CN111072318B - Graphene aerogel phase-change composite material with oriented heat conduction characteristic and preparation method thereof - Google Patents
Graphene aerogel phase-change composite material with oriented heat conduction characteristic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a graphene aerogel phase-change composite material with oriented heat conduction characteristics and a preparation method thereof, wherein the method comprises the following steps: mixing the graphene oxide solution with expanded graphite to form uniform dispersion liquid, and freezing the dispersion liquid in a liquid nitrogen atmosphere to obtain the ice-containing GO/EG anisotropic mixed hydrogel; freeze-drying the ice-containing GO/EG anisotropic mixed hydrogel in a freeze dryer to obtain GO/EG anisotropic aerogel; heating GO/EG anisotropic aerogel in an oven to obtain rGO/EG anisotropic mixed aerogel; putting the rGO/EG anisotropic mixed aerogel into molten paraffin, adsorbing the paraffin to saturation, and naturally cooling to obtain the rGO/EG mixed aerogel phase-change composite material, wherein the obtained graphene aerogel phase-change composite material has orientation heat-conducting property and good stability.
Description
Technical Field
The invention relates to the technical field of energy storage and directional heat conduction, in particular to a graphene aerogel phase-change composite material with a directional heat conduction characteristic and a preparation method thereof.
Background
The energy problem is a great problem faced by the human in the 21 st century, and every aspect of human production and life cannot leave the energy. Meanwhile, with the rapid development of the world economy, the demand of human beings on energy is higher and higher. The energy on the earth is limited, so that the heat storage and energy saving material has more and more practical significance on the reasonable utilization and saving of the energy. The advent of thermal energy storage systems has not only helped to reduce the dependence on fossil fuels, but also helped to make efficient and benign use of energy. In this system, thermal energy can be stored in sensible and latent form. The relative volume of material required for latent heat storage is smaller compared to sensible heat storage. Latent heat storage has received much attention. Latent heat storage is also called phase change heat storage. The phase-change material can absorb and release a large amount of phase-change latent heat in the phase-change process, and is widely applied to the fields of heat energy storage and temperature control. Phase change materials can be classified into inorganic phase change materials and organic phase change materials according to their physical properties. The organic phase change material has the advantages of high phase change latent heat, small supercooling degree, no phase separation and the like, is widely applied, but has the problems of small heat conductivity, easy leakage, incapability of meeting the requirement of directional heat conduction and the like, and different solutions have been proposed to overcome the problems.
Aiming at the problem of low thermal conductivity of the phase-change material, the most widely solved method is to add a thermal conductivity material. For example, metal powder, carbon material or inorganic material, a three-dimensional heat-conducting network structure is prepared, and the phase-change material is immersed in the heat-conducting network, so that the heat-conducting property of the phase-change material can be effectively improved. Finally, the phase change material is compounded with the porous material with high thermal conductivity in a microcapsule form, so that the thermal conductivity of the phase change material can be improved, and the aim of further encapsulating the phase change material is fulfilled.
Carbon materials are most widely used as heat-conducting reinforcing phase materials. Since the true densities of different types of carbon materials are not greatly different, each carbon material has advantages in practical applications. In summary, carbon additives with higher aspect ratios have better thermal conductivity enhancement. Expanded Graphite (EG) is made from natural flake graphite and exhibits better thermal properties than flake graphite. However, if EG is directly compounded with the phase change material, the two are simply physically mixed, and the phase change material may leak.
Patent CN 110205100a discloses a phase-change composite material based on reduced graphene oxide/expanded graphite mixed aerogel and a preparation method thereof, however, the composite material adopts a hydrothermal method, graphene oxide is self-assembled through high temperature and high pressure, so that isotropic mixed aerogel is obtained through preparation, and the performance does not meet the high standard use requirement.
Disclosure of Invention
The invention aims to solve the problems and provide a reduced graphene oxide/expanded graphite aerogel phase-change composite material with oriented heat conduction performance and good stability and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a graphene aerogel phase-change composite material with oriented heat conduction characteristics comprises the following steps:
mixing the graphene oxide solution with expanded graphite to form uniform dispersion liquid, and freezing the dispersion liquid in a liquid nitrogen atmosphere to obtain the ice-containing GO/EG anisotropic mixed hydrogel;
freeze-drying the ice-containing GO/EG anisotropic mixed hydrogel in a freeze dryer to obtain GO/EG anisotropic aerogel;
heating GO/EG anisotropic aerogel in an oven to obtain rGO/EG anisotropic mixed aerogel;
and putting the rGO/EG anisotropic mixed aerogel into molten paraffin, and naturally cooling after the paraffin is adsorbed to saturation to obtain the rGO/EG mixed aerogel phase-change composite material.
