CN114318468A - Graphene surface enhanced heat transfer composite material and preparation method thereof - Google Patents
Graphene surface enhanced heat transfer composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a graphene surface enhanced heat transfer composite material and a preparation method thereof, wherein the preparation method comprises the following steps: uniformly mixing a graphene material with isopropanol to form a negatively charged graphene solution; adding a magnesium salt into the graphene solution to prepare a mixed solution, wherein the weight ratio of the graphene material to the magnesium salt is 1: 5-3: 1; and taking the conductive material as a cathode, and carrying out electrophoretic deposition in the mixed solution to obtain the graphene surface enhanced heat transfer composite material. According to the invention, the graphene material and the conductive material are stably connected together through the magnesium hydroxide and the ester group formed in the electrophoretic deposition process, and the graphene material and the conductive material are used as a surface enhanced heat transfer composite material, so that the phase change heat transfer performance can be improved; the graphene material in the surface enhanced heat transfer composite material obtained by the method is connected to the surface of the conductive material in a vertical orientation mode, and the graphene material connected in the vertical orientation mode can reduce the superheat degree required by phase change heat transfer initial nucleate boiling and obviously improve the phase change heat transfer rate.
Description
Technical Field
The invention relates to the technical field of phase change heat transfer, in particular to a graphene surface enhanced heat transfer composite material and a preparation method thereof.
Background
With the rapid development of the aerospace technology, the new generation of spacecrafts such as satellites are developed in the directions of high resolution, high precision and miniaturization, the effective load of the device is increased due to the high integration of an electronic system, the heat flux density in a limited space is also increased rapidly, the local temperature of the spacecraft is easily overhigh, and the thermal control technology of the spacecraft faces greater challenges. In order to improve the reliability, stability and service life of the spacecraft, the problem of micro thermal control of high heat flux density components and assemblies in a narrow space needs to be solved, so that the maximum temperature of equipment is kept at an acceptable limit condition, and the temperature uniformity of the whole equipment is improved.
Phase change heat transfer refers to a convective heat transfer process in which heat is transferred from a wall surface to a liquid to boil and vaporize the liquid. The phase change heat transfer can obtain a great heat transfer coefficient under a small superheat degree, and the method becomes a research hotspot. The phase change heat transfer performance can be further improved through the graphene coating, and methods for enhancing the phase change heat transfer performance of aluminum metal by graphene in the prior art include a self-assembly method, a spraying method and the like. However, due to strong pi-pi bonds and van der waals force interaction between graphene sheet layers, the graphene sheet layers are easy to form irreversible aggregation or overlapping, and the graphene nano sheets are distributed on the surface of aluminum in a horizontal orientation mode, so that the phase change heat transfer performance is influenced.
Disclosure of Invention
The problem to be solved by the invention is that in the prior art, graphene nanosheets are horizontally oriented and distributed on the surface of aluminum, and irreversible agglomeration or overlapping is easily formed between graphene layers, so that the phase-change heat transfer performance is influenced.
In order to solve at least one aspect of the above problems, the present invention provides a method for preparing a graphene surface enhanced heat transfer composite, comprising the following steps:
step S1, uniformly mixing the graphene material with isopropanol to form a graphene material solution with negative electricity;
step S2, adding a magnesium salt into the graphene material solution to prepare a mixed solution, wherein the weight ratio of the graphene material to the magnesium salt is 1: 5-3: 1;
and step S3, taking the conductive material as a cathode, and performing electrophoretic deposition in the mixed solution to obtain the graphene surface enhanced heat transfer composite material.
Preferably, in the step S1, the graphene material is added into the isopropanol, and ultrasonically dispersed for 1h to form a uniform graphene solution.
Preferably, the graphene material comprises graphene oxide or reduced graphene oxide.
Preferably, the magnesium salt comprises magnesium nitrate, magnesium carbonate or magnesium sulfate.
Preferably, in the step S2, the weight ratio of the graphene material to the magnesium salt is 1: 1.
Preferably, in step S3, a platinum sheet is used as an anode in the electrophoretic deposition process.
