CN111397231A - Graphene-based selective absorption film system and preparation method of absorption layer thereof - Google Patents
Graphene-based selective absorption film system and preparation method of absorption layer thereof Download PDFInfo
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Abstract
The invention discloses a graphene-based selective absorption film system and a preparation method of an absorption layer thereof. The preparation method of the graphene absorption layer in the film system is mixed solution coating, and comprises the following steps: oxidizing and stripping graphite powder to obtain a graphene oxide aqueous solution; mixing the graphene oxide aqueous solution with the low surface tension solution to obtain a mixed solution; coating the mixed solution on the surface of the infrared reflection layer so as to obtain a graphene oxide absorption layer; and carrying out reduction treatment on the graphene oxide absorption layer so as to obtain the graphene absorption layer. The graphene absorption layer has excellent refractive index and extinction coefficient, so that the excellent spectral selectivity of the graphene-based selective absorption film system is ensured, and the photo-thermal utilization efficiency of the selective absorption surface is improved. Meanwhile, the optical band gap of the film system can be adjusted by changing the thickness of the graphene layer, and the graphene-based selective absorption film system also has long-time stability at high temperature matched with the available optical band gap, and can be widely applied to solar energy utilization systems from low temperature to high temperature.
Description
Technical Field
The invention belongs to the technical field of preparation of solar selective absorption films, and particularly relates to a solar selective absorption film system using a graphene-based material as an absorption layer, and a solution coating preparation method of the graphene absorption layer.
Background
The solar selective absorption film as an efficient solar photo-thermal conversion device has high sunlight absorptivity and very low thermal radiation emissivity, and has mature and wide commercial application in the field of solar hot water. To date, a number of selective absorber film systems have been introduced into the consumer market, such as black chromium, AlNiOX, AlN/Al, etc. Most of the commercial selective absorption films with excellent performance have the solar light absorptivity of more than 0.9, the thermal radiation emissivity of less than 0.05 and the long-time stability under the medium and low temperature use condition of less than 400 ℃. However, in recent years, many solar photo-thermal conversion application fields, such as concentrated photo-thermal photovoltaic, concentrated thermoelectric, photo-thermal high-temperature steam and the like, emerge, and higher requirements are put on the high-temperature service performance of the selective absorption film at the temperature of more than 600 ℃.
The carbon-based material generally has strong light absorption performance and high temperature stability, and has a good application prospect in a high-temperature selective absorption film system. However, the research on the shape control of the sub-wavelength interference structure of the carbon material is still incomplete, and the research on the development of selective absorption membranes mainly based on the carbon material has been limited to some extent. The graphene material serving as a typical novel carbon-based material has multi-scale assembly adjustable performance, and a selective absorption film system prepared based on the graphene material is expected to solve the problem of long-term use stability at high temperature, but the work of the aspect is still to be developed.
Disclosure of Invention
The invention aims to provide a graphene-based solar selective absorption film system and a preparation method of an absorption layer thereof, the film system has excellent high-temperature long-time tolerance and optical band gap regulation and control performance matched with the temperature tolerance, and meanwhile, the preparation method of the absorption layer has the characteristics of simple process, environmental protection and large-scale preparation.
In a first aspect of the present invention, the technical solution adopted to solve the technical problem is as follows:
a graphene-based selective absorption film system comprises a substrate layer, an infrared reflection layer, an absorption layer, and an anti-reflection layer (as shown in FIG. 1).
The antireflection layer is one or more of silicon dioxide, aluminum oxide, hafnium oxide and aluminum nitride, and the thickness of the antireflection layer is 20-300 nm.
The absorption layer is a graphene absorption layer and is composed of graphene or graphene-based composite materials, the thickness of the absorption layer is 10-500 nm, and the preferred range of the absorption layer is 30-150 nm. Further, the graphene absorption layer contains at least one of reduced graphene oxide, graphene oxide and graphene materials.
The infrared reflecting layer is formed by one of metal films of Al, W, Fe, Cu, Mo, Au and Ag, and the thickness of the infrared reflecting layer is more than 70 nm.
