CN109233282B - Carbon nanotube doped heat-conducting silicone grease for computer heat dissipation and preparation method thereof - Google Patents
Carbon nanotube doped 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 carbon nanotube-doped heat-conducting silicone grease for computer heat dissipation and a preparation method thereof. The single-walled carbon nanotube is sequentially acidified to form carboxyl, thionyl chloride is subjected to acyl chlorination, and forms amide with mercaptoaniline, and finally the mercapto group is blocked by isophorone diisocyanate to prepare the organic modified carbon nanotube; the organic modified carbon nanotube prepared by the invention is used as the filler of the heat-conducting silicone grease, so that the heat dissipation performance of the heat-conducting silicone grease is greatly improved, and the heat conductivity can reach 6.98W/(m.K).
Description
Technical Field
The invention belongs to the technical field of heat-conducting silicone grease, and particularly relates to carbon nanotube-doped heat-conducting silicone grease for computer heat dissipation and a preparation method thereof.
Background
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, and the heat generation amount thereof is increased. If the CPU does not dissipate heat well and the temperature is too high, the problems of hot start, crash and the like of the computer in the running process are easily caused. Therefore, providing a good heat dissipation system for the CPU is one of the important conditions for ensuring the normal operation of the computer.
The heat-conducting silicone grease is a paste containing silicone oil, and different heat-conducting silicone greases have different heat-conducting properties. Due to the limitations of the manufacturing process, some clearance is inevitable even with very smooth surface-to-surface contact between the CPU and the heat sink, and the existence of the clearance will seriously affect the heat dissipation effect of the CPU. People usually fill the gaps with heat-conducting silicone grease to ensure good contact between the CPU and the heat sink, increase the contact area, and finally achieve the purpose of improving the heat transfer efficiency. Therefore, the heat dissipation performance of the heat-conducting silicone grease has a critical influence on the heat dissipation of the CPU.
The carbon nano-tube has high thermal conductivity, the room temperature thermal conductivity of single-walled carbon tubes (SWNTs) calculated by molecular dynamics simulation is up to 6600W/(m.K), and the room temperature thermal conductivity of multi-walled carbon nano-tubes (MWNTs) is up to 3000W/(m.K) through experimental tests, so the carbon nano-tube is usually used as an additive of the heat-conducting silicone grease to improve the thermal conductivity of the heat-conducting silicone grease; in the Sichuan of Nanchang university, Liujunfeng et al (report of materials science and engineering, 2009, 27(2):271-273, heat-conducting property of carbon nanotube/heat-conducting silicone grease composite material), carbon nanotubes are sequentially acidified and esterified and then added into AS-610B heat-conducting silicone grease AS an additive, and the heat-conducting coefficient is improved to 0.725W/(m.K) from 0.385W/(m.K) before modification; china adhesive, 2017, 26(8):42-47, preparation of carbon nano tube/boron nitride heat-conducting silicone grease and research on heat-conducting property thereof) at the university of North China electric power, takes methyl silicone oil as base oil, absolute ethyl alcohol as a dispersing agent, and CNTs (multi-walled carbon nano tube)/BN (boron nitride) mixed material as a heat-conducting filler to prepare the CNTs/BN composite heat-conducting silicone grease; after the CNTs (multi-walled carbon nanotubes) are added, the thermal conductivity of the composite heat-conducting silicone grease is improved from 0.6117W/(m.K) to 0.6994W/(m.K), and is improved by 14.3%.
At present, although the thermal conductivity of the thermal conductive silicone grease prepared by a plurality of carbon nanotubes is also improved compared with that of the thermal conductive silicone grease prepared by doping and modifying the carbon nanotubes, the thermal conductivity of the finally prepared thermal conductive silicone grease is still lower, so that how to modify and modify the carbon nanotubes to prepare the thermal conductive silicone grease with high thermal conductivity is an important direction for the research and development of the prior art.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity carbon nanotube doped heat-conducting silicone grease for computer heat dissipation, which is characterized in that a single-walled carbon nanotube is sequentially acidified to form carboxyl, chlorinated sulfoxide acyl chloride and mercaptoaniline to form amide, and finally, an organic modified carbon nanotube is prepared by end-capping of mercapto by isophorone diisocyanate; the organic modified carbon nanotube prepared by the invention is used as the filler of the heat-conducting silicone grease, so that the heat dissipation performance of the heat-conducting silicone grease is greatly improved, and the heat conductivity can reach 6.98W/(m.K).
