CN105566918A - Silicon sheet and preparation method thereof - Google Patents
Silicon sheet and preparation method thereof Download PDFInfo
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- CN105566918A CN105566918A CN201410598318.4A CN201410598318A CN105566918A CN 105566918 A CN105566918 A CN 105566918A CN 201410598318 A CN201410598318 A CN 201410598318A CN 105566918 A CN105566918 A CN 105566918A
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Abstract
The invention relates to a silicon sheet. The silicon sheet contains heat conduction powder, and benchmarked against the total weight of the silicon sheet, the weight of the heat conducting powder is 90-97%. The invention further relates to a preparation method of the silicon sheet, and the preparation method comprises the following steps: (1) mixing vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor and a catalyst to obtain an organic silicon cross-linking system; (2) ball-milling the heat conducting powder, the organic silicon cross-linking system and an organic solvent; (3) performing spray granulation on a mixture obtained via ball-milling to prepare a powder; (4) dry-pressing the powder; (5) enabling cross-linking reaction of a sheet obtained via dry-pressing. The invention further relates to the silicon sheet prepared by the preparation method. The silicon sheet has the advantages of simple preparation process, excellent heat conduction property, relatively low production cost and the like, and can meet the heat dissipation requirement of an electronic product module.
Description
Technical field
The present invention relates to a kind of silica gel piece, a kind of preparation method of silica gel piece, and silica gel piece prepared by the method.
Background technology
Along with the high speed development of the industries such as aviation, automobile, electronics, the requirement of people to thermally conductive material is more and more higher.Organosilicon, because of heat-resisting, the insulation of its excellence, the performance such as weather-proof, becomes the excellent carrier of heat-conductive composite material.But current organosilicon matrix material heat conductivility is poor, and need in preparation process to add coupling agent, complicated process of preparation, cost is also higher, has had a strong impact on the application of organosilicon thermally conductive material.
Therefore, the organosilicon thermally conductive material that a kind of preparation technology is simple, excellent thermal conductivity, production cost are lower is badly in need of at present.
Summary of the invention
The object of the invention is to there is complicated process of preparation, heat conductivility is poor, production cost is high defect to overcome organosilicon thermally conductive material in prior art, providing a kind of silica gel piece, a kind of preparation method of silica gel piece, and silica gel piece prepared by the method.
The present inventor finds under study for action, when the thermal conductivity of silica gel piece is more than 6W/mK, can significantly improve the heat conductivility of silica gel piece, and production cost is lower, and the preparation technology of silica gel piece is also simpler.
Therefore, to achieve these goals, on the one hand, the invention provides a kind of silica gel piece, the thermal conductivity of this silica gel piece is more than 6W/mK.
On the other hand, present invention also offers a kind of preparation method of silica gel piece, the method comprises:
(1) vinyl silicone oil, containing hydrogen silicone oil, inhibitor, catalyzer are mixed, obtain organosilicon crosslinked system;
(2) heat conduction powder, organosilicon crosslinked system and organic solvent are carried out ball milling;
(3) mixture mist projection granulating ball milling obtained, obtained powder;
(4) powder is carried out dry-pressing formed;
(5) the dry-pressing formed sheet material obtained is carried out crosslinking reaction.
The third aspect, present invention also offers silica gel piece prepared by aforesaid method.
Silica gel piece of the present invention has the advantages such as preparation technology is simple, excellent thermal conductivity, production cost are lower, can meet the cooling requirements of electronic product module.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of silica gel piece, the thermal conductivity of this silica gel piece is more than 6W/mK.
Preferably, the thermal conductivity of silica gel piece is 6-6.8W/mK.
According to silica gel piece of the present invention, as long as the thermal conductivity of silica gel piece is more than 6W/mK, the thermal conductivity of silica gel piece can be improved, but in order to improve the thermal conductivity of silica gel piece further, containing heat conduction powder in silica gel piece, with the gross weight of described silica gel piece for benchmark, the content of described heat conduction powder is 90-97 % by weight.
