CN108587576B - Heat-conducting silicone grease for computer heat dissipation and preparation method thereof - Google Patents
Heat-conducting silicone grease for computer heat dissipation and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of heat-conducting silicone grease, and particularly relates to heat-conducting silicone grease for computer heat dissipation and a preparation method thereof; the heat-conducting silicone grease for computer heat dissipation consists of organic silicone oil and a nano aluminum-silicon composite material; the nano aluminum-silicon composite material is prepared by taking aluminum nitrate as an aluminum source and ethyl orthosilicate as a silicon source through a sol-gel method. Compared with single nanometer aluminum oxide, the thermal conductivity of the prepared thermal-conductive silicone grease is obviously improved by adopting the nanometer aluminum-silicon composite material prepared by the invention as the thermal-conductive filler, and can reach 5.8W/(m.K) at most, and the thermal-conductive silicone grease can be used for CPU radiators of large computers.
Description
Technical Field
The invention belongs to the technical field of heat-conducting silicone grease, and particularly relates to heat-conducting silicone grease for computer heat dissipation and a preparation method thereof.
Background
With the increasing functions and performances of microprocessors and the miniaturization and high efficiency of electronic products, the requirements for heat dissipation of electronic components are higher and higher, and the problem of overheating of electronic components caused by poor heat dissipation becomes an important bottleneck limiting the development of electronic technology. Thermally conductive greases are a thermal interface material used in electronic thermal management systems to shorten the heat transfer path and reduce the thermal resistance. The heat-conducting cassia grease has the advantages of no thickening at low temperature, no thinning at high temperature, no volatilization, no solidification, low oil separation and the like. Compared with other thermal interface materials, the heat-conducting resin has the best comprehensive performance, thereby gaining more and more attention, and can be widely applied to electronic components and parts and heat dissipation plates or radiators, such as power amplifiers, transistors, electron tubes, CPUs and other electronic devices.
With the rapid development of computer technology, the operation speed of a Central Processing Unit (CPU) as a core of a computer system is faster and faster, but the heat productivity is also increased, and if the heat dissipation condition is poor, the temperature of the CPU is too high, which easily causes the problems of automatic hot start, crash and the like in the running process of the computer, so that providing a good heat dissipation system for the CPU is an important condition for ensuring the normal work of the computer. Statistically, the computer CPU failures due to overheating account for 55% of the total CPU failures, and the reliability decreases by 50% for every 10% increase in operating temperature. In order to improve the thermal conductivity of the heat-conducting silicone grease composition, the solid content in the heat-conducting silicone grease composition is usually increased, but the solid content of the conventional heat-conducting silicone grease composition reaches 90%, so that the thermal conductivity of the heat-conducting silicone grease composition is improved from the aspect of simply increasing the solid content, and no space is provided for improving the thermal conductivity of the heat-conducting silicone grease composition.
Al2O3In the heat-conducting polymer composite material, such as heat-conducting silicon rubber and heat-conducting silicon grease, the dispersibility is good, the distribution is uniform, and the heat-conducting polymer composite material has the advantages of good dispersibility and uniform distributionThe heat conduction effect is good, so that Al2O3 is used for improving the heat conductivity of the heat conduction butterfat composite material; however, Al2O3The heat conductivity of the heat-conducting silicone grease prepared when the heat-conducting silicone grease is used as a heat-conducting filler is not high; von Brilliant et Al (Chinese adhesive 2016,8:451-2O3The silane coupling agent is adopted for surface treatment, when the filling amount is 88.8 percent, the thermal conductivity is only 1.34W/(m.K), and ZnO and Al are adopted for subsequent treatment2O3Compounding at a specific ratio only improves the thermal conductivity to 3.98W/(m.K), at which time the loading has reached 92%.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides heat-conducting silicone grease for computer heat dissipation. The heat-conducting silicone grease prepared by the invention has high heat conductivity, and can be used for heat dissipation of parts such as a CPU (central processing unit) of a large-scale computer.
