CN114907698B - Modified graphene oxide heat-conducting silicone grease and preparation method thereof - Google Patents
Modified graphene oxide heat-conducting silicone grease and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of heat conduction materials, and provides modified graphene oxide heat conduction silicone grease and a preparation method thereof. The preparation method comprises the following steps: s1, preparing flake graphite, sodium nitrate, KMnO 4 Mixing with concentrated sulfuric acid, and reacting to obtain a reaction product; adding the reaction product into water for dilution, and then dropwise adding hydrogen peroxide until the brown yellow color appears, so as to obtain graphene oxide; s2, mixing graphene oxide, heat conducting powder and ethanol, performing ultrasonic dispersion to obtain a mixed solution, and mixing the mixed solution with an aqueous solution of a coupling agent to react to obtain modified graphene oxide; and S3, mixing the modified graphene oxide with silicone oil, and reacting to obtain the modified graphene oxide heat-conducting silicone grease. The modified graphene oxide heat-conducting silicone grease prepared by the method disclosed by the invention is high in heat conductivity and long in service life.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to modified graphene oxide heat conduction silicone grease and a preparation method thereof.
Background
With the development of technology, the performance of electronic devices is continuously improved, and internal parts with high frequency and high power consumption are developed towards the directions of small size and high integration level. Under the background of smaller and smaller equipment volume, heat dissipation problems are necessarily faced to exert more performances, and heat-conducting silicone grease is developed for the heat dissipation problems. However, the thermal conductivity of the conventional heat-conducting silicone grease is only 6.44W/(m.k), the thermal conductivity is too low, and as the silicone oil is solidified and free silicon hydroxyl remains, the silicone oil is degraded after being heated, the thermal conductivity of the heat-conducting silicone grease is reduced, and the service life of the heat-conducting silicone grease is shortened.
Therefore, how to increase the thermal conductivity of the thermally conductive silicone grease and extend the service life thereof is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a modified graphene oxide heat-conducting silicone grease and a preparation method thereof. The invention aims to solve the technical problems of low heat conductivity, short service life and the like of the traditional heat conduction silicone grease.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of modified graphene oxide heat-conducting silicone grease, which comprises the following steps:
s1, preparing flake graphite, sodium nitrate, KMnO 4 Mixing with concentrated sulfuric acid, and reacting to obtain a reaction product; adding the reaction product into water for dilution, and then dropwise adding hydrogen peroxide until the brown yellow color appears, so as to obtain graphene oxide;
s2, mixing graphene oxide, heat conducting powder and ethanol, performing ultrasonic dispersion to obtain a mixed solution, and mixing the mixed solution with an aqueous solution of a coupling agent to react to obtain modified graphene oxide;
and S3, mixing the modified graphene oxide with silicone oil, and reacting to obtain the modified graphene oxide heat-conducting silicone grease.
Further, in the step S1, the crystalline flake graphite, sodium nitrate and KMnO 4 And concentrated sulfuric acid in the mass-volume ratio of 1.5-2.0 g: 0.75-1.0 g:9.0 to 10.0g: 180.0-200.0 mL;
the mass fraction of the concentrated sulfuric acid is more than or equal to 90%; the grain diameter of the crystalline flake graphite is 100-120 mu m.
Further, the temperature of the mixing in the step S1 is less than or equal to 0 ℃; the reaction temperature is 30-50 ℃ and the reaction time is 18-24 h.
Further, in the step S1, the volume ratio of water to concentrated sulfuric acid is 600-700: 180-200; the mass fraction of the hydrogen peroxide is 20-40%.
Further, in the step S2, the mass-volume ratio of graphene oxide, heat conducting powder and ethanol is 1.0-1.5 g:55.0 to 60.0g: 150.0-200.0 mL;
the volume ratio of the aqueous solution of the coupling agent to the ethanol is 50-60: 150-200; the mass fraction of the aqueous solution of the coupling agent is 3-7%.
Further, the reaction temperature in the step S2 is 50-70 ℃ and the reaction time is 3-4 h; the power of ultrasonic dispersion is 200-300W, and the time is 20-40 min.
Further, in the step S2, the heat conducting powder is one or more of boron nitride, silicon carbide, aluminum powder and aluminum oxide, and the particle size of the heat conducting powder is 50-100 nm;
the coupling agent is one or more of KH550, KH560, KH570 and Z6040.
Further, in the step S3, the mass ratio of the modified graphene oxide to the silicone oil is 55 to 60: 100-120;
the silicone oil is one or more of dimethyl silicone oil, benzyl silicone oil, vinyl silicone oil, hydroxyl silicone oil, carboxyl silicone oil, amino silicone oil and long-chain alkyl silicone oil.