The oriented freezing method is carried out at ultralow temperature, the graphene oxide expanded graphite is directionally frozen by liquid nitrogen, the change of the freezing temperature has obvious gradient, when the graphene oxide expanded graphite is frozen, ice crystals are orderly arranged upwards, graphene oxide sheets have hydrophilicity and are attached to the surface of an ice template for arrangement, a graphene sheet layer shows the structure of the ice template after freeze-drying, deicing and reduction, namely the ordered fence shape, the anisotropic graphene oxide expanded graphene aerogel is formed, the oriented structural characteristic is achieved, the aerogel is compounded with paraffin, and the phase-change composite material with structural anisotropy and oriented heat conduction characteristic can be prepared.
Preferably, the graphene oxide is prepared by adopting a modified Hummer method, and the concentration of the graphene oxide solution is 8-12 mg/ml.
Preferably, the expanded graphite accounts for 20-80% of the total mass of the graphene oxide and the expanded graphite.
Preferably, the dispersion is frozen in a liquid nitrogen atmosphere for 50-70 min.
Preferably, the temperature of the freeze dryer is-70-0 ℃, and the freeze-drying time is 40-60 h.
Preferably, the oven temperature is 240-260 ℃, and the heating time is 1.5-2.5 h.
Preferably, the rGO/EG anisotropic mixed aerogel is cut into round cakes with the thickness of 2-8 cm, and then is put into completely molten paraffin.
The phase-change composite material consists of aerogel with an anisotropic structure and a phase-change material, wherein the phase-change material is paraffin, the aerogel consists of reduced graphene oxide and expanded graphite, and the mass fraction of the expanded graphite in the aerogel is 20-80%.
The structure of the graphene oxide mainly comprises two parts, namely an oxidized region (hydrophilic region) and an unoxidized region (hydrophobic region), and can be regarded as a product obtained after the inner part and the edge of a graphene sheet layer are modified by oxygen-containing functional groups (mainly comprising hydroxyl, carboxyl, epoxy and the like), and the special structure enables the graphene oxide to be regarded as a two-dimensional polymer, an anisotropic colloid, an amphiphilic substance and the like. When expanded graphite mixes with graphite oxide, because expanded graphite has the hydrophobicity, consequently graphite oxide's hydrophobic end and expanded graphite contact, hydrophilic end and aqueous solution contact to form comparatively stable graphite oxide expanded graphite mixed suspension, the graphite alkene aerogel has excellent heat conductivity, can be used for improving phase change material thermal conductivity. The expanded graphite has porosity, and the expanded graphite with a three-dimensional structure not only has a good heat conducting network, but also has the porosity which is more beneficial to adsorbing the phase-change material.
The key point of the invention is that the graphene oxide expanded graphite is directionally frozen by liquid nitrogen, so that the change of the freezing temperature has obvious gradient, when the graphene oxide expanded graphite is frozen, ice crystals are orderly arranged upwards, graphene oxide sheets have good hydrophilicity and are easy to adhere to an ice template to grow, after freeze-drying, deicing and reduction are carried out, graphene sheet layers show the structure of the original ice template, namely an ordered fence shape, and the graphene oxide expanded graphene anisotropic aerogel is formed.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
(1) the method adopts an ultralow-temperature directional freezing method, and realizes directional assembly of graphene oxide through arrangement and extrusion of the graphene oxide by the ice crystals, so that the anisotropic reduced graphene oxide/expanded graphite mixed aerogel phase-change composite material is prepared, the application field of the phase-change material is greatly widened, and the phase-change material with a directional heat conduction structure is often needed in the fields of buildings, solar heat collection equipment, electronic heat dissipation and the like; the patent CN 110205100a adopts a hydrothermal method in the preparation method, and graphene oxide is self-assembled at high temperature and high pressure to obtain isotropic mixed aerogel, which cannot be applied to more occasions.
