CN103171207A - Heat sink material and preparation method thereof - Google Patents
Heat sink material and preparation method thereof Download PDFInfo
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- CN103171207A CN103171207A CN2013100708097A CN201310070809A CN103171207A CN 103171207 A CN103171207 A CN 103171207A CN 2013100708097 A CN2013100708097 A CN 2013100708097A CN 201310070809 A CN201310070809 A CN 201310070809A CN 103171207 A CN103171207 A CN 103171207A
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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.Yet 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 tradition LED chip, its structure as shown in Figure 1, being provided with substrate 3'(below LED chip 1' is heat sink material), 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'.
Aspect system radiating, especially power-type LED, select suitable substrate, and its thermal diffusivity and reliability are had material impact.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.
The conventional substrate material adopts minority can satisfy the metal or alloy material of high heat conductance basically at present.But, in order to ensure electrical insulating property, and chip is fully contacted with substrate, need to apply high molecular polymer deielectric-coating 2' between chip 1' and substrate 3', but, the thermal conductivity of this high molecular polymer deielectric-coating 2' is usually very low, formed the thermal resistance interface between chip and substrate, and the temperature rising can cause degradation.In addition, be mechanical bond between this high molecular polymer deielectric-coating 2' and substrate, in conjunction with defective tightness, also affected heat conducting performance.
Graphite is a kind of good heat sink material, and its thermal conductivity factor is high, can reach 100w/ (mK) ~ 1000w/ (mK).The crystal structure that has hexagonal crystal system and layered arrangement due to graphite has determined that graphite has 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 advantages of excellent performance, with low cost, resistance is large, and its thermal coefficient of expansion is 3.7 * l0
-6/ ℃, thermal conductivity is 80w/ (mK)～270w/ (mK).Therefore, if with graphite and carborundum combination, can obtain having good insulating properties, the heat sink material of thermal conductivity and the lower coefficient of expansion, this case produces therefrom.
Summary of the invention
Be combined for the insulating barrier of conventional substrate heat sink material the technical deficiency part that exists with heat conduction-heat dissipating layer, technical problem to be solved by this invention is to provide the heat sink material that a kind of i.e. insulation again can heat conduction-heat radiation.
Another technical problem to be solved by this invention be to provide a kind of technique simply, the preparation method of heat sink material cheaply.
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, top at this graphite matrix is combined with one deck silicon carbide layer in the metallurgical binding mode, and this graphite matrix is that thermal conductivity factor is greater than graphite sheet or the graphite composite sheet take graphite as raw material or the graphite composite plate material of 150w/ (mK).
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%; Add appropriate water to saturated in described ratio above-mentioned organic bond, 50 ~ 80 ℃ of heating water baths obtain clear solution; Other raw materials that weigh up are in proportion mixed with mentioned solution, and stirring obtains mixed slurry;
(2) graphite matrix decontamination and activation process: graphite matrix is placed in deoil liquid or industrial alcohol or acetone of alkalescence 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; At last, to graphite matrix Ultrasonic Cleaning 10 ~ 20min;
(3) apply: on the mixed slurry that step (1) is made is uniformly coated on that step (2) processed graphite matrix surface, with 60 ~ 120 ℃ of maintenances 1 ~ 10 hour, obtain graphite-silicon carbide compound base substrate in baking oven;
(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 ℃ of sintering with 2 ~ 20 ℃ of speed per minute, be incubated 1 ~ 4 hour; Naturally after the cooling, goods are taken out in blow-on, obtain described heat sink material.
Further comprise step (5): described goods are placed under the sintering furnace inert gas shielding of 2000 ~ 2500 ℃ or vacuum are incubated processing in 1 ~ 2 hour, the more complete densification of coat of silicon carbide of the heat sink material of gained after cooling.
Further comprise step (6) post processing: the graphite of step (4) or step (5) gained-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.
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 mainly the powder constituent of 0.1 ~ 10 um by granularity; Chemical composition requires: SiC content is greater than 98%.
In described step (1), described silica flour adopt purity greater than 99%, granularity is 0.1 ~ 10 um purpose industrial silica fume.
In described step (2), described chemical activation liquid is acid solution; As can be 20 ~ 30% salpeter solution or 30 ~ 40% sulfuric acid solutions.
