal temperatures, wash.Then adopt sulfuric acid (30%) to the graphite matrix activation 10min after deoiling, washing, to increase the contact area of coating and matrix material.Finally, to graphite matrix Ultrasonic Cleaning 10min.
3. apply: obtained mixed slurry is uniformly coated on the graphite matrix that processed on the surface, thickness is needed to control voluntarily by technique.In baking oven, 120 DEG C keep drying for 1 hour.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in ordinary sinter stove, is warming up to 1000 DEG C with 10 DEG C of speed per minute under argon shield, is more then warming up to 1490 DEG C of sintering with 5 DEG C of speed per minute, is incubated 3 hours.Temperature fall is to less than 120 DEG C, and goods are taken out in blow-on.
5. high-temperature process: said products is placed in 2400 DEG C, Ar-sintering stove insulation 1 hour, coat of silicon carbide is finer and close.
6. post processing: graphitic carbonaceous silicon coating material step (4) or step (5) obtained requires to be processed into required shape, thickness and surface finish process according to encapsulation.
The sample that this method obtains, SiC layer density reaches 98.5%, and overall thermal conductivity is 232w/ (mK).
embodiment three
1. batching slurrying: silicon carbide powder, silica flour, carbon black, methylcellulose and polyvinyl alcohol are got powder according to the ratio of mass ratio 60:24:12:2:2, and wherein silicon carbide powder particle diameter is 5 μm.Taking-up methylcellulose and polyvinyl alcohol add a certain amount of water to saturated, and heating water bath 80 DEG C, stirs and obtain clear solution.Then silicon carbide powder, silica flour, carbon black mixing are added in solution and be put into mixer and carry out stirring after 0.5 hour, take out slurry.
2. graphite matrix decontamination and activation process: adopt alcohol to deoil process to graphite matrix at normal temperatures, wash.Then adopt nitric acid (30%) to the graphite matrix activation 10min after deoiling, washing, to increase the contact area of coating and matrix material.Finally, to graphite matrix Ultrasonic Cleaning 10min.
3. apply: obtained mixed slurry is uniformly coated on the graphite matrix that processed on the surface, thickness is needed to control voluntarily by technique.In baking oven, 120 DEG C keep drying for 1 hour.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in ordinary sinter stove, is warming up to 1000 DEG C with 10 DEG C of speed per minute under argon shield, is more then warming up to 1490 DEG C of sintering with 5 DEG C of speed per minute, is incubated 3 hours.Temperature fall is to less than 120 DEG C, and goods are taken out in blow-on.
5. high-temperature process: goods are placed in 2400 DEG C, Ar-sintering stove insulation 1 hour, coat of silicon carbide is finer and close.
6. post processing: the graphitic carbonaceous silicon coating material obtained is required to be processed into required shape, thickness and surface finish process according to encapsulation by step (4) or step (5).
The sample that this method obtains, SiC layer density reaches 99%, and overall thermal conductivity is 238w/ (mK).
embodiment four
1. batching slurrying: silicon carbide powder, silica flour, graphite powder and methylcellulose are got powder according to the ratio of mass ratio 50:34:12:4, and wherein particle diameter is 3 μm of silicon carbide powders and 10 μm of silicon carbide powder mass ratios is 2:1.Take out methylcellulose and add a certain amount of water to saturated, heating water bath 60 DEG C, stirs and obtains clear solution.Then silicon carbide powder, silica flour, graphite powder mixing are added in solution and be put into mixer and carry out stirring after 1 hour, take out slurry.
2. graphite matrix decontamination and activation process: adopt acetone to deoil process to graphite matrix at normal temperatures, wash.Then HNO is adopted
3(30%) to the graphite matrix activation 10min after deoiling, washing, to increase the contact area of coating and matrix material.Finally, to graphite matrix Ultrasonic Cleaning 15min.
3. apply: obtained mixed slurry is uniformly coated on the graphite matrix that processed on the surface, thickness is needed to control voluntarily by technique.In baking oven, 80 DEG C keep drying for 3 hours.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in ordinary sinter stove, is warming up to 1000 DEG C with 10 DEG C of speed per minute under argon shield, is more then warming up to 1480 DEG C of sintering with 5 DEG C of speed per minute, is incubated 2 hours.Temperature fall is to 120 DEG C, and goods are taken out in blow-on.
5. high-temperature process: sintering furnace said products being placed in 2200 DEG C, be incubated 1.5 hours under vacuo or under protective atmosphere, coat of silicon carbide is finer and close.
6. post processing: graphitic carbonaceous silicon coating material step (4) or step (5) obtained requires to be processed into required shape, thickness and surface finish process according to encapsulation.
The sample that this method obtains, SiC layer density reaches 98%, and overall thermal conductivity is 225w/ (mK).
embodiment five
1. batching slurrying: silicon carbide micro-powder (ratio that granularity is 5 μm is 10 μm with granularity is 2:1), silica flour, graphite and methylcellulose are got powder according to mass ratio 41:42:12:5 ratio, and produced slip by method described in embodiment four.
2 ~ 5 steps are identical with above-described embodiment four.
The sample that this method is produced, SiC layer density is 97%, and bulk thermal conductivity is 210w/ (mK), and thermal coefficient of expansion is 4.6 × 10-6/ DEG C.