Preferably, in step S3, the reaction voltage during the electrophoretic deposition process is 220V, and the reaction time is 2 min.
Preferably, the conductive material includes an aluminum sheet, a copper sheet, a carbon cloth, or a carbon fiber.
According to the preparation method, a graphene material and a magnesium salt are prepared into a mixed solution, as a functional group with negative electricity exists on the surface of the graphene material, and magnesium ions have positive charges, the magnesium ions can be adsorbed on the surface of the graphene material under the attraction effect of the positive charges and the negative charges, when a conductive material is used as a cathode to carry out electrophoretic deposition in the mixed solution, particles mixed into the solution are subjected to redox reaction on an anode and the cathode under the action of an electric field, the magnesium ions adsorbed on the surface of the graphene material react with hydroxyl on the surface of the conductive material to generate magnesium hydroxide, and the graphene material is connected with the conductive material through the bridge action of the magnesium hydroxide; in addition, functional groups such as carboxyl on the surface of the graphene material can react with hydroxyl on the surface of the conductive material to generate ester groups, so that the connection stability of the graphene material and the conductive material can be further improved; the graphene material and the conductive material are stably connected together through the magnesium hydroxide and the ester group formed in the electrophoretic deposition process, and the graphene material is used as a graphene surface enhanced heat transfer composite material, so that the phase change heat transfer performance can be improved; due to the fact that repulsion exists among magnesium ions, graphene materials can be prevented from being stacked mutually, the graphene materials in the surface enhanced heat transfer composite material obtained through the method are connected to the conductive material in a vertical orientation mode, active sites can be increased through the vertically-oriented connected graphene materials, the superheat degree required by phase change heat transfer nuclear boiling initiation is reduced, the vertically-oriented graphene material structure has the function of restraining bubble growth, bubbles are promoted to be separated in a small-size state, and the phase change heat transfer rate can be remarkably improved.
The invention also aims to provide a graphene surface enhanced heat transfer composite material, which is prepared by the preparation method of the graphene surface enhanced heat transfer composite material.
Preferably, the graphene material comprises a conductive material and a graphene material adsorbed on the conductive material, and the graphene material is connected on the conductive material in a vertical orientation mode.
The beneficial effects of the graphene surface enhanced heat transfer composite material provided by the invention are the same as the preparation method of the graphene surface enhanced heat transfer composite material, and are not repeated herein.
Drawings
FIG. 1 is a flowchart of a method for preparing a graphene surface enhanced heat transfer composite material according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the redox reaction mechanism in the electrophoretic deposition process;
FIG. 3 is a SEM electron microscope top view of the surface graphene reinforced heat transfer composite in the embodiment of the invention;
FIG. 4 is an SEM electron microscope side view of the graphene surface enhanced heat transfer composite in the embodiment of the invention;
FIG. 5 is a schematic structural view of a heat flux density measuring apparatus;
FIG. 6 is a comparison of heat flow density curves for different materials in accordance with an embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments thereof are described in detail below.
It should be noted that the features in the embodiments of the present invention may be combined with each other without conflict. The terms "comprising," "including," "containing," and "having" are intended to be inclusive, i.e., that additional steps and other ingredients may be added without affecting the result. The above terms encompass the terms "consisting of … …" and "consisting essentially of … …". Materials, equipment and reagents are commercially available unless otherwise specified.
The embodiment of the invention provides a preparation method of a graphene surface enhanced heat transfer composite material, which comprises the following steps of:
step S1, uniformly mixing the graphene material with isopropanol to form a graphene material solution with negative electricity;
step S2, adding a magnesium salt into the graphene material solution to prepare a mixed solution, wherein the weight ratio of the graphene material to the magnesium salt is 1: 5-3: 1;
and step S3, taking the conductive material as a cathode, and performing electrophoretic deposition in the mixed solution to obtain the graphene surface enhanced heat transfer composite material.
