CN114408911A - Preparation method of graphene-based aerogel with ultra-fast light-thermal response - Google Patents

Preparation method of graphene-based aerogel with ultra-fast light-thermal response Download PDF

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CN114408911A
CN114408911A CN202210048446.6A CN202210048446A CN114408911A CN 114408911 A CN114408911 A CN 114408911A CN 202210048446 A CN202210048446 A CN 202210048446A CN 114408911 A CN114408911 A CN 114408911A
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CN114408911B (en
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吴晓宏
石婷
姚远
卢松涛
李杨
秦伟
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Harbin Institute of Technology
Chongqing Research Institute of Harbin Institute of Technology
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Abstract

The invention discloses a preparation method of graphene aerogel with ultra-fast light-thermal response, and belongs to the field of photo-thermal response materials. The invention aims to solve the technical problems of long response time and low steady-state temperature of the traditional carbon-based photo-thermal material. The method of the invention comprises the following steps: step one, under stirring, sequentially adding graphene oxide sponge and acidified carbon nanotubes into deionized water, uniformly dispersing, adding lithium sulfate, performing liquid-phase self-assembly after the lithium sulfate is added, quickly freezing after the self-assembly is finished, and freeze-drying; and step two, vacuum drying and constant-temperature calcining under the protection of inert gas to obtain the graphene-based aerogel. The aerogel prepared by the invention has ultra-fast photo-thermal response, and the advantage of high steady-state temperature makes the aerogel hopeful to realize potential application in multiple fields.

Description

Preparation method of graphene-based aerogel with ultra-fast light-thermal response
Technical Field
The invention belongs to the field of photo-thermal response materials, and particularly relates to a preparation method of graphene-based aerogel with ultra-fast photo-thermal response.
Background
With the increasing exhaustion of non-renewable energy sources such as coal, petroleum, natural gas and the like, the development and utilization of solar energy have become important contents of sustainable development strategies of various countries. The photothermal conversion is one of important ways to effectively utilize solar energy, and can effectively expand the application range of the solar energy to important research and application fields such as photothermal therapy, water body environment purification, seawater desalination, catalysis and the like. Therefore, the search for and development of high-efficiency photothermal conversion materials has been extensively studied by scientists.
The photothermal material converts solar energy into heat energy, specifically, electrons in the material interact with incident photons, and the absorption of photon energy is realized through two modes of ion excimer resonance or energy level transition, so that hot electrons in an excited state are generated. The thermal electrons in the excited state realize energy transfer and redistribution to the thermal equilibrium state development through secondary radiation or vibration relaxation. The process from the electron absorption photon in the material entering an excited state to the restoration of thermal equilibrium is macroscopically represented by the generation and diffusion of thermal energy (temperature) and the influence of factors such as the physical property, the structure and the size of the photo-thermal material. Currently, the photothermal material systems studied mainly include: plasma metal material, carbon-based material, and semiconductor material. Among these photothermal materials, the plasmonic metal nanoparticles have relatively good photothermal conversion capability, but have high cost, limited storage capacity and further improved stability; for semiconductor materials, the light absorption capability is weak and the material is unstable; and for the carbon material, it has excellent light absorption ability, thermal conductivity and physicochemical stability. The graphene-based photothermal material has weakly bound pi electrons in the energy level, and the electrons are excited to be promoted from a ground state (highest occupied molecular orbital, HOMO) to a higher-energy orbital (lowest unoccupied molecular orbital, LUMO). The excited electrons release heat when they return to their ground state by relaxation, so that they have good broadband light absorption ability and light-to-heat conversion ability, and have attracted much attention from scientists. However, graphene-based materials have the problems of long response time and low steady-state temperature, and the development and utilization of carbon-based photothermal materials are greatly limited by the two.
Disclosure of Invention
The invention aims to solve the technical problems of long response time and low steady-state temperature of the traditional carbon-based photothermal material, thereby greatly limiting the application of the carbon-based photothermal material in related fields; the invention provides a preparation method of three-dimensional highly-directionally-arranged radial centrosymmetric graphene-based aerogel. The aerogel prepared by the method has ultra-fast photo-thermal response and high steady-state temperature.