After adopting such scheme, with graphite and carborundum combination, form the heat sink material with metallurgical bonding interface of graphite-carborundum, and this material have good insulating properties, thermal conductivity and the lower coefficient of expansion due to the present invention.
And the present invention adopts graphite-coat of silicon carbide method, and silicon melts also and material with carbon element (comprising graphite matrix) reaction Formed SiClx, makes coating and graphite matrix formation metallurgical binding.Coat of silicon carbide is very little on the heat conductivility impact of graphite sheet, not even impact.Adopt at last high temperature again the processing method of sintering improved density and the conjugation of material, thereby further promoted the heat conductivility of material.
Raw material and proportioning that the present invention adopts, scientific and reasonable, the overall thermal conductivity of the heat sink material that makes is more than 150w/ (mK), and SiC layer density reaches 95 ~ 99%, and the density of material own is low simultaneously, can satisfy 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, simplifies encapsulating structure, reduces costs.
Description of drawings
Fig. 1 is the schematic diagram of traditional LED chip radiator structure;
Fig. 2 is the structural representation of heat sink material of the present invention.
The specific embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
Disclosed is a kind of heat sink material, as shown in Figure 1, this heat sink material comprises graphite matrix 1, top at this graphite matrix 1 is combined with one deck silicon carbide layer 2 in the metallurgical binding mode, and the thermal conductivity factor that this graphite matrix 1 is is greater than graphite sheet or the graphite composite sheet take graphite as raw material or the graphite composite plate material of 150w/ (mK).Because silicon carbide layer 2 has high-insulativity, therefore can simplify encapsulating structure directly with on LED chip 3 side of being fitted in team silicon carbide layers 2, reduced cost.
The present invention has also disclosed a kind of preparation method of above-mentioned heat sink material, and 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 that 3um silicon carbide powder and 10um silicon carbide powder mass ratio are 2:1.Take out methylcellulose and add a certain amount of water to saturated, 60 ℃ of heating water baths, stirring obtains clear solution.Then silicon carbide powder, silica flour, graphite powder are mixed add be put into mixer in solution and stir 1 hour after, take out slurry.
2. graphite matrix decontamination and activation process: adopt acetone at normal temperatures to graphite matrix processings of deoiling, wash.Then adopt HNO
3(20%) to the activation of the graphite matrix after deoiling 10min, washing afterwards is to increase the contact area of coating and matrix material.At last to graphite matrix Ultrasonic Cleaning 15min.
3. apply: the mixed slurry that makes is uniformly coated on the graphite matrix surface of processing, and thickness is by the control voluntarily of technique needs, if anisotropic graphite monocrystalline, the face of selection must be perpendicular to the graphite bedding angle.80 ℃ keep oven dry in 3 hours in baking oven.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in the ordinary sinter stove, is warming up to 1000 ℃ with 10 ℃ of speed per minute under argon shield, more then be warming up to 1350 ℃ of sintering with 5 ℃ of speed per minute, be incubated 3 hours.Naturally cool to below 120 ℃, goods are taken out in blow-on.
5. high-temperature process: can be that heat sink material carries out high-temperature process again with the above-mentioned made graphite that obtains-silicon carbide compound body, performance be better like this.Specific practice is: said products is placed in 2200 ℃ of insulations of Ar-sintering stove 1.5 hours, and coat of silicon carbide is finer and close like this.
6. post processing: the graphite of step (4) or step (5) gained-silicon carbide compound body (heat sink material) also can require to be processed into required shape, thickness according to encapsulation, and effects on surface carries out polishing, can make like this LED chip and its in conjunction with 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 the silicon carbide powder particle diameter is 0.5um.Take out polyvinyl alcohol and add a certain amount of water to saturated, 80 ℃ of heating water baths, stirring obtains clear solution.Then silicon carbide powder, silica flour, carbon black are mixed add be put into mixer in solution and stir 0.5 hour after, take out slurry.
2. graphite matrix decontamination and activation process: adopt alcohol at normal temperatures to graphite matrix processings of deoiling, wash.Then adopt sulfuric acid (30%) to the activation of the graphite matrix after deoiling 10min, washing is to increase the contact area of coating and matrix material.At last, to graphite matrix Ultrasonic Cleaning 10min.