The above, be only preferred embodiment of the present invention, is not used for limiting scope of the invention process.Therefore the change in every case done according to claim of the present invention and description or modification, all should belong within scope that patent of the present invention contains.
Claims (8)
1. a preparation method for heat sink material, is characterized in that comprising the following steps:
(1) batching slurrying: pulping raw material comprises silicon carbide micro-powder 30 ~ 60%, silica flour 20 ~ 60% and carbon source 10 ~ 20% in mass ratio; Wherein said carbon source comprises two parts, and a part is from one or more combinations in graphite powder, carbon black, petroleum coke, and this part addition is 8 ~ 15%, and another part is from organic bond, and addition is 2 ~ 5%; Above-mentioned organic bond is added appropriate water to saturated in described ratio, and 50 ~ 80 DEG C of heating water baths, obtain clear solution; Other raw materials weighed up in proportion are mixed with above-mentioned solution, stirs and obtain mixed slurry;
(2) graphite matrix decontamination and activation process: graphite matrix is placed in deoil liquid or industrial alcohol or acetone of alkalescence and cleans, then adopt chemical activation liquid to the graphite matrix activation process 5 ~ 15min after washing after deoiling, to increase the contact area of coating and matrix material; Finally, to graphite matrix Ultrasonic Cleaning 10 ~ 20min;
(3) apply: mixed slurry obtained for step (1) is uniformly coated on graphite matrix that step (2) process on the surface, with 60 ~ 120 DEG C of maintenances 1 ~ 10 hour in baking oven, obtains graphite-silicon carbide compound base substrate;
(4) reaction-sintered: above-mentioned dried graphite-silicon carbide compound base substrate is placed in sintering furnace, under inert gas or the protection of flowing hydrogen atmosphere, is warming up to 1300 ~ 1500 DEG C of sintering with 2 ~ 20 DEG C of speed per minute, is incubated 1 ~ 4 hour; After Temperature fall, goods are taken out in blow-on, obtain described heat sink material; This heat sink material comprises graphite matrix, be combined with one deck silicon carbide layer at the top of this graphite matrix in metallurgical binding mode, this graphite matrix is that thermal conductivity factor is greater than the graphite sheet of 150w/ (mK) or take graphite as graphite composite sheet or the graphite composite plate material of raw material.
2. the preparation method of a kind of heat sink material according to claim 1; it is characterized in that comprising high temperature processing step further: described goods are placed in insulation process in 1 ~ 2 hour under the sintering furnace inert gas shielding of 2000 ~ 2500 DEG C or vacuum, the more complete densification of coat of silicon carbide of the heat sink material of gained after cooling.
3. the preparation method of a kind of heat sink material according to claim 1 and 2, it is characterized in that comprising post-processing step further: the graphite obtained-coat of silicon carbide heat sink material is required to be processed into required shape, thickness according to encapsulation, and effects on surface carries out polishing.
4. the preparation method of a kind of heat sink material according to claim 1 and 2, is characterized in that: in described step (1), and described organic bond is one or more combinations in CMC, methylcellulose, polyvinyl alcohol.
5. the preparation method of a kind of heat sink material according to claim 1 and 2, is characterized in that: in described step (1), and described silicon carbide micro-powder is the powder constituent of 0.1 ~ 10 μm primarily of granularity; Chemical composition requires: SiC content is greater than 98%.
6. the preparation method of a kind of heat sink material according to claim 1 and 2, is characterized in that: in described step (1), the industrial silica fume that described silica flour adopts purity to be greater than 99%, granularity is 0.1 ~ 10 μm.
7. the preparation method of a kind of heat sink material according to claim 1 and 2, is characterized in that: in described step (2), and described chemical activation liquid is acid solution.
8. the preparation method of a kind of heat sink material according to claim 7, is characterized in that: described chemical activation liquid is salpeter solution or 30 ~ 40% sulfuric acid solutions of 20 ~ 30%.
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CN106058029A (en) * | 2016-07-26 | 2016-10-26 | 黄宇 | Heat sink material for semiconductors |
CN106206922A (en) * | 2016-07-26 | 2016-12-07 | 黄宇 | A kind of novel heat sink material |
CN106129239A (en) * | 2016-07-26 | 2016-11-16 | 黄宇 | A kind of novel high-performance heat sink material |
CN105957951A (en) * | 2016-07-26 | 2016-09-21 | 黄宇 | Novel heat sink material for semiconductors |
CN106318337A (en) * | 2016-07-26 | 2017-01-11 | 黄宇 | Heat sink material |
CN106129238A (en) * | 2016-07-26 | 2016-11-16 | 黄宇 | A kind of high-performance heat sink material |
CN111348821A (en) * | 2018-12-21 | 2020-06-30 | 财团法人工业技术研究院 | Graphite mold for glass shaping and manufacturing method thereof |
CN111463113B (en) * | 2020-05-25 | 2023-04-11 | 哈尔滨晶创科技有限公司 | Processing method for protecting silicon carbide surface in semi-insulating SiC ion doping annealing process |
CN114349513B (en) * | 2022-01-19 | 2023-03-17 | 东莞市鸿亿导热材料有限公司 | Insulating radiating fin preparation process and insulating radiating fin |
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