Further, the reaction temperature in the step S3 is 50-70 ℃ and the reaction time is 20-40 min.
The invention provides the modified graphene oxide heat-conducting silicone grease prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the coupling agent can enable graphene oxide and heat conducting powder to be more easily dispersed in the silicone oil, so that a heat conducting channel of the graphene oxide and the heat conducting powder in the silicone oil is established, and the heat resistance among the silicone oil, the graphene oxide and the heat conducting powder is reduced. The graphene oxide and the heat conducting powder conduct heat cooperatively, so that the heat conducting effect of 1+1>2 is achieved, free silicon hydroxyl is remained after the graphene oxide and the silicone oil are solidified to generate connection, the pyrolysis temperature of the silicone oil is increased, the heat conductivity of the heat conducting silicone grease is improved, and the service life of the heat conducting silicone grease is prolonged.
Detailed Description
The invention provides a preparation method of modified graphene oxide heat-conducting silicone grease, which comprises the following steps:
s1, preparing flake graphite, sodium nitrate, KMnO 4 Mixing with concentrated sulfuric acid, and reacting to obtain a reaction product; adding the reaction product into water for dilution, and then dropwise adding hydrogen peroxide until the brown yellow color appears, so as to obtain graphene oxide;
s2, mixing graphene oxide, heat conducting powder and ethanol, performing ultrasonic dispersion to obtain a mixed solution, and mixing the mixed solution with an aqueous solution of a coupling agent to react to obtain modified graphene oxide;
and S3, mixing the modified graphene oxide with silicone oil, and reacting to obtain the modified graphene oxide heat-conducting silicone grease.
In the invention, the step S1 comprises flake graphite, sodium nitrate and KMnO 4 And concentrated sulfuric acid in the mass-volume ratio of 1.5-2.0 g: 0.75-1.0 g:9.0 to 10.0g:180.0 to 200.0mL, preferably 1.6 to 1.9g: 0.78-0.9 g:9.2 to 9.8g:185.0 to 195.0mL, more preferably 1.7 to 1.8g:0.8 to 0.85g:9.4 to 9.6g: 188.0-192.0 mL;
the mass fraction of the concentrated sulfuric acid is more than or equal to 90%, preferably more than or equal to 92%, and more preferably more than or equal to 95%; the particle size of the flake graphite is 100 to 120. Mu.m, preferably 105 to 115. Mu.m, and more preferably 110. Mu.m.
In the present invention, the temperature of the mixing in the step S1 is not more than 0 ℃, preferably not more than-1 ℃, and more preferably not more than-3 ℃; the reaction temperature is 30-50 ℃, preferably 35-45 ℃, and more preferably 38-42 ℃; the time is 18 to 24 hours, preferably 20 to 23 hours, and more preferably 22 hours.
In the invention, the volume ratio of water to concentrated sulfuric acid in the step S1 is 600-700: 180 to 200, preferably 620 to 680:185 to 195, more preferably 640 to 660:187 to 190; the mass fraction of the hydrogen peroxide is 20-40%, preferably 25-35%, and more preferably 30%.
In the invention, the mass-volume ratio of graphene oxide, heat conducting powder and ethanol in the step S2 is 1.0-1.5 g:55.0 to 60.0g:150.0 to 200.0mL, preferably 1.1 to 1.4g: 56.0-59.0 g:160.0 to 190.0mL, more preferably 1.2 to 1.3g:57.0 to 58.0g: 170.0-180.0 mL;
the volume ratio of the aqueous solution of the coupling agent to the ethanol is 50-60: 150 to 200, preferably 52 to 58:160 to 190, more preferably 54 to 56: 170-180 parts; the mass fraction of the aqueous solution of the coupling agent is 3 to 7%, preferably 4 to 6%, and more preferably 5%.
In the present invention, the temperature of the reaction in the step S2 is 50 to 70 ℃, preferably 55 to 65 ℃, and more preferably 58 to 62 ℃; the time is 3 to 4 hours, preferably 3.2 to 3.8 hours, and more preferably 3.4 to 3.6 hours; the power of ultrasonic dispersion is 200 to 300W, preferably 220 to 280W, and more preferably 240 to 260W; the time is 20 to 40 minutes, preferably 24 to 36 minutes, and more preferably 28 to 35 minutes.