According to the first aspect of the invention, the invention provides a preparation method of an organic modified carbon nanotube, wherein the organic modified carbon nanotube is prepared by introducing carboxyl on a single-walled carbon nanotube through acidification of concentrated sulfuric acid and concentrated nitric acid, reacting thionyl chloride with the carboxyl to form acyl chloride, forming amide by p-mercaptoaniline and the acyl chloride, and finally blocking the amide by isophorone diisocyanate;
preferably, the preparation method of the organic modified carbon nanotube specifically comprises the following steps:
1) 20mg of single-walled carbon nanotubes were placed in 25ml of a mixed solution of concentrated sulfuric acid and concentrated nitric acid (concentrated sulfuric acid/concentrated nitric acid ═ 3:1) performing medium-ultrasonic reflux reaction for 6-8h, and cooling to roomCentrifuging at 3000rpm after warming, washing with water until the filtrate becomes neutral, and vacuum drying at 90 deg.C to constant weight to obtain carboxyl carbon nanotube; FT-IR (KBr) 1730cm-1Characteristic peak of carbonyl group of (a); introducing carboxyl on the surface of the single-walled carbon nanotube under an acidic condition;
2) 15mg of carboxyl carbon nano-tube is put in 10ml of SOCl2Then 0.2g of nitrogen-nitrogen dimethylformamide is dripped for reflux reaction for 16-24h, then the temperature is reduced to room temperature, centrifugation is carried out at 3000rpm, and drying is carried out at 60 ℃ until the weight is constant, thus obtaining the acyl chloride-based carbon nano tube; the carboxyl in the carboxyl carbon nano tube is converted into acyl chloride so as to improve the activity and introduce p-mercaptoaniline;
3) placing 15mg and 3mg of acyl chloride carbon nano tube and p-mercaptoaniline in 5ml of toluene, carrying out reflux reaction for 6-8h, then cooling to room temperature, centrifuging at 3000rpm, and carrying out vacuum drying at 70 ℃ to constant weight to obtain an amide carbon nano tube; introducing p-mercaptoaniline onto the single-walled carbon nanotube by forming amide bond, and forming exposed mercapto;
4) dispersing 100mg of amido carbon nano tube in 10ml of nitrogen-nitrogen dimethyl formamide by ultrasonic, then adding 100mg of isophorone diisocyanate and 50mg of triethylamine to react for 12-24h under the nitrogen atmosphere, centrifuging at 3000rpm after the reaction is finished, washing the centrifugate by dichloromethane and nitrogen-nitrogen dimethyl formamide in sequence, and drying in vacuum at 60 ℃ to constant weight to obtain the organic modified carbon nano tube; the step is to use isophorone diisocyanate as a blocking agent to block the exposed sulfydryl on the carbon nano tube to form the final organic modified carbon nano tube;
according to another aspect of the invention, the invention provides the use of the organic modified carbon nano tube, which is mixed with organic silicone oil for preparing heat-conducting silicone grease;
preferably, the weight percentage of the organic modified carbon nano tube in the heat-conducting silicone grease is 50-90 wt%;
preferably, the organic silicone oil is dimethyl silicone oil, epoxy modified silicone oil, vinyl silicone oil, benzyl silicone oil or hydroxyl silicone oil;
preferably, the organic silicone oil is hydroxyl silicone oil, the hydroxyl content of the hydroxyl silicone oil is 7.2 wt%, and the viscosity at 25 ℃ is 19.6mm2/s；
Preferably, the organic silicone oil is hydroxyl silicone oil, and the weight percentage of the organic modified carbon nano tube in the heat-conducting silicone grease is 70-80 wt%;
according to another aspect of the present invention, the present invention provides a method for preparing a heat conductive silicone grease, comprising the steps of: placing the organic modified carbon nano tube in methanol for uniform ultrasonic dispersion, and then adding amphoteric surfactant sodium dodecyl aminopropionate and organic silicone oil for 2-4h of ultrasonic treatment at 30-40 ℃; cooling to 0-5 deg.C, removing solvent methanol under pressure of-0.09 MPa, removing methanol, heating to 90 deg.C, and vacuum drying for 3-5h to obtain the final product. In order to solve the problem that nano particles in the organic modified carbon nano tubes in the heat-conducting silicone grease are easy to accumulate to influence the heat conductivity of the heat-conducting silicone grease, a small amount of amphoteric surfactant sodium dodecyl aminopropionate is added into the system, and the problems of uneven distribution and low heat conductivity of the organic modified carbon nano tubes are solved by adopting solvent ultrasound and low-temperature ultrasound decompression desolventizing in the preparation process, so that the characteristic of high heat conductivity of the carbon nano tubes is utilized to the maximum extent.