The invention realizes the aim through the following technical scheme that the heat-conducting silicone grease for computer heat dissipation consists of organic silicone oil and a nano aluminum-silicon composite material; the nano aluminum-silicon composite material is prepared by taking aluminum nitrate as an aluminum source and ethyl orthosilicate as a silicon source by a sol-gel method;
preferably, the specific preparation method of the nano aluminum-silicon composite material comprises the following steps:
dissolving aluminum nitrate in deionized water, adding ethyl orthosilicate, mixing at 30-50 ℃, and then dropwise adding ammonia water to adjust the pH of the system to 7-8; stirring for 1-4h for aging, cooling to room temperature, filtering, washing, drying at 120 ℃ to constant weight, and roasting at 400 ℃ to 300 ℃ for 4-6h to obtain the nano aluminum-silicon composite material; calculated according to molar ratio, ethyl orthosilicate: 1:5-8 of aluminum nitrate; preferably, the preparation process is carried out with heat preservation and stirring for 2h for aging, and the weight ratio of ethyl orthosilicate: 1:7 of aluminum nitrate;
in the process of preparing the nano aluminum-silicon composite material by the sol-gel method, the tetraethoxysilane is continuously hydrolyzed into SiO2And combining with Al species, aging and calcining to obtain alumina as main material and SiO as doped material2The nano aluminum-silicon composite material contains aluminum oxide and SiO2Forming a structure of mutual inclusion; the structure of the nano aluminum-silicon composite material is adjusted by controlling the proportion of the ethyl orthosilicate and the aluminum nitrate and the aging time of the ethyl orthosilicate and the aluminum nitrate, so that the properties of the nano aluminum-silicon composite material are influenced.
Preferably, the organic silicone oil is dimethyl silicone oil, epoxy modified silicone oil, vinyl silicone oil, benzyl silicone oil or hydroxyl silicone oil, and more preferably epoxy modified silicone oil; when the organic silicone oil is screened, the heat-conducting silicone grease prepared from the epoxy modified silicone oil is surprisingly found to have high heat conductivity, and the heat-conducting path of the heat-conducting silicone grease is improved probably because the compatibility between the epoxy modified silicone oil and the filler can be improved due to the introduction of the epoxy group.
Preferably, the weight of the nano aluminum-silicon composite material is 40-75% of that of the heat-conducting silicone grease, and more preferably 68%;
according to another aspect of the invention, the invention provides a preparation method of heat-conducting silicone grease for computer heat dissipation, which comprises the steps of adding a nano aluminum-silicon composite material into organic silicone oil, uniformly mixing the materials by using a colloid mill, drying the materials in an oven at 150 ℃ for 30min to thicken the materials, and then carrying out ultrasonic treatment at 60-70 ℃ for 1-2 days to obtain the heat-conducting silicone grease containing the nano aluminum-silicon composite material.
The invention adopts a sol-gel method to prepare Al for the first time2O3As a host material, SiO2The nanometer aluminum-silicon composite material which is doped with the material and is included mutually is used as the heat conduction material of the heat conduction silicone grease, compared with the prior art, the invention has the following advantages:
1) the invention prepares the nano aluminum-silicon composite material by the sol-gel method for the first time to replace the traditional Al2O3As a heat-conducting filler, the heat conductivity of the heat-conducting silicone grease is improved;
2) compared with the traditional silane coupling agent surface coating modification, the invention adopts sol-gelPreparation of Al2O3As a host material, SiO2Is a nano aluminum silicon composite material which is doped with materials and is included mutually;
3) the heat-conducting silicone grease prepared by the self-made nano aluminum-silicon composite material and the epoxy modified silicone oil has the heat conductivity as high as 5.8W/(m.K).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention.
The raw material sources are as follows: the dimethyl silicone oil is silicone oil which is obtained from Daokoning and has the trade name of PMX-200 and the trade name of 50 CS; the epoxy modified silicone oil is from Shandong Dayihua chemical Co., Ltd, and is DY-E701 epoxy modified silicone oil, the epoxy value is 0.08mol/100g, and the viscosity is 1100cp (25 ℃); the vinyl silicone oil is from pure chemical organosilicon material company of Shenzhen, the viscosity is 2060mPa.S, and the vinyl content is 1.1 percent wt; the benzyl silicone oil is BSO-30150 benzyl silicone oil from Shenzhen Chunhang chemical organosilicon material company; the hydroxyl silicone oil is from Shenzhen Chunchang chemical organosilicon material company, and the hydroxyl content is 7.2 percent by weight; the remaining reagents in the examples are all conventional reagents which are commercially available.