In step S1, the graphene material is added to isopropanol, and ultrasonically dispersed for 1 hour to form a uniform graphene solution. Wherein the graphene material comprises Graphene Oxide (GO) or reduced graphene oxide (rGO). Graphene materials such as GO and rGO have stronger hydrophilicity and exhaust performance, and can promote liquid to flow in a circulating mode between a dry area and a wet area, and the liquid is connected to the surface of a heat conduction substrate to accelerate the cooling rate and improve the heat transfer effect. The graphene material can be fully dispersed in isopropanol by an ultrasonic dispersion mode, so that a uniform graphene solution is obtained.
In step S2, magnesium salt is added into the graphene solution to prepare a mixed solution, wherein the weight ratio of the graphene material to the magnesium salt is 1: 5-3: 1. Wherein the magnesium salt is magnesium nitrate, magnesium carbonate or magnesium sulfate. Magnesium ions are contained in the magnesium salt, the magnesium ions have positive charges, a large number of functional groups with negative charges are distributed on the surface of the graphene material, and through the attraction effect of the positive charges and the negative charges, a large number of magnesium ions can be adsorbed on the surface of the graphene material. The weight ratio of graphene material to magnesium salt is preferably set to 1: 1.
In step S3, the platinum sheet is used as an anode and the conductive material is used as a cathode, and the electrophoretic deposition is performed in the mixed solution, wherein the reflection voltage is set to 220V during the electrophoretic deposition, and the reaction time is 2 min. Wherein the conductive material comprises an aluminum sheet, a copper sheet, carbon cloth or carbon fiber.
As shown in fig. 2, in the electrophoretic deposition process, due to the existence of a strong electric field, the particles in the mixed solution undergo redox reactions on the positive and negative electrode materials, wherein the anode undergoes the following reactions:
4OH--4e-→2H2O+O2
and the reaction at the cathode is as follows:
O2+2H2O+4e-→4OH-
NO3 -+H2O+2e-→NO2 -+2OH-
Mg2++2OH-→Mg(OH)2
namely, magnesium ions in the solution react with hydroxyl groups on the cathode conductive material to generate magnesium hydroxide, and the magnesium ions are connected with the graphene material on one hand and connected with the cathode conductive material through the hydroxyl groups on the other hand, so that the graphene material can be connected with the conductive material through the bridge action of the magnesium hydroxide to form a composite material, and due to the existence of repulsion among the magnesium ions, the graphene materials can be prevented from being stacked with each other, so that the graphene material is connected on the conductive material in a vertical orientation mode, active sites can be increased by the vertically-oriented graphene material, the superheat degree required by the boiling initiation of phase-change heat transfer nuclei is reduced, and the vertically-oriented structure of the graphene material has the function of inhibiting the growth of bubbles, so that the bubbles are separated in a small-size state, and the phase-change heat transfer rate can be remarkably improved.
In addition, a large number of carboxyl groups and other groups are distributed on the graphene material and can react with hydroxyl groups on the conductive material to form ester groups, and the ester groups are connected by strong chemical bonds, and the amount of the ester groups is also increased along with the rise of temperature in the phase change heat transfer process, so that the connection stability of the graphene material and the conductive material can be further enhanced.
Another embodiment of the present invention provides a graphene surface enhanced heat transfer composite material, which is prepared by the above preparation method of the graphene surface enhanced heat transfer composite material, and includes a conductive material and a graphene material adsorbed on the conductive material, wherein the graphene material is connected to the conductive material in a vertical orientation manner.
The preparation method of the graphene surface enhanced heat transfer composite material is described by combining the following specific embodiments:
example 1
1.1, adding reduced graphene oxide (rGO) into isopropanol, and performing ultrasonic dispersion for 1h to obtain a uniformly dispersed GO solution;
1.2, adding magnesium nitrate into the rGO solution, and uniformly mixing to obtain a mixed solution of rGO and magnesium nitrate, wherein the mass ratio of the rGO to the magnesium nitrate is 1: 1;
and 1.3, taking a platinum sheet as an anode and an aluminum sheet as a cathode, wherein the reaction voltage is 220V, and the reaction time is 2min, so that the particles in the mixed solution are subjected to redox reaction on the anode and the cathode, and the rGO is adsorbed on the aluminum sheet and is connected with the aluminum sheet in a vertical orientation mode, thereby obtaining the graphene surface enhanced heat transfer composite material.