Preferably, the addition amount of the sodium dodecyl aminopropionate is 0.2 to 0.8 weight percent of the weight of the organic modified carbon nano tube;
compared with the prior art, the invention has the following advantages:
1) the organic modified carbon nano tube prepared by carrying out organic modification on the carbon nano tube can be used for preparing heat-conducting silicone grease with high heat conductivity;
2) according to the invention, the sodium dodecyl aminopropionate is added in the preparation process of the heat-conducting silicone grease, and the problem of uneven distribution of the organic modified carbon nanotubes is solved by adopting solvent ultrasound and low-temperature ultrasound decompression desolventizing in the preparation process, so that the heat conductivity of the heat-conducting silicone grease is improved.
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.
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.
The single-walled carbon nanotube used in the examples is from Beijing German island gold technology, Inc., model is CNT400, the tube diameter is 1-2nm, the length is 0.5-2 μm; 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 pure chemical organosilicon material company of Shenzhen city, the hydroxyl content is 7.2 percent by weight, and the viscosity at 25 ℃ is 19.6mm2(s) a ring content of 15.8% wt; the remaining reagents in the examples are all conventional reagents which are commercially available.
Example 1
The organic modified carbon nano tube is prepared according to the following process: 1. acidifying the single-walled carbon nanotube by adopting concentrated sulfuric acid and concentrated nitric acid to introduce carboxyl; 2. reacting the carboxyl formed by acidification with thionyl chloride to form acyl chloride; 3. p-mercaptoaniline and acyl chloride are adopted to form amide; 4. the final organic modified carbon nano tube is formed by blocking sulfydryl in p-mercaptoaniline with isophorone diisocyanate, and the specific preparation method comprises the following steps:
1) placing 20g of single-walled carbon nanotube into 200ml of mixed solution of 98 wt% concentrated sulfuric acid and 68 wt% concentrated nitric acid (volume ratio of concentrated sulfuric acid to concentrated nitric acid is 3:1), performing ultrasonic reflux reaction for 6-8h, cooling to room temperature, centrifuging at 3000rpm, washing with water until filtrate is neutral, and performing vacuum drying at 90 ℃ to constant weight to obtain the carboxyl carbon nanotube; FT-IR (KBr pellet) appearance 1730cm-1The characteristic peak of carbonyl group of (a), confirming that carboxyl group is already present on the carbon nanotube;
2) taking 15g of carboxyl carbon nano-tube and placing in 100ml of SOCl2In (1),then 0.2g of nitrogen-nitrogen dimethylformamide is dripped for reflux reaction for 16-24h, the temperature is reduced to room temperature, centrifugation is carried out at 3000rpm, and drying is carried out at 60 ℃ until the weight is constant, thus obtaining the acyl chloride-based carbon nano tube;
3) placing 15g and 3g of acyl chloride carbon nano tube and p-mercaptoaniline in 500ml of toluene, carrying out reflux reaction for 6-8h, then cooling to room temperature, centrifuging at 3000rpm, and carrying out vacuum drying at 70 ℃ to constant weight to obtain an amide carbon nano tube;
4) and (2) ultrasonically dispersing 100g of amido carbon nano tube in 1L of nitrogen-nitrogen dimethyl formamide, then adding 100g of isophorone diisocyanate and 5g of triethylamine to react for 12-24h under the nitrogen atmosphere, centrifuging at 3000rpm after the reaction is finished, washing the centrifuged substance with 500ml of dichloromethane and 500ml of nitrogen-nitrogen dimethyl formamide in sequence, and drying in vacuum at 60 ℃ to constant weight to obtain the organic modified carbon nano tube.
Example 2
Adding organic modified carbon nanotubes (the filling amount of the organic modified carbon nanotubes 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 an oven at 130 ℃ 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, wherein the heat conductivity is tested to be 3.69W/(m.K).
Example 3
Selection of the type of silicone oil: adding organic modified carbon nanotubes (the filling amount of the organic modified carbon nanotubes is 60 wt%, and the filling amount of the organic silicon oil is 40 wt%) into organic silicon oil, uniformly mixing by using a stainless steel colloid mill, drying in an oven at 130 ℃ for 30min to thicken the mixture, then carrying out ultrasonic treatment at 60-70 ℃ for 1-2 days to obtain the heat-conducting silicone grease, and testing the heat conductivity of the heat-conducting silicone grease prepared by different organic silicon oils, wherein the heat conductivity is shown in table 1:
TABLE 1 thermal conductivity of thermally conductive silicone grease prepared from different silicone oils
The test result shows that the heat conductivity of the heat-conducting silicone grease composed of the hydroxyl silicone oil and the organic modified carbon nano tube is higher than that of other types of silicone oil, probably because oxygen atoms in the hydroxyl silicone oil can better form hydrogen bonds with the organic modified carbon nano tube, the compatibility of the silicone oil and the organic modified carbon nano tube is increased, and thus the heat-conducting path of the heat-conducting silicone grease is improved.