(2) The reduced graphene oxide/expanded graphite anisotropic aerogel phase-change composite material prepared by the technology has excellent directional heat-conducting property and structural stability compared with a phase-change material, along with the increase of expanded graphite, the heat-conducting coefficient of the reduced graphene oxide/expanded graphite anisotropic aerogel phase-change composite material is gradually increased, the three-dimensional structure of the aerogel has excellent heat conductivity, and the porous structure of the aerogel is favorable for adsorbing the phase-change material and also has certain packaging property.
Drawings
FIG. 1 is a flow chart of the preparation of a reduced graphene oxide/expanded graphite anisotropic aerogel phase change composite;
fig. 2 is an FTIR plot of reduced graphene oxide/expanded graphite anisotropic aerogels before and after high temperature reduction;
FIG. 3 is a diagram of reduced graphene oxide/expanded graphite anisotropic aerogel phase-change composite material in different proportions;
fig. 4 is SEM photographs of reduced graphene oxide/expanded graphite anisotropic aerogel sides at different magnifications;
fig. 5 is SEM photographs of reduced graphene oxide/expanded graphite anisotropic aerogel front surfaces at different magnifications;
fig. 6 is a thermal conductivity diagram of a reduced graphene oxide/expanded graphite anisotropic aerogel phase change composite.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The reduced graphene oxide/expanded graphite anisotropic aerogel phase-change composite material is mainly prepared and synthesized from graphene oxide, expanded graphite and a phase-change material, and the specific preparation process is shown in figure 1.
The paraffin used by the invention is provided by the national drug group chemical reagent company Limited, and has the specification of chemical purity, the melting point of 48-52 ℃ and the density of 0.86g/cm3. Natural flake graphite of 200 mesh was purchased from shanghai monosail graphite products ltd. Expanded Graphite (EG) is supplied by Hebei Baoding Shuixing cemented carbide Co., Ltd, and has an expansion rate of 150ml/g and an average particle diameter before expansion of 0.18 mm.
Example 1
(1) Graphene Oxide (GO) was prepared by oxidizing natural graphite powder according to the modified Hummers method.
(2) Adding the graphene oxide solution with the concentration of 10mg/ml into the expanded graphite accounting for 20% of the total mass, and uniformly stirring to obtain the dispersion liquid.
(3) And (3) placing the dispersion liquid in a liquid nitrogen atmosphere, and freezing for 1h to obtain the ice-containing GO/EG anisotropic mixed hydrogel.
(4) And (3) freeze-drying the ice-containing GO/EG anisotropic mixed hydrogel for 40-60h in a freeze dryer at the temperature of 0-70 ℃ to obtain the GO/EG anisotropic aerogel.
(5) Putting the GO/EG anisotropic aerogel into an oven, starting the oven to heat, timing for 2 hours after the temperature reaches 250 ℃, keeping the temperature for 2 hours to obtain the rGO/EG anisotropic aerogel, and displaying FTIR (infrared spectroscopy) graphs of the reduced graphene oxide/expanded graphite anisotropic aerogel before and after high-temperature reduction in fig. 2.
(6) Cut into the cake that thickness is 2 ~ 8cm with rGO/EG mixed aerogel, put into complete melting paraffin, rGO/EG mixed aerogel adsorbs paraffin rapidly, treats that paraffin adsorbs to saturation, takes out, and natural cooling obtains rGO/EG mixed aerogel phase change composite. The physical diagram of the obtained reduced graphene oxide/expanded graphite anisotropic phase-change composite material is shown in fig. 3. The scanning electron microscope shows that the reduced graphene oxide/expanded graphite aerogel is anisotropic, and the side section is in a fence shape, as shown in fig. 4. The normal section is mostly a small graphene sheet, as shown in fig. 5.
FIG. 2 is a Fourier infrared spectrum detection result of the reduced graphene oxide/expanded graphite anisotropic aerogel obtained in example 1 before and after high-temperature reduction, and it can be seen that the sample is 1734cm before reduction-1At 1200cm C ═ O peak-1At a C-O-C peak of 1050cm-1The C-O peak has a larger peak value, which indicates that the graphene oxide before reduction contains a large amount of oxygen-containing functional groups. After reduction, these peaks are significantly reduced, but do not disappear, meaning that the oxygen-containing groups cannot be completely reduced by high-temperature reduction, and the oxygen-containing functional groups still remain in the reduced graphene oxide/expanded graphite anisotropic aerogel after reduction. Meanwhile, according to the infrared spectrum, the change of the carbon chain structure can be observed. Before reduction, 1620cm-1There is a distinct peak, which is the skeletal oscillation of C ═ C. The double bond vibration of the reduced sample almost disappeared, but at 1580cm-1Shows an absorption peak of a benzene ring skeleton, 739cm-1An absorption peak of a long-chain carbon chain appears, which indicates that a typical hydrocarbon structure appears after the sample is reduced, the property is changed from hydrophilic to hydrophobic, and meanwhile, the carbon chain tends to be lengthened and ordered; on the other hand, the double bond was changed to a benzene ring and a single bond, which also confirmed that the reduction reaction did occur in the sample.