Example 2
2.1, adding Graphene Oxide (GO) into isopropanol, and performing ultrasonic dispersion for 1h to obtain a uniformly dispersed GO solution;
2.2, adding magnesium sulfate into the GO solution, and uniformly mixing to obtain a mixed solution of GO and magnesium sulfate, wherein the mass ratio of GO to magnesium sulfate is 1: 3;
and 2.3, taking a platinum sheet as an anode and a copper sheet as a cathode, wherein the reaction voltage is 220V, and the reaction time is 2min, so that the particles in the mixed solution are subjected to redox reaction on the anode and the cathode, and the GO is adsorbed on the copper sheet and is connected with the copper sheet in a vertical orientation mode, thereby obtaining the graphene surface enhanced heat transfer composite material.
Example 3
3.1, adding reduced graphene oxide (rGO) into isopropanol, and performing ultrasonic dispersion for 1h to obtain a uniformly dispersed GO solution;
3.2, adding magnesium carbonate into the rGO solution, and uniformly mixing to prepare a mixed solution of the rGO and the magnesium carbonate, wherein the mass ratio of the rGO to the magnesium carbonate is 1: 5;
and 3.3, taking a platinum sheet as an anode and an aluminum sheet as a cathode, wherein the reaction voltage is 220V, and the reaction time is 2min, so that the particles in the mixed solution are subjected to redox reaction on the anode and the cathode, and the rGO is adsorbed on the aluminum sheet and is connected with the aluminum sheet in a vertical orientation mode, thereby obtaining the graphene surface enhanced heat transfer composite material.
Experimental example 1
The composite material formed by the reduced graphene oxide prepared in example 1 and the aluminum sheet was observed under an SEM electron microscope.
Fig. 3 and 4 are top and side views, respectively, of the composite under SEM electron microscopy, and from fig. 3 and 4 it can be seen that rGO is attached to the surface of the aluminum sheet with less overlap by vertical orientation. The method is mainly characterized in that in the electrophoretic deposition process, an anode and a cathode generate redox reaction, magnesium ions in a mixed solution are firstly combined with rGO to change the electronegativity of the rGO, and magnesium hydroxide is generated through the redox reaction generated by the cathode and can be used as a bridge to connect the rGO with an aluminum sheet; meanwhile, due to the existence of repulsive force between magnesium ions, stacking between the rGO sheet layers can be prevented, and the rGO can be connected to the aluminum sheet in a vertical orientation mode.
Experimental example 2
The heat flow density curves of pure aluminum and the Al/rGO pool boiling heat transfer material prepared in example 1 were tested respectively in the following manner:
pure aluminum and the Al/rGO pool boiling heat transfer material prepared in example 1 were used as samples to be tested, respectively, and the material heat flux density was tested by a set of self-made measuring devices, which consisted of a heating system, a sealing system and a data acquisition system, as shown in FIG. 5. The heating system is composed of a copper heating block andthe sample to be measured is formed by processing threaded connection, and the thread size is
The length is 7 mm. The copper heating block and the sample to be measured are both provided with
Holes, 9mm deep, represent the position of a thermocouple of type K (± 0.2K). The spacing between each thermocouple in the copper block was 5mm for measuring the temperature gradient (T) in the direction of heat flow1、T2、T3). In addition, a thermocouple inside the sample to be measured is used to measure the wall temperature (T)w). Adopts alumina silicate ceramic fiber (k is less than 0.14W m)-1k-1) The copper heating block was wrapped and a water resistant sealant was applied around the aluminum sample to reduce heat loss from the apparatus to the surrounding environment. A data acquisition system (HIOKI LR8450, japan) was used to monitor the temperature change of the thermocouple. Further, the movement of the underwater steam bubbles was observed by a high-speed camera (FASTCAM Mini UX100, japan).