Example 4
When the type of the organic silicon oil is determined to be hydroxyl silicon oil, the invention researches the filling amount of the organic modified carbon nano tube: adding organic modified carbon nanotubes into hydroxyl silicone oil (changing the filling amount of the hydroxyl silicone oil and the organic modified carbon nanotubes), uniformly mixing by using a stainless steel colloid mill, drying in an oven at 130 ℃ for 30min to thicken the mixture, then carrying out ultrasonic treatment at 60-70 ℃ for 1-2 days to obtain the heat-conducting silicone grease, and testing the heat conductivity of the heat-conducting silicone grease prepared according to different filling amount proportions, wherein the heat conductivity is shown in table 2:
TABLE 2 influence of the filling ratio of hydroxy silicone oil to organically modified carbon nanotubes on the thermal conductivity
Example 5
In order to overcome the technical problem that the organic modified carbon nano tube is easy to aggregate when hydroxyl silicone oil and the organic modified carbon nano tube are mixed by a colloid mill, and the heat-conducting silicone grease can be conveniently dispersed on a radiating surface, the invention tries to prepare the heat-conducting silicone grease by a method of ultrasonic mixing in a solvent and then desolventizing, and the method comprises the following steps:
putting 10.0g of organic modified carbon nano tube into 200ml of methanol for uniform ultrasonic dispersion, and then adding 0.05g of amphoteric surfactant sodium dodecyl aminopropionate and 2.5g of hydroxy silicone oil for ultrasonic treatment at 30-40 ℃ for 2-4 h; cooling to 0-5 deg.C, removing solvent methanol under pressure of-0.09 MPa, removing methanol, heating to 90 deg.C, and vacuum drying for 3-5h to obtain the final product.
The heat-conducting silicone grease prepared by the method has no obvious aggregation phenomenon of the organic modified carbon nano tubes in the preparation process, the heat conductivity of the prepared heat-conducting silicone grease is detected to be 6.98W/(m.K), and the method has better mixing effect than that of a colloid mill.
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 (4)
1. The application of the organic modified carbon nanotube is characterized in that: mixing with organic silicone oil to prepare heat-conducting silicone grease; the organic silicone oil is hydroxyl silicone oil; the weight percentage of the organic modified carbon nano tube in the heat-conducting silicone grease is 50-90 wt%;
the organic modified carbon nano tube is prepared by the following method: the organic modified carbon nano tube is prepared by introducing carboxyl on a single-walled carbon nano tube by acidification of concentrated sulfuric acid and concentrated nitric acid, reacting thionyl chloride with the carboxyl to form acyl chloride, forming amide by p-mercaptoaniline and the acyl chloride, and finally sealing by isophorone diisocyanate; the method comprises the following steps:
1) placing the single-walled carbon nanotube into a mixed solution of concentrated sulfuric acid and concentrated nitric acid for ultrasonic reflux reaction, then cooling to room temperature for centrifugation, washing with water until filtrate becomes neutral, and drying to constant weight to obtain the carboxyl carbon nanotube;
2) placing carboxyl carbon nanotube in SOCl2Then, dropwise adding nitrogen-nitrogen dimethyl formamide for reflux reaction, cooling to room temperature after the reaction is finished, centrifuging, and drying to constant weight to obtain the acyl chloride-based carbon nano tube;
3) placing acyl chloride carbon nano-tubes and p-mercaptoaniline in toluene, carrying out reflux reaction, cooling to room temperature after the reaction is finished, centrifuging, and drying to constant weight to obtain amide carbon nano-tubes;
4) and (2) ultrasonically dispersing the amido carbon nano tube in nitrogen-nitrogen dimethyl formamide, then adding isophorone diisocyanate and triethylamine to react in a nitrogen atmosphere, centrifuging after the reaction is finished, washing a centrifugate with dichloromethane and nitrogen-nitrogen dimethyl formamide in sequence, and drying to constant weight to obtain the organic modified carbon nano tube.
2. Use according to claim 1, characterized in that: the weight percentage of the organic modified carbon nano tube in the heat-conducting silicone grease is 70-80 wt%.
3. A method for preparing a heat conductive silicone grease for use according to claim 1, characterized in that: placing the organic modified carbon nano tube in methanol for uniform ultrasonic dispersion, and then adding amphoteric surfactant sodium dodecyl aminopropionate and organic silicone oil for 2-4h of ultrasonic treatment at 30-40 ℃; cooling to 0-5 ℃, removing the solvent methanol under the pressure of P = -0.09MPa by ultrasonic decompression, heating to 90 ℃ after the methanol is removed completely, and drying in vacuum for 3-5h to obtain the heat-conducting silicone grease.
4. The production method according to claim 3, characterized in that: the addition amount of the sodium dodecyl aminopropionate is 0.2 to 0.8 weight percent of the weight of the organic modified carbon nano tube.
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