Fig. 4 is a scanning electron microscope image of a side section of the reduced graphene oxide/expanded graphite anisotropic aerogel obtained in example 1, and it can be seen that graphene obviously grows along the vertical direction and presents a fence shape, each layer of graphene is connected by scattered graphene sheets, and the expanded graphite is hidden in the graphene sheet layer; fig. 5 is a scanning electron microscope image of a cross section of the reduced graphene oxide/expanded graphite anisotropic aerogel obtained in example 1, and we can see that most of the electron microscope images of the cross section are small graphene sheets, and the graphene sheets almost perpendicular to the drawing surface can be observed from the electron microscope image with a large magnification, and many gaps are filled between the sheets.
Example 2
(1) Graphene Oxide (GO) was prepared by oxidizing natural graphite powder according to the modified Hummers method.
(2) Adding the graphene oxide solution with the concentration of 10mg/ml into expanded graphite accounting for 40% of the total mass, and uniformly stirring to obtain a dispersion liquid.
(3) And (3) placing the dispersion liquid in a liquid nitrogen atmosphere, and freezing for 1h to obtain the ice-containing GO/EG anisotropic mixed hydrogel.
(4) And (3) freeze-drying the ice-containing GO/EG anisotropic mixed hydrogel for 40-60h in a freeze dryer at the temperature of 0-70 ℃ to obtain the GO/EG anisotropic aerogel.
(5) And placing the GO/EG anisotropic aerogel in a drying oven, starting the drying oven to heat, timing for 2 hours after the temperature reaches 250 ℃, and keeping the temperature for 2 hours to obtain the rGO/EG anisotropic aerogel.
(6) Cut into the cake that thickness is 2 ~ 8cm with rGO/EG mixed aerogel, put into complete melting paraffin, rGO/EG mixed aerogel adsorbs paraffin rapidly, treats that paraffin adsorbs to saturation, takes out, and natural cooling obtains rGO/EG mixed aerogel phase change composite. The physical diagram of the obtained reduced graphene oxide/expanded graphite anisotropic phase-change composite material is shown in fig. 3.
Example 3
(1) Graphene Oxide (GO) was prepared by oxidizing natural graphite powder according to the modified Hummers method.
(2) Adding the graphene oxide solution with the concentration of 10mg/ml into the expanded graphite accounting for 60% of the total mass, and uniformly stirring to obtain the dispersion liquid.
(3) And (3) placing the dispersion liquid in a liquid nitrogen atmosphere, and freezing for 1h to obtain the ice-containing GO/EG anisotropic mixed hydrogel.
(4) And (3) freeze-drying the ice-containing GO/EG anisotropic mixed hydrogel for 40-60h in a freeze dryer at the temperature of 0-70 ℃ to obtain the GO/EG anisotropic aerogel.
(5) And placing the GO/EG anisotropic aerogel in a drying oven, starting the drying oven to heat, timing for 2 hours after the temperature reaches 250 ℃, and keeping the temperature for 2 hours to obtain the rGO/EG anisotropic aerogel.
(6) Cut into the cake that thickness is 2 ~ 8cm with rGO/EG mixed aerogel, put into complete melting paraffin, rGO/EG mixed aerogel adsorbs paraffin rapidly, treats that paraffin adsorbs to saturation, takes out, and natural cooling obtains rGO/EG mixed aerogel phase change composite. The physical diagram of the obtained reduced graphene oxide/expanded graphite anisotropic phase-change composite material is shown in fig. 3.
Example 4
(1) Graphene Oxide (GO) was prepared by oxidizing natural graphite powder according to the modified Hummers method.
(2) Adding the graphene oxide solution with the concentration of 10mg/ml into the expanded graphite accounting for 60% of the total mass, and uniformly stirring to obtain the dispersion liquid.