According to silica gel piece of the present invention, heat conduction powder in silica gel piece can be the heat conduction powder of this area routine, be preferably selected from least one in aluminum oxide, zinc oxide, silicon-dioxide, aluminium nitride, boron nitride and silicon carbide, be more preferably aluminum oxide and/or zinc oxide, the thermal conductivity of silica gel piece can be improved further, thus improve the thermal conductivity of silica gel piece further.When heat conduction powder is the mixture of aluminum oxide and zinc oxide, the weight ratio of aluminum oxide and zinc oxide is preferably 1:0.2-1.
According to silica gel piece of the present invention, wherein, the size of heat conduction powder can be the conventional specification for the preparation of the heat conduction powder of heat-conducting silica gel sheet in this area, but, in order to improve the thermal conductivity of silica gel piece further, preferably, the particle diameter of heat conduction powder is 0.5-4.5 μm.
On the other hand, present invention also offers a kind of preparation method of silica gel piece, the method comprises:
(1) vinyl silicone oil, containing hydrogen silicone oil, inhibitor, catalyzer are mixed, obtain organosilicon crosslinked system;
(2) heat conduction powder, organosilicon crosslinked system and organic solvent are carried out ball milling;
(3) mixture mist projection granulating ball milling obtained, obtained powder;
(4) powder is carried out dry-pressing formed;
(5) the dry-pressing formed sheet material obtained is carried out crosslinking reaction.
According to method of the present invention, wherein, as long as adopt aforesaid method to prepare silica gel piece, the thermal conductivity of obtained silica gel piece can be improved, but, in order to improve the thermal conductivity of obtained silica gel piece further, preferably, described heat conduction powder is selected from least one in aluminum oxide, zinc oxide, silicon-dioxide, aluminium nitride, boron nitride and silicon carbide, is more preferably aluminum oxide and/or zinc oxide, the thermal conductivity of silica gel piece can be improved further, thus improve the thermal conductivity of silica gel piece further.When heat conduction powder is the mixture of aluminum oxide and zinc oxide, the weight ratio of aluminum oxide and zinc oxide is preferably 1:0.2-1.
According to method of the present invention, wherein, the size of heat conduction powder can be the conventional specification for the preparation of the heat conduction powder of heat-conducting silica gel sheet in this area, but, in order to improve the thermal conductivity of obtained silica gel piece further, preferably, the particle diameter of heat conduction powder is 0.5-4.5 μm.
According to method of the present invention, wherein, in step (5), the condition of crosslinking reaction can be the condition of the crosslinking reaction of this area routine, but, in order to improve the thermal conductivity of obtained silica gel piece further, preferably, the condition of crosslinking reaction comprises: temperature is 130-180 DEG C, and the time is 15-60min.
According to method of the present invention, wherein, in step (1), amount ratio between vinyl silicone oil, containing hydrogen silicone oil, inhibitor, catalyzer can be the amount ratio of this area routine, such as, the weight ratio of vinyl silicone oil, containing hydrogen silicone oil, inhibitor, catalyzer can be 100:7-15:0.02-0.1:0.02-0.1.
According to method of the present invention, wherein, in step (2), heat conduction powder, amount ratio between organosilicon crosslinked system and organic solvent can be the amount ratio of this area routine, such as, the weight ratio of heat conduction powder, organosilicon crosslinked system and organic solvent can be 100:3-6:200-500.
In the present invention, organic solvent can be the organic solvent of this area routine, such as, can be selected from least one in normal hexane, acetone, diformazan Benzene and Toluene.
In the present invention, the method for ball milling and condition can adopt ball milling method and the condition of this area routine, and the condition of such as ball milling can comprise: ball milling 2-4h in ball grinder.
According to method of the present invention, wherein, in step (3), the condition of mist projection granulating can be the condition of the mist projection granulating of this area routine, and preferably, the condition of mist projection granulating comprises: temperature is 70-100 DEG C.When in this temperature range, there is not crosslinking reaction in the mixture that ball milling can be made to obtain in mist projection granulating process.Wherein, the method for mist projection granulating can be the method for the mist projection granulating of this area routine.