3. apply: the mixed slurry that makes is uniformly coated on the graphite matrix surface of processing, and thickness is by the control voluntarily of technique needs.120 ℃ keep oven dry in 1 hour in baking oven.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in the ordinary sinter stove, is warming up to 1000 ℃ with 10 ℃ of speed per minute under argon shield, more then be warming up to 1490 ℃ of sintering with 5 ℃ of speed per minute, be incubated 3 hours.Naturally cool to below 120 ℃, goods are taken out in blow-on.
5. high-temperature process: said products is placed in 2400 ℃ of insulations of Ar-sintering stove 1 hour, and coat of silicon carbide is finer and close.
6. post processing: the graphitic carbon SiClx coating material that step (4) or step (5) are obtained requires to be processed into required shape, thickness and surface finish according to encapsulation and processes.
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 the silicon carbide powder particle diameter is 5um.Take out methylcellulose and polyvinyl alcohol and add a certain amount of water to saturated, 80 ℃ of heating water baths, stirring obtains clear solution.Then silicon carbide powder, silica flour, carbon black are mixed add be put into mixer in solution and stir 0.5 hour after, take out slurry.
2. graphite matrix decontamination and activation process: adopt alcohol at normal temperatures to graphite matrix processings of deoiling, wash.Then adopt nitric acid (30%) to the activation of the graphite matrix after deoiling 10min, washing is to increase the contact area of coating and matrix material.At last, to graphite matrix Ultrasonic Cleaning 10min.
3. apply: the mixed slurry that makes is uniformly coated on the graphite matrix surface of processing, and thickness is by the control voluntarily of technique needs.120 ℃ keep oven dry in 1 hour in baking oven.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in the ordinary sinter stove, is warming up to 1000 ℃ with 10 ℃ of speed per minute under argon shield, more then be warming up to 1490 ℃ of sintering with 5 ℃ of speed per minute, be incubated 3 hours.Naturally cool to below 120 ℃, goods are taken out in blow-on.
5. high-temperature process: goods are placed in 2400 ℃ of insulations of Ar-sintering stove 1 hour, and coat of silicon carbide is finer and close.
6. post processing: step (4) or step (5) are required to be processed into required shape, thickness and surface finish processing with the graphitic carbon SiClx coating material that obtains according to encapsulation.
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 that 3um silicon carbide powder and 10um silicon carbide powder mass ratio are 2:1.Take out methylcellulose and add a certain amount of water to saturated, 60 ℃ of heating water baths, stirring obtains clear solution.Then silicon carbide powder, silica flour, graphite powder are mixed add be put into mixer in solution and stir 1 hour after, take out slurry.
2. graphite matrix decontamination and activation process: adopt acetone at normal temperatures to graphite matrix processings of deoiling, wash.Then adopt HNO
3(30%) to the activation of the graphite matrix after deoiling 10min, washing is to increase the contact area of coating and matrix material.At last, to graphite matrix Ultrasonic Cleaning 15min.
3. apply: the mixed slurry that makes is uniformly coated on the graphite matrix surface of processing, and thickness is by the control voluntarily of technique needs.80 ℃ keep oven dry in 3 hours in baking oven.
4. reaction-sintered: above-mentioned dried graphite-silicon carbide green body is placed in the ordinary sinter stove, is warming up to 1000 ℃ with 10 ℃ of speed per minute under argon shield, more then be warming up to 1480 ℃ of sintering with 5 ℃ of speed per minute, be incubated 2 hours.Naturally cool to 120 ℃, goods are taken out in blow-on.
5. high-temperature process: said products is placed in the sintering furnace of 2200 ℃, under vacuum or under protective atmosphere, insulation is 1.5 hours, and coat of silicon carbide is finer and close.
6. post processing: the graphitic carbon SiClx coating material that step (4) or step (5) are obtained requires to be processed into required shape, thickness and surface finish according to encapsulation and processes.
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 (granularity be 5um be 10um ratio is 2:1 with granularity), silica flour, graphite and methylcellulose are got powder according to mass ratio 41:42:12:5 ratio, and produce slip by the described method of 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/ ℃.