(3) And (3) placing the dispersion liquid in a liquid nitrogen atmosphere, and freezing for 1h to obtain the ice-containing GO/EG anisotropic mixed hydrogel.
(4) And (3) freeze-drying the ice-containing GO/EG anisotropic mixed hydrogel for 40-60h in a freeze dryer at the temperature of 0-70 ℃ to obtain the GO/EG anisotropic aerogel.
(5) And placing the GO/EG anisotropic aerogel in a drying oven, starting the drying oven to heat, timing for 2 hours after the temperature reaches 250 ℃, and keeping the temperature for 2 hours to obtain the rGO/EG anisotropic aerogel.
(6) Cut into the cake that thickness is 2 ~ 8cm with rGO/EG mixed aerogel, put into complete melting paraffin, rGO/EG mixed aerogel adsorbs paraffin rapidly, treats that paraffin adsorbs to saturation, takes out, and natural cooling obtains rGO/EG mixed aerogel phase change composite.
The thermal conductivity of the series of reduced graphene oxide/expanded graphite anisotropic aerogel phase-change composite materials with variable doping amounts is shown in fig. 6.
Fig. 6 is thermal conductivity data of reduced graphene oxide/expanded graphite anisotropic aerogel phase-change composites obtained in examples 1, 2, 3, and 4. The thermal conductivity of the pure paraffin measured at room temperature was 0.19 W.K-1m-1. As can be seen from the figure, the thermal conductivity of the phase-change composite material is obviously gradually increased along with the gradual increase of the doping amount of the expanded graphite. When the content of the expanded graphite is 80 ms%, the longitudinal thermal conductivity of the phase-change composite material is 0.789WK-1m-1Compared with pure paraffin, the thermal conductivity is increased by 280%, and in the patent CN 110205100A, the same raw material is adopted, and the thermal conductivity of the phase-change composite material obtained by the preparation method is 0.6 W.K-1m-1By adopting the method disclosed by the invention to prepare the phase-change composite material with the directional heat conduction characteristic, the heat conductivity can be improved by 31.5%, and the method is obviously improved.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (4)
1. A preparation method of a graphene aerogel phase change composite material with oriented heat conduction characteristics is characterized by comprising the following steps:
mixing the graphene oxide solution with expanded graphite to form uniform dispersion liquid, and freezing the dispersion liquid in a liquid nitrogen atmosphere to obtain the ice-containing GO/EG anisotropic mixed hydrogel;
freeze-drying the ice-containing GO/EG anisotropic mixed hydrogel in a freeze dryer to obtain GO/EG anisotropic aerogel;
heating GO/EG anisotropic aerogel in an oven to obtain rGO/EG anisotropic mixed aerogel;
putting the rGO/EG anisotropic mixed aerogel into molten paraffin, and naturally cooling after the paraffin is adsorbed to saturation to obtain an rGO/EG mixed aerogel phase-change composite material;
freezing the dispersion liquid in liquid nitrogen atmosphere for 50-70 min; the temperature of the freeze dryer is-70-0 ℃, and the freeze drying time is 40-60 h;
the expanded graphite accounts for 20-80% of the total mass of the graphene oxide and the expanded graphite;
the temperature of the oven is 240 ℃ and 260 ℃, and the heating time is 1.5-2.5 h.
2. The preparation method of the graphene aerogel phase change composite material as claimed in claim 1, wherein the graphene oxide is prepared by a modified Hummer method, and the concentration of the graphene oxide solution is 8-12 mg/ml.
3. The preparation method of the graphene aerogel phase-change composite material according to claim 1, wherein the rGO/EG anisotropic mixed aerogel is cut into round cakes with the thickness of 2-8 cm, and then is placed in completely molten paraffin.
4. The graphene aerogel phase-change composite material with oriented heat conduction characteristics, which is obtained by the preparation method of any one of claims 1 to 3.
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| CN113372883B (en) * | 2021-06-07 | 2022-05-17 | 山东国烯新材料创新中心有限公司 | High-thermal-conductivity composite phase change material based on solvent replacement method and preparation method thereof |
| CN113980468A (en) * | 2021-11-11 | 2022-01-28 | 华东理工大学 | Preparation method of vertically-oriented three-dimensional expanded graphite heat conductor and reinforced heat-conducting polymer matrix composite material thereof |
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