In the present invention, the heat conductive powder in the step S2 is one or more of boron nitride, silicon carbide, aluminum powder and aluminum oxide, preferably one or more of boron nitride, silicon carbide and aluminum powder, and more preferably boron nitride and/or silicon carbide; the particle size of the heat conducting powder is 50-100 nm, preferably 60-90 nm, and more preferably 70-80 nm;
the coupling agent is one or more of KH550, KH560, KH570 and Z6040, preferably one or more of KH550, KH560 and KH570, and more preferably KH550 and/or KH560.
In the invention, the mass ratio of the modified graphene oxide to the silicone oil in the step S3 is 55-60: 100 to 120, preferably 56 to 59:104 to 116, more preferably 57 to 58:108 to 114;
the silicone oil is one or more of dimethyl silicone oil, benzyl silicone oil, vinyl silicone oil, hydroxyl silicone oil, carboxyl silicone oil, amino silicone oil and long-chain alkyl silicone oil, preferably one or more of dimethyl silicone oil, benzyl silicone oil, vinyl silicone oil and hydroxyl silicone oil, and further preferably dimethyl silicone oil and/or benzyl silicone oil.
In the present invention, the temperature of the reaction in the step S3 is 50 to 70 ℃, preferably 55 to 65 ℃, and more preferably 58 to 62 ℃; the time is 20 to 40 minutes, preferably 22 to 35 minutes, and more preferably 25 to 30 minutes.
The invention also provides the modified graphene oxide heat-conducting silicone grease prepared by the preparation method.
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Mixing 2g of flake graphite with 180.00ml of 98% concentrated sulfuric acid and 1g of sodium nitrate at 0 ℃, and slowly adding 9.00g of KMnO 4 Reacting for 20 hours at 40 ℃, slowly adding the mixture into 600.00mL of water to dilute the mixture after the reaction is finished, then dropwise adding 30% hydrogen peroxide until the mixture turns brown, and obtaining graphene oxide after filtering, washing and drying;
1.2g of graphene oxide and 55.0g of alumina are placed into 150.00mL of ethanol to be dispersed for 30min by ultrasonic (240W), then 55mL of KH570 water solution with mass fraction of 5% is added, and the mixture is stirred for 30min and reacts for 3h at 60 ℃, and the modified graphene oxide is obtained through centrifugation, washing, drying and grinding.
55.00g of modified graphene oxide and 100g of dimethyl silicone oil are mixed and reacted at 60 ℃ for 30min to obtain the modified graphene oxide heat-conducting silicone grease.
Through detection, the thermal conductivity of the modified graphene oxide thermal conduction silicone grease prepared in the embodiment is 8.44W/m.K.
Example 2
Mixing 1.8g of flake graphite, 190.00ml of 98% concentrated sulfuric acid and 1g of sodium nitrate at 0 ℃, and slowly adding 10.00g of KMnO 4 Reacting for 20 hours at 40 ℃, slowly adding 650.00mL of water after the reaction is finished for dilution, then dropwise adding 30% hydrogen peroxide until brown yellow appears, and obtaining graphene oxide after filtering, washing and drying;
1.2g of graphene oxide and 60.0g of boron nitride are placed into 180.00mL of ethanol to be dispersed for 30min by ultrasonic (260W), then 55mL of KH550 aqueous solution with mass fraction of 5% is added, and the mixture is stirred for 30min and reacts for 3.5h at 60 ℃, and the modified graphene oxide is obtained after centrifugation, washing, drying and grinding.
60.00g of modified graphene oxide and 100g of benzyl silicone oil are mixed and reacted at 60 ℃ for 30min to obtain the modified graphene oxide heat-conducting silicone grease.
Through detection, the thermal conductivity of the modified graphene oxide thermal conduction silicone grease prepared in the embodiment is 8.5W/m.K.
Example 3
Mixing 2g of flake graphite with 180.00ml of 98% concentrated sulfuric acid and 1g of sodium nitrate at 0 ℃, and slowly adding 9.00g of KMnO 4 Reacting for 18 hours at 50 ℃, slowly adding the mixture into 700.00mL of water to dilute the mixture after the reaction is finished, then dropwise adding 30% hydrogen peroxide until the mixture turns brown yellow, and obtaining graphene oxide after filtering, washing and drying;
1.4g of graphene oxide and 55.0g of silicon carbide are placed into 180.00mL of ethanol to be dispersed for 30min by ultrasonic (220W), then 55mL of KH560 aqueous solution with mass fraction of 5% is added, and the mixture is stirred for 30min and reacts for 3h at 60 ℃, and the modified graphene oxide is obtained through centrifugation, washing, drying and grinding.
55.00g of modified graphene oxide and 100g of vinyl silicone oil are mixed and reacted at 60 ℃ for 30min to obtain the modified graphene oxide heat-conducting silicone grease.