The above is only preferred embodiment of the present invention, is not to limit scope of the invention process.Therefore variation or the modification in every case done according to claim of the present invention and specification are within all should belonging to the scope that patent of the present invention contains.
Claims (9)
1. heat sink material, it is characterized in that: comprise graphite matrix, top at this graphite matrix is combined with one deck silicon carbide layer in the metallurgical binding mode, and this graphite matrix is that thermal conductivity factor is greater than graphite sheet or the graphite composite sheet take graphite as raw material or the graphite composite plate material of 150w/ (mK).
2. the preparation method of heat sink material according to claim 1, 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%; Add appropriate water to saturated in described ratio above-mentioned organic bond, 50 ~ 80 ℃ of heating water baths obtain clear solution; Other raw materials that weigh up are in proportion mixed with mentioned solution, and stirring obtains mixed slurry;
(2) graphite matrix decontamination and activation process: graphite matrix is placed in deoil liquid or industrial alcohol or acetone of alkalescence 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; At last, to graphite matrix Ultrasonic Cleaning 10 ~ 20min;
(3) apply: on the mixed slurry that step (1) is made is uniformly coated on that step (2) processed graphite matrix surface, with 60 ~ 120 ℃ of maintenances 1 ~ 10 hour, obtain graphite-silicon carbide compound base substrate in baking oven;
(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 ℃ of sintering with 2 ~ 20 ℃ of speed per minute, be incubated 1 ~ 4 hour; Naturally after the cooling, goods are taken out in blow-on, obtain described heat sink material.
3. the preparation method of a kind of heat sink material according to claim 2; it is characterized in that further comprising high temperature processing step: described goods are placed under the sintering furnace inert gas shielding of 2000 ~ 2500 ℃ or vacuum are incubated processing in 1 ~ 2 hour, the more complete densification of coat of silicon carbide of the heat sink material of gained after cooling.
4. the preparation method of according to claim 2 or 3 described a kind of heat sink materials, it is characterized in that further comprising post-processing step: the graphite that obtains-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.
5. the preparation method of according to claim 2 or 3 described a kind of heat sink materials, it is characterized in that: in described step (1), described organic bond is one or more combinations in CMC, methylcellulose, polyvinyl alcohol.
6. the preparation method of according to claim 2 or 3 described a kind of heat sink materials, it is characterized in that: in described step (1), described silicon carbide micro-powder is mainly the powder constituent of 0.1 ~ 10 um by granularity; Chemical composition requires: SiC content is greater than 98%.
7. the preparation method of according to claim 2 or 3 described a kind of heat sink materials is characterized in that: in described step (1), described silica flour adopt purity greater than 99%, granularity is 0.1 ~ 10 um purpose industrial silica fume.
8. the preparation method of according to claim 2 or 3 described a kind of heat sink materials, it is characterized in that: in described step (2), described chemical activation liquid is acid solution.
9. the preparation method of a kind of heat sink material according to claim 8, it is characterized in that: described chemical activation liquid is 20 ~ 30% salpeter solution or 30 ~ 40% sulfuric acid solutions.
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| CN105957951A (en) * | 2016-07-26 | 2016-09-21 | 黄宇 | Novel heat sink material for semiconductors |
| CN106058029A (en) * | 2016-07-26 | 2016-10-26 | 黄宇 | Heat sink material for semiconductors |
| CN106129239A (en) * | 2016-07-26 | 2016-11-16 | 黄宇 | A kind of novel high-performance heat sink material |
| CN106129238A (en) * | 2016-07-26 | 2016-11-16 | 黄宇 | A kind of high-performance heat sink material |
| CN106206922A (en) * | 2016-07-26 | 2016-12-07 | 黄宇 | A kind of novel heat sink material |
| CN106318337A (en) * | 2016-07-26 | 2017-01-11 | 黄宇 | 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 |
| CN111463113A (en) * | 2020-05-25 | 2020-07-28 | 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 |
| CN114349513A (en) * | 2022-01-19 | 2022-04-15 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105957951A (en) * | 2016-07-26 | 2016-09-21 | 黄宇 | Novel heat sink material for semiconductors |
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| 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 |
| CN111463113A (en) * | 2020-05-25 | 2020-07-28 | 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 |
| 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 |
| CN114349513A (en) * | 2022-01-19 | 2022-04-15 | 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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