The graphene-based aerogel with highly oriented arrangement and radial centrosymmetric structure obtained by the method has ultrafast photo-thermal response and high steady-state temperature. Under the condition of illumination, the graphene-based aerogel material with a special structure obtained by the method can rapidly absorb photon energy, pi-pi transition occurs, excited electrons are relaxed by electron-phonon coupling, and the excited electrons are transferred into lattice vibration. In the highly oriented array structure, the further collective macroscopic arrangement of the electric dipoles accelerates the surface temperature of the material to reach a steady state. Therefore, the aerogel prepared by the invention has ultra-fast photo-thermal response, and the advantage of high steady-state temperature makes the aerogel hopefully realize potential application in multiple fields.
In order to realize the technical problem, the invention adopts the following technical scheme:
the invention aims to provide a preparation method of a three-dimensional highly-directionally-arranged radial centrosymmetric graphene-based aerogel, which comprises the following steps:
step one, under stirring, sequentially adding graphene oxide sponge and acidified carbon nanotubes into deionized water, uniformly dispersing, adding lithium sulfate, performing liquid-phase self-assembly after the lithium sulfate is added, quickly freezing after the self-assembly is finished, and freeze-drying;
step two, vacuum drying is carried out, and constant-temperature calcination is carried out under the protection of inert gas to obtain the graphene-based aerogel;
wherein the mass ratio of the graphene oxide sponge to the acidified carbon nanotube to the lithium sulfate in the first step is (20-60) to (10-40) to (10-30).
Further limiting, in the first step, the volume ratio of the total mass of the graphene oxide sponge, the acidified carbon nanotubes and the lithium sulfate to the deionized water is (0.6-3) g: (10-50) mL.
Further, the preparation method of the graphene oxide sponge in the first step is as follows: using crystalline flake graphite and 98% (mass) concentrated sulfuric acid (H)2SO4) Sodium nitrate (NaNO)3) Potassium permanganate (KMnO)4) And 30% by mass of hydrogen peroxide as a raw material, preparing graphene oxide by a liquid phase stripping method (Hummers), centrifugally washing the graphene oxide solution until the pH value of the solution is 7 after the reaction is finished, and freeze-drying the graphene oxide solution at-10 ℃ to obtain the graphene oxide sponge.
Further, the step one of acidifying the carbon nanotubes is performed according to the following steps: adding 120mL of concentrated sulfuric acid and 40mL of concentrated nitric acid into 1g of carbon nano tube, magnetically stirring, condensing and refluxing for 3h at 55 ℃, washing with deionized water until the pH value is 7 after the reaction is finished, and freeze-drying to obtain the acidified carbon nano tube.
Further, the step one is defined by utilizing liquid nitrogen to carry out quick freezing.
Further defined, the freeze-drying in step one is performed according to the following steps: and (3) putting the frozen solid into a freeze dryer, and continuously freeze-drying for 50-90 h at the vacuum degree of 0.5-10 Pa and the temperature of-10 ℃.
Further, the vacuum drying in the second step is performed according to the following steps: taking out the freeze-dried material, placing the material in a vacuum oven, and carrying out constant temperature treatment for 24-48 h at the vacuum degree of 2-10 Pa and the temperature of 60 ℃.
Further limiting, the constant-temperature calcination in the second step is carried out in a tubular furnace, the protective gas is nitrogen, and the constant-temperature calcination is carried out for 2 to 4 hours at the temperature of between 100 and 400 ℃.
The lithium sulfate adopted by the invention promotes self-assembly to form an orderly-arranged structure; after liquid phase self-assembly occurs in a mixed solution in which graphene oxide, carbon nano tubes and lithium sulfate exist simultaneously, the mixed solution is quickly frozen by liquid nitrogen in a bidirectional cold source, the radial growth of ice crystals is not laminar, and the irregular shape is accompanied by the change of thickness and roughness, so that a highly ordered structure is generated. The ice crystals are removed during sublimation, forming this highly ordered aerogel structure.