According to method of the present invention, wherein, in step (4), dry-pressing formed condition can be the dry-pressing formed condition of this area routine, and such as, dry-pressing formed condition can comprise: pressure is 8-80MPa.Wherein, dry-pressing formed method can be the dry-pressing formed method of this area routine.
According to method of the present invention, wherein, vinyl silicone oil can be the vinyl silicone oil for the preparation of silica gel piece of this area, such as, can be vinyl-terminated silicone fluid.In the present invention, to the viscosity of vinyl silicone oil and contents of ethylene, there is no particular limitation, and such as its viscosity can be 100-50000cp, and with the mole number of vinyl silicone oil for benchmark, the content of described vinyl silicone oil medium vinyl is 0.2-2mol%.According to method of the present invention, wherein, containing hydrogen silicone oil can be the conventional containing hydrogen silicone oil for the preparation of silica gel piece in this area, such as, can be end hydrogen silicone oil.In the present invention, to the content of SiH in containing hydrogen silicone oil, there is no particular limitation, and such as, in containing hydrogen silicone oil, the content of SiH can be 0.05-0.5 % by weight.
According to method of the present invention, wherein, inhibitor can be the inhibitor that the prevention crosslinking reaction of this area routine occurs, and such as it can be selected from least one in 3-methyl isophthalic acid-butine-3-alcohol, 1-ethynylcyclohexanol, methylhydrazine, phenylhydrazine, triphenylphosphine, triphenyl phosphite, sulfoxide type.
According to method of the present invention, wherein, catalyzer can be the catalyzer for catalyzed ethylene base silicone oil and containing hydrogen silicone oil generation crosslinking reaction of this area routine, described catalyzer is preferably the 8th group 4 transition metal and compound thereof or title complex, be more preferably platinum class catalyzer, at least one more preferably in Platinic chloride-Virahol, Platinic chloride-divinyl tetramethyl disiloxane and Platinic chloride-diethyl phthalate.
The third aspect, present invention also offers silica gel piece prepared by aforesaid method.
In silica gel piece of the present invention, the loading level of heat conduction powder is up to 90-97 % by weight, and thermal conductivity can reach more than 6W/mK, and therefore, silica gel piece of the present invention has excellent heat conductivility.
Embodiment
Embodiment 1
The present embodiment is for illustration of silica gel piece of the present invention and preparation method thereof.
(1) by vinyl silicone oil, (viscosity is 100cp, contents of ethylene is 0.2mol%), containing hydrogen silicone oil (content of SiH is 0.05 % by weight), 1-ethynylcyclohexanol, Platinic chloride-divinyl tetramethyl disiloxane mix according to weight ratio 100:7:0.06:0.02, obtains organosilicon crosslinked system;
(2) aluminum oxide (particle diameter is 4.5 μm), organosilicon crosslinked system and normal hexane are carried out ball milling 3h according to weight ratio 100:3:200;
(3) mixture obtained by ball milling carries out mist projection granulating at 80 DEG C, obtained powder;
(4) by powder at pressure be 8MPa condition under carry out dry-pressing formed, obtain the sheet material that thickness is 2mm;
(5) by the dry-pressing formed sheet material obtained crosslinking reaction 15min at 180 DEG C, obtained silica gel piece A1.
Embodiment 2
The present embodiment is for illustration of silica gel piece of the present invention and preparation method thereof.
(1) by vinyl silicone oil, (viscosity is 20000cp, contents of ethylene is 2mol%), containing hydrogen silicone oil (content of SiH is 0.5 % by weight), triphenylphosphine, Platinic chloride-Virahol mix according to weight ratio 100:11:0.06:0.02, obtains organosilicon crosslinked system;
(2) zinc oxide (particle diameter is 4.5 μm), organosilicon crosslinked system and normal hexane are carried out ball milling 2h according to weight ratio 100:3.5:400;
(3) mixture obtained by ball milling carries out mist projection granulating at 85 DEG C, obtained powder;
(4) by powder at pressure be 40MPa condition under carry out dry-pressing formed, obtain the sheet material that thickness is 2mm;
(5) by the dry-pressing formed sheet material obtained crosslinking reaction 60min at 150 DEG C, obtained silica gel piece A2, the loading level of zinc oxide in obtained silica gel piece, according to residual component Mass Calculation after spraying, the results are shown in Table 1.