And (3) testing thermal conductivity: the thermal conductivity of the thermal conductive silicone grease prepared in different embodiments of the invention is tested by a thermal flow method by adopting a thermal conductivity tester with the model number of DRL-III-P, and the test standard is MIL-I-49456A.
And (3) viscosity testing: measured by an NDJ-7 rotational viscometer according to the requirements of GB/T2794-1995 & ltdetermination of adhesive viscosity'; pouring the prepared heat-conducting silicone grease into a rotational viscometer at the temperature of 25 +/-0.1 ℃, continuously rotating for 2min at the rotating speed of 7.5rpm, stabilizing the degree, measuring for three times on average, and taking the average value obtained by the three times;
example 1
Adding a nano aluminum-silicon composite material (the filling amount of the nano aluminum-silicon composite material is 60 wt%, and the filling amount of the dimethyl silicone oil is 40 wt%) into dimethyl silicone oil, uniformly mixing by using a stainless steel colloid mill, drying in a drying oven at 150 ℃ for 30min to thicken the nano aluminum-silicon composite material, and then carrying out ultrasonic treatment at 60-70 ℃ for 1-2 days to obtain the heat-conducting silicone grease containing the nano aluminum-silicon composite material.
Preparing a nano aluminum-silicon composite material: dissolving aluminum nitrate in deionized water, adding 20mmol of tetraethoxysilane, mixing at 30-50 ℃, and then dropwise adding ammonia water to adjust the pH of the system to 7-8; preserving heat, stirring and aging, then cooling to room temperature, filtering, washing, drying at the temperature of 100-.
The invention inspects the influence of ethyl orthosilicate and aluminum nitrate with different molar ratios and nano aluminum-silicon composite materials prepared by different heat preservation stirring aging times on the heat-conducting performance of the heat-conducting silicone grease, and the table 1 shows that:
TABLE 1 thermal conductivity of thermally conductive Silicone greases
Note: the Si/Al molar ratio refers to the molar dosage ratio of the ethyl orthosilicate to the aluminum nitrate in the preparation process of the nano aluminum-silicon composite material.
The above results show that when a small amount of tetraethoxysilane is added (sequence 7, Si/Al is 1:10), the thermal conductivity of the prepared heat-conducting silicone grease is hardly improved, the thermal conductivity of the heat-conducting silicone grease is remarkably improved by continuously increasing the molar amount of tetraethoxysilane, and when Si/Al is 1:7, the thermal conductivity reaches 2.96W/(m · K), but when the molar amount of tetraethoxysilane is continuously increased, the thermal conductivity is rather lowered, and when Si/Al is 1:1, the thermal conductivity is lowered to 0.96, which is rather lower than that when tetraethoxysilane is not added, so that the Si/Al molar ratio is controlled to be tetraethoxysilane: preferably, the ratio of aluminum nitrate to aluminum nitrate is 1: 5-8; when the nano aluminum-silicon composite material is prepared, the aging time also influences the thermal conductivity of the prepared heat-conducting silicone grease, and the aging time is preferably 3 hours.
Example 2
The optimal preparation process of the selected nano aluminum-silicon composite material comprises the following steps: dissolving 140mmol of aluminum nitrate in 500ml of deionized water, then adding 20mmol of ethyl orthosilicate, mixing at 30-50 ℃, and then dropwise adding ammonia water to adjust the pH value of the system to 7-8; preserving heat, stirring and aging for 3h, then cooling to room temperature, filtering, washing, drying at the temperature of 100 ℃ and 120 ℃ to constant weight, and finally heating to the temperature of 300 ℃ and 400 ℃ and roasting for 4-6h to obtain the nano aluminum-silicon composite material.
The invention screens the influence of different organic silicon oils on the heat conductivity of the heat-conducting silicone grease, and the method comprises the following steps:
adding a nano aluminum-silicon composite material (the filling amount of the nano aluminum-silicon composite material is 60 wt%, the filling amount of the dimethyl silicone oil is 40 wt%) into organic silicone oil, uniformly mixing by using a stainless steel colloid mill, drying in a drying oven at 150 ℃ for 30min to thicken the nano aluminum-silicon composite material, and then carrying out ultrasonic treatment at 60-70 ℃ for 1-2 days to obtain the heat-conducting silicone grease containing nano copper particles, wherein the heat conductivity of the heat-conducting silicone grease prepared by different organic silicone oils is shown in table 2:
TABLE 2 influence of the type of silicone oil on the thermal conductivity of thermally conductive greases
Test results show that the heat-conducting silicone grease prepared from different silicone oils has different heat conductivities, wherein the heat-conducting silicone grease prepared from epoxy modified silicone oil has the best heat conductivity effect.