Compared with the prior art, the invention has the following beneficial effects:
on one hand: a large number of light trap structures are constructed by the special three-dimensional porous graphene-based aerogel array structure which is radially and centrally symmetrical, so that excellent light collection is realized, and effective absorption of solar radiation is improved. On the other hand: according to the special highly-oriented graphene-based aerogel structure, under the illumination condition, the carbon material absorbs photon energy to generate pi-pi transition, excited electrons are relaxed by electron-phonon coupling and transferred into lattice vibration, and further collective macroscopic arrangement of electric dipoles in a three-dimensional highly-oriented array structure can accelerate the increase of the surface temperature of the material.
For a better understanding of the nature and technical aspects of the present invention, reference should be made to the following detailed description of the invention, taken in conjunction with the accompanying drawings, which are provided for purposes of illustration and description, and are not intended to limit the invention.
Drawings
Fig. 1 is a temperature-time diagram and an infrared thermal imaging diagram of a graphene-based aerogel prepared by the method of example 1, wherein (a) the temperature-time diagram (b) in fig. 1 is an infrared thermal imaging diagram;
fig. 2 is a temperature-time chart and an infrared thermal imaging chart of the graphene-based aerogel prepared by the method of example 2, wherein in fig. 2, (a) the temperature-time chart, (b) the infrared thermal imaging chart;
fig. 3 is a temperature-time chart and an infrared thermal imaging chart of the graphene-based aerogel prepared by the method of example 3, wherein in fig. 2, (a) the temperature-time chart, (b) the infrared thermal imaging chart;
fig. 4 is a temperature-time chart and an infrared thermal imaging chart of the graphene-based aerogel prepared by the method of example 4, wherein in fig. 2, (a) the temperature-time chart, (b) the infrared thermal imaging chart;
FIG. 5 is a schematic diagram and a physical representation of a three-dimensional graphene-based aerogel prepared by the method of example 4;
FIG. 6 is a scanning electron microscope image of a three-dimensional graphene-based aerogel prepared by the method of example 4;
FIG. 7 is a scanning electron microscope photograph of a product prepared by the method of comparative example 1.
Detailed Description
The invention will be better understood by reference to the following examples. The invention is not limited to what has been described in the detailed description.
The graphene oxide sponges used in the following examples were prepared by the following steps: preparing graphene oxide by using crystalline flake graphite, 98 mass percent of concentrated sulfuric acid, sodium nitrate, potassium permanganate and 30 mass percent of hydrogen peroxide as raw materials through a liquid phase stripping method, centrifugally washing until the pH value of the solution is 7 after the reaction is finished, and freeze-drying at-10 ℃ to obtain the graphene oxide sponge.
The acidified carbon nanotubes used in the following examples were prepared by the following steps: adding 120mL of concentrated sulfuric acid and 40mL of concentrated nitric acid into 1g of carbon nano tube, magnetically stirring, condensing and refluxing for 3h at 55 ℃, washing with deionized water until the pH value is 7 after the reaction is finished, and freeze-drying to obtain the acidified carbon nano tube.
Example 1: in this embodiment, a preparation method of the graphene-based aerogel with ultra-fast photo-thermal response is performed according to the following steps:
step one, under stirring, sequentially adding 0.6g of sponge and 0.2g of acidified carbon nano tube into 30mL of deionized water, uniformly dispersing, adding 0.2g of lithium sulfate, carrying out liquid-phase self-assembly after the lithium sulfate is added, quickly freezing by using liquid nitrogen after the self-assembly is finished, putting the frozen solid into a freeze dryer, and continuously freeze-drying for 60 hours at the temperature of minus 10 ℃ under the vacuum degree of 2 Pa;
and step two, taking out the freeze-dried material, placing the material in a vacuum oven, carrying out constant temperature treatment for 24 hours at the vacuum degree of 5Pa and the temperature of 60 ℃, then placing the material in a tubular furnace, and calcining the material for 3 hours at the constant temperature of 100 ℃ under the protection of nitrogen to obtain the graphene-based aerogel.
The photothermal response test was performed at 1 sun. The temperature-time diagram and the infrared thermal imaging diagram of the graphene-based aerogel prepared by the method of this example are shown in fig. 1, and it can be seen from fig. 1a that the graphene-based aerogel shows a temperature response (40s, 59.8 ℃) and a uniform temperature distribution (fig. 1 b).