Embodiment 3
The present embodiment is for illustration of silica gel piece of the present invention and preparation method thereof.
(1) by vinyl silicone oil, (viscosity is 50000cp, contents of ethylene is 1.5mol%), containing hydrogen silicone oil (content of SiH is 0.25 % by weight), phenylhydrazine, Platinic chloride-diethyl phthalate mix according to weight ratio 100:15:0.02:0.1, obtains organosilicon crosslinked system;
(2) aluminum oxide and zinc oxide mix (weight ratio of aluminum oxide and zinc oxide is 3:1, and particle diameter is 0.5 μm), organosilicon crosslinked system and normal hexane are carried out ball milling 4h according to weight ratio 100:5:500;
(3) mixture obtained by ball milling carries out mist projection granulating at 100 DEG C, obtained powder;
(4) by powder at pressure be 50MPa condition under carry out dry-pressing formed, obtain the sheet material that thickness is 2mm;
(5) by the dry-pressing formed sheet material obtained crosslinking reaction 30min at 130 DEG C, obtained silica gel piece A3.
Embodiment 4
The present embodiment is for illustration of silica gel piece of the present invention and preparation method thereof.
Silica gel piece is prepared according to the method for embodiment 1, unlike, replace the aluminum oxide of same particle size by the boron nitride of same particle size, obtained silica gel piece A4.
Embodiment 5
The present embodiment is for illustration of silica gel piece of the present invention and preparation method thereof.
Silica gel piece is prepared according to the method for embodiment 1, unlike, be that the aluminum oxide of 4.5 μm replaces with the aluminum oxide that particle diameter is 10 μm by particle diameter, obtained silica gel piece A5.
Comparative example 1
First prepare A glue and B glue, wherein, the component concentration of A glue is: 50 parts of vinyl silicone oils, and 7 parts hydrogeneous, 0.06 part of hexalin: 210.5 parts of aluminum oxide powders; The component concentration of B glue is: 50 parts of vinyl silicone oils, 0.02 part of Platinic chloride-divinyl tetramethyl disiloxane, 217.5 parts of aluminum oxide powders, can obtain as long as its component is carried out mixing by the preparation of A glue and B glue, be then that 1:1 mixes by A glue and B glue according to weight ratio, and stir 0.5h, obtained slurry, again by this slurry calendering formation, then crosslinked 0.5h at 120 DEG C, obtains the silica gel piece D1 with embodiment 1 same thickness.
Test case
The loading level of the heat conduction powder of the silica gel piece D1 that the silica gel piece A1-A5 adopting thermogravimetry mensuration embodiment 1-5 to obtain and comparative example 1 obtain.Concrete grammar is: weighed by silica gel piece, then under air atmosphere, 800 DEG C are warming up to from 25 DEG C with the speed of 5 DEG C/min, the remaining solid obtained when being warming up to 800 DEG C is the heat conduction powder of filling in this silica gel piece, is then weighed by remaining solid, calculates the loading level of heat conduction powder.
The silica gel piece A1-A5 obtained by embodiment 1-5 and the obtained silica gel piece D1 of comparative example 1 carries out heat conductivility test, and the method for heat conductivility test is that laser shines method, and equipment is laser heat conducting instrument, and model is NETZSCHLFA447, and test result is in table 1.
Table 1
| Sample number into spectrum | Loading level (% by weight) | Thermal conductivity (W/mK) |
| A1 | 97.1 | 6.8 |
| A2 | 96.6 | 6.8 |
| A3 | 95.2 | 6.7 |
| A4 | 90.9 | 6.1 |
| A5 | 90.1 | 6 |
| D1 | 80 | 1.5 |
Embodiment 1-5 is compared can be found out with comparative example 1, and in silica gel piece of the present invention, the loading level of heat conduction powder is up to 90-97 % by weight, and thermal conductivity can reach more than 6W/mK, and therefore, silica gel piece of the present invention has excellent heat conductivility.