The substrate layer is made of any material which is in contact with the infrared reflecting layer, and the thickness is not limited.
In a second aspect of the present invention, the present invention provides a method for preparing an absorption layer in a graphene-based selective absorption film, comprising the following steps:
s1, oxidizing and stripping graphite powder to obtain a graphene oxide aqueous solution;
s2, mixing the graphene oxide aqueous solution with the low surface tension solution to obtain a mixed solution which is easy to coat and form a film;
s3, coating the mixed solution on the surface of the infrared reflection layer to obtain a graphene oxide absorption layer;
and S4, carrying out reduction treatment on the graphene oxide absorption layer to obtain the graphene absorption layer.
Further, the low surface tension solution in step S2 is at least one of ethanol, acetone, isopropanol, and ethylene glycol;
further, the coating method in the step S3 adopts at least one of spin coating, blade coating, pulling, spray coating, dipping, and stamping.
Further, the reduction treatment in step S4 is performed by one of a reducing agent fumigation method and a high-temperature heat treatment method.
The invention has the beneficial effects that:
(1) due to the fact that the graphene thin layer with the optimal thickness is used as the absorption layer, excellent spectrum selectivity is obtained, the sunlight absorption rate can be larger than 0.92, and the infrared reflectivity is as low as 0.04;
(2) the graphene-based selective absorption film is subjected to heat treatment at 800 ℃ for 96 hours in an argon atmosphere, has no obvious deterioration of spectral selectivity, and has good high-temperature stability;
(3) by changing the thickness of the graphene absorption layer, the optical band gap of the film system is adjustable within the range of 1.1-3.2 mu m, and the combination of the high-temperature stability shows that the film system has the prospect of covering various solar energy utilization fields from low temperature to high temperature;
(4) the graphene absorption layer prepared by the solution coating method has the advantages of simple process, environmental protection and large-scale preparation.
The foregoing and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, and may be embodied in the form of the following description.
Drawings
FIG. 1 is a schematic structural diagram of a graphene-based selective absorption membrane system;
wherein, 1 is a substrate layer, 2 is an infrared reflecting layer, and 3 is a graphene absorption layer; and 4, an antireflection layer.
FIG. 2 is a radiation absorption spectrum according to example 1 of the present invention;
FIG. 3 is a radiation absorption spectrum according to example 2 of the present invention;
FIG. 4 is a radiation absorption spectrum according to example 3 of the present invention;
FIG. 5 is a comparative spectrum of absorption of radiation before and after heat treatment at 800 ℃ for 96 hours in an argon atmosphere according to example 4 of the present invention.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
In a first aspect of the present invention, the present invention provides a graphene-based selective absorption membrane system. As shown in fig. 1, the infrared absorption film consists of a substrate layer, an infrared reflecting layer, an absorption layer and an antireflection layer.
The specific implementation process is as follows:
(1) preparing a base layer and an infrared reflecting layer: in some embodiments of the present invention, the polished metal sheet is selected to serve as both the base layer and the IR reflecting layer, and the top surface of the metal sheet is polished to a roughness below 10 nm. It is noted that the base layer need not be the same as the infrared reflecting layer, but may be any material. Meanwhile, the polishing of the upper surface of the metal sheet is to satisfy the spectrum function of the infrared reflecting layer, and the thickness of the infrared reflecting layer is ensured to be more than 70 nm.
(2) Pretreatment of the surface of the infrared reflection layer: removing attached impurities on the surface of the polished metal sheet, respectively ultrasonically cleaning the polished metal sheet in acetone and ethanol for 15-30 minutes, and carrying out nitrogen purging and vacuum storage;
(3) preparation of the absorbing layer: preparing a graphene absorption layer on the surface of the pretreated metal sheet through the processes of drying after solution coating, vacuum sputtering coating, chemical vapor deposition, friction stir welding, powder sintering and the like, wherein the thickness of the graphene absorption layer is within the range of 10-500 nm, and the roughness of the graphene absorption layer is in the same order of magnitude as that of the surface of the polished metal sheet. The graphene absorption layer contains at least one of graphene oxide, reduced graphene oxide and graphene.