Example 2: in this embodiment, a preparation method of the graphene-based aerogel with ultra-fast photo-thermal response is performed according to the following steps:
step one, under stirring, sequentially adding 0.6g of graphene oxide sponge and 0.2g of acidified carbon nano tube into 30mL of deionized water, uniformly dispersing, adding 0.2g of lithium sulfate, performing liquid-phase self-assembly after the lithium sulfate is added, rapidly freezing by using liquid nitrogen after the self-assembly is finished, putting the frozen solid into a freeze dryer, and continuously freeze-drying for 60 hours at the temperature of minus 10 ℃ under the vacuum degree of 2 Pa;
and step two, taking out the freeze-dried material, placing the material in a vacuum oven, carrying out constant temperature treatment for 24 hours at the vacuum degree of 5Pa and the temperature of 60 ℃, then placing the material in a tube furnace, and calcining for 3 hours at the constant temperature of 200 ℃ under the protection of nitrogen to obtain the graphene-based aerogel.
The photothermal response test was performed at 1 sun. The temperature-time graph and the infrared thermal imaging graph of the graphene-based aerogel prepared by the method of the present embodiment are shown in fig. 2, and it can be seen from fig. 2a that the graphene-based aerogel shows a temperature response (40s, 66 ℃) and a uniform temperature distribution (fig. 2 b).
Example 3: in this embodiment, a preparation method of the graphene-based aerogel with ultra-fast photo-thermal response is performed according to the following steps:
step one, under stirring, sequentially adding 0.6g of graphene oxide sponge and 0.2g of acidified carbon nano tube into 30mL of deionized water, uniformly dispersing, adding 0.2g of lithium sulfate, performing liquid-phase self-assembly after the lithium sulfate is added, rapidly freezing by using liquid nitrogen after the self-assembly is finished, putting the frozen solid into a freeze dryer, and continuously freeze-drying for 60 hours at the temperature of minus 10 ℃ under the vacuum degree of 2 Pa;
and step two, taking out the freeze-dried material, placing the material in a vacuum oven, carrying out constant temperature treatment for 24 hours at the vacuum degree of 5Pa and the temperature of 60 ℃, then placing the material in a tube furnace, and calcining for 3 hours at the constant temperature of 300 ℃ under the protection of nitrogen to obtain the graphene-based aerogel.
The photothermal response test was performed at 1 sun. The temperature-time diagram and the infrared thermal imaging diagram of the graphene-based aerogel prepared by the method of this embodiment are shown in fig. 1, and it can be seen from fig. 3a that the graphene-based aerogel shows a temperature response (25s, 76.1 ℃) and a uniform temperature distribution (fig. 3 b).
Example 4: in this embodiment, a preparation method of the graphene-based aerogel with ultra-fast photo-thermal response is performed according to the following steps:
step one, under stirring, sequentially adding 0.6g of graphene oxide sponge and 0.2g of acidified carbon nano tube into 30mL of deionized water, uniformly dispersing, adding 0.2g of lithium sulfate, performing liquid-phase self-assembly after the lithium sulfate is added, rapidly freezing by using liquid nitrogen after the self-assembly is finished, putting the frozen solid into a freeze dryer, and continuously freeze-drying for 60 hours at the temperature of minus 10 ℃ under the vacuum degree of 2 Pa;
and step two, taking out the freeze-dried material, placing the material in a vacuum oven, carrying out constant temperature treatment for 24 hours at the vacuum degree of 5Pa and the temperature of 60 ℃, then placing the material in a tubular furnace, and calcining for 3 hours at the constant temperature of 400 ℃ under the protection of nitrogen to obtain the graphene-based aerogel.
The photothermal response test was performed at 1 sun. The temperature-time diagram and the infrared thermal imaging diagram of the graphene-based aerogel prepared by the method of this embodiment are shown in fig. 1, and it can be seen from fig. 4a that the graphene-based aerogel shows a temperature response (8s, 91.5 ℃) and a uniform temperature distribution (fig. 4 b).