Embodiment 1 is compared can find out with embodiment 4, when heat conduction powder be aluminum oxide and/or zinc oxide time, the heat conductivility of obtained silica gel piece can be improved further.
Embodiment 1 is compared can find out with embodiment 5, when the particle diameter of heat conduction powder is 0.5-4.5 μm, the heat conductivility of obtained silica gel piece can be improved further, namely adopt comparatively small particle size conductive powder, the heat conductivility of obtained silica gel piece can be improved further.
Silica gel piece of the present invention has the advantages such as preparation technology is simple, excellent thermal conductivity, production cost are lower, can meet the cooling requirements of electronic product module.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (17)
1. a silica gel piece, is characterized in that, the thermal conductivity of this silica gel piece is more than 6W/mK.
2. silica gel piece according to claim 1, wherein, containing heat conduction powder in this silica gel piece, with the gross weight of described silica gel piece for benchmark, the content of described heat conduction powder is 90-97 % by weight.
3. silica gel piece according to claim 2, wherein, described heat conduction powder is selected from least one in aluminum oxide, zinc oxide, silicon-dioxide, aluminium nitride, boron nitride and silicon carbide, is preferably aluminum oxide and/or zinc oxide.
4. the silica gel piece according to Claims 2 or 3, wherein, the particle diameter of described heat conduction powder is 0.5-4.5 μm.
5. a preparation method for silica gel piece, is characterized in that, the method comprises:
(1) vinyl silicone oil, containing hydrogen silicone oil, inhibitor, catalyzer are mixed, obtain organosilicon crosslinked system;
(2) heat conduction powder, organosilicon crosslinked system and organic solvent are carried out ball milling;
(3) mixture mist projection granulating ball milling obtained, obtained powder;
(4) powder is carried out dry-pressing formed;
(5) the dry-pressing formed sheet material obtained is carried out crosslinking reaction.
6. method according to claim 5, wherein, in step (5), the condition of crosslinking reaction comprises: temperature is 130-180 DEG C, and the time is 15-60min.
7. method according to claim 5, wherein, described heat conduction powder is selected from least one in aluminum oxide, zinc oxide, silicon-dioxide, aluminium nitride, boron nitride and silicon carbide, is preferably aluminum oxide and/or zinc oxide.
8. the method according to claim 5 or 7, wherein, the particle diameter of described heat conduction powder is 0.5-4.5 μm.
9. method according to claim 5, wherein, in step (1), the weight ratio of vinyl silicone oil, containing hydrogen silicone oil, inhibitor, catalyzer is 100:7-15:0.02-0.1:0.02-0.1.
10. method according to claim 5, wherein, in step (2), the weight ratio of heat conduction powder, organosilicon crosslinked system and organic solvent is 100:3-6:200-500.
11. methods according to claim 5, wherein, in step (3), the condition of mist projection granulating comprises: temperature is 70-100 DEG C.
12. methods according to claim 5, wherein, in step (4), dry-pressing formed condition comprises: pressure is 8-80MPa.
13. methods according to claim 5 or 9, wherein, the viscosity of described vinyl silicone oil is 100-50000cp, and with the mole number of vinyl silicone oil for benchmark, the content of described vinyl silicone oil medium vinyl is 0.2-2mol%.
14. methods according to claim 5 or 9, wherein, with the gross weight of containing hydrogen silicone oil for benchmark, in described containing hydrogen silicone oil, the content of SiH is 0.05-0.5 % by weight.
15. methods according to claim 5 or 9, wherein, described inhibitor is selected from least one in 3-methyl isophthalic acid-butine-3-alcohol, 1-ethynylcyclohexanol, methylhydrazine, phenylhydrazine, triphenylphosphine, triphenyl phosphite, sulfoxide type.
16. methods according to claim 5 or 9, wherein, described catalyzer is the 8th group 4 transition metal and compound thereof or title complex, be preferably platinum class catalyzer, be more preferably at least one in Platinic chloride-Virahol, Platinic chloride-divinyl tetramethyl disiloxane and Platinic chloride-diethyl phthalate.
17. silica gel pieces prepared according to method described in any one in claim 5-16.
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Application publication date: 20160511 |