Example 3
When the parameters of the sequence 5 in the table 1 are selected as the optimal preparation process of the nano aluminum-silicon composite material and the epoxy modified silicone oil is selected as the organic silicone oil, the filling amount of the nano aluminum-silicon composite material is researched, and the method comprises the following steps:
adjusting the weight ratio of the epoxy modified silicone oil to the nano aluminum-silicon composite material, adding the nano aluminum-silicon composite material into the epoxy modified silicone oil, uniformly mixing by using a stainless steel colloid mill, drying in a drying oven at 150 ℃ for 30min to thicken the mixture, and then carrying out ultrasonic treatment at 60-70 ℃ for 1-2 days to obtain the heat-conducting silicone grease containing the nano copper particles, wherein the heat conductivity of the heat-conducting silicone grease prepared by different filling amounts of the nano aluminum-silicon composite material is shown in Table 3:
TABLE 3 influence of nano-Al-Si composite material filling amount on thermal conductivity of heat-conducting silicone grease
| Loading/wt% | Thermal conductivity/W/(m.K) | viscosity/mPa.S |
| 40 | 2.79 | 6080 |
| 50 | 3.68 | 13600 |
| 60 | 4.28 | 28120 |
| 70 | 5.69 | 43640 |
| 80 | 5.60 | 62400 |
| 90 | 5.61 | 71600 |
| 63 | 5.72 | 29840 |
| 68 | 5.80 | 33680 |
Note: the filling amount refers to the weight percentage of the nano aluminum-silicon composite material in the heat-conducting silicone grease.
Generally, as the filling amount of the heat conductive filler increases, the thermal conductivity thereof increases, and the filling amount of the heat conductive filler is generally increased as much as possible in order to increase the thermal conductivity of the heat conductive silicone grease; however, the filling amount of the nano aluminum-silicon composite material is slightly reduced after being more than 70 percent by weight, and the viscosity is gradually increased along with the increase of the filling amount of the nano aluminum-silicon composite material, so the viscosity and the thermal conductivity are comprehensively considered, and the filling amount is selected to be 68 percent to be the most excellent.
Although the embodiments of the present invention have been described in detail, it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention.
Claims (3)
1. The utility model provides a heat conduction silicone grease for computer heat dissipation which characterized in that: the heat-conducting silicone grease for computer heat dissipation consists of organic silicone oil and a nano aluminum-silicon composite material; the nano aluminum-silicon composite material is prepared by taking aluminum nitrate as an aluminum source and ethyl orthosilicate as a silicon source by a sol-gel method;
the specific preparation method of the nano aluminum-silicon composite material comprises the following steps: dissolving aluminum nitrate in deionized water, adding ethyl orthosilicate, mixing at 30-50 ℃, and then dropwise adding ammonia water to adjust the pH of the system to 7-8; stirring for 2h for aging, cooling to room temperature, filtering, washing with water, drying at 120 ℃ to constant weight, and calcining at 400 ℃ to 300 ℃ to 6h to obtain the nano aluminum-silicon composite material; calculated according to molar ratio, ethyl orthosilicate: aluminum nitrate =1: 7; the weight of the nano aluminum-silicon composite material is 40-75% of that of the heat-conducting silicone grease;
the organic silicone oil is epoxy modified silicone oil.
2. The heat-conductive silicone grease for dissipating heat from a computer of claim 1, wherein: the weight of the nano aluminum-silicon composite material is 68 percent of that of the heat-conducting silicone grease.
3. The preparation method of the heat-conducting silicone grease for computer heat dissipation of claim 1, characterized by comprising the following steps: adding the nano aluminum-silicon composite material into the organic silicon oil, uniformly mixing by using a colloid mill, drying in an oven at 150 ℃ for 30min to thicken the mixture, and then carrying out ultrasonic treatment at 60-70 ℃ for 1-2 days to obtain the heat-conducting silicone grease containing the nano aluminum-silicon composite material.
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| "氧化铝/碳材料导热硅脂的研究";李婧璇等;《青岛科技大学学报(自然科学版)》;20180228;第39卷(第1期);第54-58页 * |
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