TABLE 1 comparison of Properties of different photothermal materials
Figure BDA0003473489100000051
As can be seen from comparison in table 1, the graphene-based aerogel prepared in this embodiment has high photo-thermal conversion capability and stable temperature, and the physical diagram and schematic diagram of the graphene aerogel are shown in fig. 5a and b; the scan is shown in fig. 6.
Comparative example 1: step one, under stirring, sequentially adding 0.6g of graphene oxide sponge and 0.2g of acidified carbon nano tube into 30mL of deionized water, uniformly dispersing, quickly freezing by using liquid nitrogen, putting the frozen solid into a freeze dryer, and continuously freeze-drying for 60 hours at the temperature of-10 ℃ under the vacuum degree of 2 Pa;
and step two, taking out the freeze-dried material, placing the material in a vacuum oven, carrying out constant temperature treatment for 24 hours at the vacuum degree of 5Pa and the temperature of 60 ℃, then placing the material in a tubular furnace, and calcining for 3 hours at the constant temperature of 400 ℃ under the protection of nitrogen to obtain the graphene-based aerogel. The scan is shown in fig. 7, and a highly directional array structure cannot be formed.

Claims (10)

1. A preparation method of graphene-based aerogel with ultra-fast light-thermal response is characterized by comprising the following steps:
step one, under stirring, sequentially adding graphene oxide sponge and acidified carbon nanotubes into deionized water, uniformly dispersing, adding lithium sulfate, performing liquid-phase self-assembly after the lithium sulfate is added, quickly freezing after the self-assembly is finished, and freeze-drying;
step two, vacuum drying is carried out, and constant-temperature calcination is carried out under the protection of inert gas to obtain the graphene-based aerogel;
wherein the mass ratio of the graphene oxide sponge to the acidified carbon nanotube to the lithium sulfate in the first step is (20-60) to (10-40) to (10-30).
2. The preparation method according to claim 1, wherein the mass ratio of the graphene oxide sponge, the acidified carbon nanotubes and the lithium sulfate in the first step is 60: 20.
3. The preparation method according to claim 1, wherein the volume ratio of the total mass of the graphene oxide sponge, the acidified carbon nanotubes and the lithium sulfate to the deionized water in the first step is (0.6-3) g: (10-50) mL.
4. The preparation method according to claim 1, wherein the preparation method of the graphene oxide sponge in the first step is as follows: preparing graphene oxide by using crystalline flake graphite, 98 mass percent of concentrated sulfuric acid, sodium nitrate, potassium permanganate and 30 mass percent of hydrogen peroxide as raw materials through a liquid phase stripping method, centrifugally washing until the pH value of the solution is 7 after the reaction is finished, and freeze-drying at-10 ℃ to obtain the graphene oxide sponge.
5. The method of claim 1, wherein the step of acidifying the carbon nanotubes in the first step is performed by: adding 120mL of concentrated sulfuric acid and 40mL of concentrated nitric acid into 1g of carbon nano tube, magnetically stirring, condensing and refluxing for 3h at 55 ℃, washing with deionized water until the pH value is 7 after the reaction is finished, and freeze-drying to obtain the acidified carbon nano tube.
6. The method according to claim 1, wherein the rapid freezing is performed by using liquid nitrogen in the first step.
7. The method of claim 1, wherein the step one of freeze-drying is performed by the steps of: and (3) putting the frozen solid into a freeze dryer, and continuously freeze-drying for 50-90 h at the vacuum degree of 0.5-10 Pa and the temperature of-10 ℃.
8. The method of claim 1, wherein the vacuum drying in step two is performed by the steps of: taking out the freeze-dried material, placing the material in a vacuum oven, and carrying out constant temperature treatment for 24-48 h at the vacuum degree of 2-10 Pa and the temperature of 60 ℃.
9. The preparation method according to claim 1, wherein the constant-temperature calcination in the second step is performed in a tubular furnace, the protective gas is nitrogen, and the constant-temperature calcination is performed at 100-400 ℃ for 2-4 h.
10. The preparation method according to claim 1, wherein the calcination is carried out at a constant temperature of 400 ℃ for 3 hours in the second step.
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