The water in the container is first heated to boiling state and maintained for half an hour to eliminate insoluble gas in the water. Surface temperature T of sample to be measuredwAfter reaching 100 ℃, the test is started, the heating rod is increased by 5W power from the initial power, and the test is waited after the power is increased until T1，T2，T3The temperature is not changing and a steady state is reached, at which time relevant temperature data is recorded. And increasing the power of the heating rod by 5W again, and repeating the steps to finally obtain the critical heat flow density, and then finishing the test (the critical heat flow density refers to the maximum heat flow density obtained in the test process). By measuring T1And T2、T2And T3、T1And T3The temperature difference between the two is combined with the known heat conductivity of the copper block, and the heat flow density q' is calculated according to the Fourier heat conduction law:
in the formula, kCuIs a copper blockThermal coefficient of 401W m-1 K-1Δ x is thermocouple T1And T2The spacing therebetween. Degree of superheat Δ T of wall surfacewCan be calculated by the following formula:
ΔTw＝Tw-Tsat
wherein T iswIs the wall temperature, T, of the sample to be measuredsatIs the water saturation boiling temperature of 100 ℃.
In fig. 6, the abscissa represents the degree of superheat Δ T of the wall surfacewThe ordinate represents the heat flow density q ″, Al represents pure aluminum, and Al/rGO represents the graphene surface enhanced heat transfer composite material prepared in example 1, and as can be seen from fig. 6, the graphene surface enhanced heat transfer composite material prepared in example 1 has a larger critical heat flow density (CHF) and a smaller phase change heat transfer nucleation boiling superheat degree (ONB) compared to pure aluminum, wherein CHF is increased by 95%, indicating that the graphene surface enhanced heat transfer composite material prepared in the embodiment of the present invention significantly improves the phase change heat transfer performance compared to pure aluminum.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (10)
1. The preparation method of the graphene surface enhanced heat transfer composite material is characterized by comprising the following steps:
step S1, uniformly mixing the graphene material with isopropanol to form a graphene material solution with negative electricity;
step S2, adding a magnesium salt into the graphene solution to prepare a mixed solution, wherein the weight ratio of the graphene material to the magnesium salt is 1: 5-3: 1;
and step S3, taking the conductive material as a cathode, and performing electrophoretic deposition in the mixed solution to obtain the graphene surface enhanced heat transfer composite material.
2. The method for preparing the surface-enhanced heat transfer composite material according to claim 1, wherein in the step S1, the graphene material is added into the isopropanol and ultrasonically dispersed for 1h to form a uniform graphene solution.
3. The method for preparing the surface enhanced heat transfer composite material according to claim 1, wherein the graphene material comprises graphene oxide or reduced graphene oxide.
4. The method for preparing the surface-enhanced heat transfer composite material according to claim 1, wherein the magnesium salt comprises magnesium nitrate, magnesium carbonate or magnesium sulfate.
5. The method for preparing the surface enhanced heat transfer composite material according to claim 1, wherein in the step S2, the weight ratio of the graphene material to the magnesium salt is 1: 1.
6. The method for preparing a surface enhanced heat transfer composite according to claim 1, wherein in step S3, a platinum sheet is used as an anode in the electrophoretic deposition process.
7. The method for preparing a surface enhanced heat transfer composite material according to claim 1, wherein in step S3, the reaction voltage during the electrophoretic deposition process is 220V, and the reaction time is 2 min.
8. The method for preparing the surface-enhanced heat transfer composite material according to claim 1, wherein the conductive material comprises an aluminum sheet, a copper sheet, a carbon cloth or a carbon fiber.
9. A surface enhanced heat transfer composite material, characterized by being produced by the method for producing a surface enhanced heat transfer composite material according to any one of claims 1 to 8.
10. The surface-enhanced heat transfer composite of claim 9, comprising an electrically conductive material and a graphene material adsorbed on the electrically conductive material, wherein the graphene material is attached to the electrically conductive material by vertical orientation.
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| CN102021633A (en) * | 2009-09-09 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of graphene thin film field emission material |
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| TW202108964A (en) * | 2019-08-30 | 2021-03-01 | 國立中央大學 | A heat transfer enhancement device having graphene |
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| CN102021633A (en) * | 2009-09-09 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of graphene thin film field emission material |
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| TW202108964A (en) * | 2019-08-30 | 2021-03-01 | 國立中央大學 | A heat transfer enhancement device having graphene |
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