Through detection, the thermal conductivity of the modified graphene oxide thermal conduction silicone grease prepared in the embodiment is 8.47W/m.K.
Comparative example 1
60.00g of boron nitride and 100g of benzyl silicone oil are mixed and reacted for 30min at 60 ℃ to obtain the common heat-conducting silicone grease.
The thermal conductivity of the common heat-conducting silicone grease prepared in the comparative example is 5.2W/m.K.
Comparative example 2
Mixing 60.00g of boron nitride, 1.2g of graphene oxide and 100g of benzyl silicone oil, and reacting at 60 ℃ for 30min to obtain the graphene oxide heat-conducting silicone grease.
Through detection, the thermal conductivity of the graphene oxide thermal conduction silicone grease prepared in the comparative example is 5.4W/m.K.
Performance testing
To test the service life of the modified graphene oxide thermally conductive silicone grease, the modified oxygen in example 2 was usedAnd (3) carrying out high-temperature baking at 150 ℃ for 1000 hours on the graphene-converted heat-conducting silicone grease, observing the form of a sample, and testing the change rate of the thermal resistance of the sample. The results show that: the modified graphene oxide heat-conducting silicone grease in example 2 has no cracking and pulverization phenomena, and has a thermal resistance value of only 0.026 ℃ in 2 The temperature of the mixture/W is raised to 0.029℃ in 2 and/W, the thermal resistance change is not large, which indicates that the modified graphene oxide heat conduction silicone grease in the embodiment 2 has high thermal stability and long service life.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The preparation method of the modified graphene oxide heat-conducting silicone grease is characterized by comprising the following steps of:
s1, preparing flake graphite, sodium nitrate, KMnO 4 Mixing with concentrated sulfuric acid, and reacting to obtain a reaction product; adding the reaction product into water for dilution, and then dropwise adding hydrogen peroxide until the brown yellow color appears, so as to obtain graphene oxide;
s2, mixing graphene oxide, heat conducting powder and ethanol, performing ultrasonic dispersion to obtain a mixed solution, and mixing the mixed solution with an aqueous solution of a coupling agent to react to obtain modified graphene oxide;
s3, mixing the modified graphene oxide with silicone oil and then reacting to obtain the modified graphene oxide heat-conducting silicone grease;
in the step S1, the crystalline flake graphite, sodium nitrate and KMnO 4 And concentrated sulfuric acid massThe product ratio is 1.5-2.0 g: 0.75-1.0 g:9.0 to 10.0g: 180.0-200.0 mL; the mass fraction of the concentrated sulfuric acid is more than or equal to 90%; the grain diameter of the flake graphite is 100-120 mu m;
in the step S2, the mass volume ratio of graphene oxide, heat conducting powder and ethanol is 1.0-1.5 g:55.0 to 60.0g: 150.0-200.0 mL; the volume ratio of the aqueous solution of the coupling agent to the ethanol is 50-60: 150-200; the mass fraction of the aqueous solution of the coupling agent is 3-7%.
2. The method according to claim 1, wherein the temperature of mixing in step S1 is 0 ℃ or less; the reaction temperature is 30-50 ℃ and the reaction time is 18-24 h.
3. The preparation method according to claim 1 or 2, wherein the volume ratio of water to concentrated sulfuric acid in the step S1 is 600-700: 180-200; the mass fraction of the hydrogen peroxide is 20-40%.
4. The preparation method according to claim 3, wherein the reaction temperature in the step S2 is 50-70 ℃ for 3-4 hours; the power of ultrasonic dispersion is 200-300W, and the time is 20-40 min.
5. The preparation method of claim 1, 2 or 4, wherein the heat conducting powder in the step S2 is one or more of boron nitride, silicon carbide, aluminum powder and aluminum oxide, and the particle size of the heat conducting powder is 50-100 nm;
the coupling agent is one or more of KH550, KH560, KH570 and Z6040.
6. The preparation method according to claim 5, wherein the mass ratio of the modified graphene oxide to the silicone oil in the step S3 is 55-60: 100-120;
the silicone oil is one or more of dimethyl silicone oil, benzyl silicone oil, vinyl silicone oil, hydroxyl silicone oil, carboxyl silicone oil, amino silicone oil and long-chain alkyl silicone oil.
7. The method according to claim 1, 4 or 6, wherein the reaction in the step S3 is carried out at a temperature of 50 to 70℃for 20 to 40 minutes.
8. The modified graphene oxide heat-conducting silicone grease prepared by the preparation method of any one of claims 1 to 7.
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