(4) Preparing an antireflection layer: and depositing a low-refractive-index interference thin layer on the surface of the graphene absorption layer by processes such as a sol-gel method, vacuum sputtering coating, chemical vapor deposition and the like. The material of the antireflection layer can be one or more of silicon dioxide, aluminum oxide, hafnium oxide and aluminum nitride, and the thickness of the antireflection layer is 20-300 nm
In a second aspect of the present invention, the present invention provides a method for preparing an absorption layer in a graphene-based selective absorption film. The preparation method comprises oxidation stripping treatment, mixing treatment, solution coating treatment and reduction treatment. The method comprises the following specific steps:
s1: oxidative stripping treatment
In some embodiments of the invention, a Hummers method can be adopted to prepare the graphene oxide aqueous solution from graphite powder, specifically, 9g of graphite powder, 9g of sodium nitrate and 240m L concentrated sulfuric acid (98 wt%) are uniformly mixed, 24g of potassium permanganate is added under the condition of ice-bath stirring, the temperature is raised to 35 ℃, the stirring is carried out for 2 hours, deionized water with the volume of 400m L is slowly added, the temperature is raised to 90 ℃, the stirring is carried out for 0.5 hour, then deionized water with the volume of 1000m L is added, the stirring is uniformly carried out, the mixture is cooled to the room temperature, 60m L hydrogen peroxide (30 wt%) is added, the filtration is carried out, and the centrifugal washing is carried out to obtain the graphene oxide aqueous solution.
According to the embodiment of the present invention, the concentration of the graphene oxide aqueous solution prepared by the oxidation exfoliation treatment is not particularly limited, and may be selected by those skilled in the art according to actual needs, and according to the embodiment of the present invention, the concentration of the graphene oxide aqueous solution prepared may be 2 to 15mg · m L-1。
S2: mixing treatment
In this step, a graphene oxide aqueous solution is mixed with a low surface tension solvent to obtain a mixed solution.
According to an embodiment of the present invention, the low surface tension solvent may be at least one selected from ethanol, acetone, isopropanol, and ethylene glycol.
According to the specific embodiment of the invention, the volume ratio of the low surface tension solvent to the graphene oxide aqueous solution can be (1-100): 1. no low surface tension solvent is used or the volume ratio is lower than (1-100): 1, the obtained solution does not have good coating performance, and a flat and ultrathin graphene oxide thin layer is not easy to prepare. The volume ratio is large (1-100): 1, the efficiency of preparing the graphene oxide thin layer is greatly reduced.
S3: solution coating process
In the step, the mixed solution is coated by a solution and then dried to deposit a graphene oxide absorption layer which is uniform and flat and has a thickness of submicron level on the surface of the infrared reflection layer. The solution coating method may employ at least one of spin coating, doctor coating, drawing, spray coating, dipping, and embossing. According to the graphene oxide concentration of the mixed solution and the expected coating thickness, proper coating processes and detailed parameters such as coating speed, drying temperature, coating repetition times and the like are automatically determined so as to ensure sufficient uniform flatness and accurate graphene oxide layer thickness.
S4: reduction treatment
In the step, the graphene oxide absorption layer is subjected to reduction treatment, so that the graphene absorption layer with excellent selective spectral performance is obtained. The extinction coefficient of unreduced graphene oxide is about 0.02 and is obviously lower than that of reduced graphene (0.25-1.5), and the too low extinction coefficient causes that the graphene oxide absorption layer is not fully dissipated and absorbed in a light interference period and then is reflected back to the surrounding environment. According to an embodiment of the present invention, the reduction treatment may be one of a reducing agent fumigation method and a high temperature heat treatment method.
According to an embodiment of the present invention, the above-mentioned method for fumigating and reducing reagent comprises: heating hydrazine hydrate, hydroiodic acid or vitamin C solution to 80-95 ℃ so as to obtain reducing steam, and fumigating the sample coated with the graphene oxide absorption layer for 1-3 h by using the reducing steam.
According to an embodiment of the present invention, the high-temperature heating reduction method includes: and annealing the sample coated with the graphene oxide absorption layer for 1-3 h at 200-1000 ℃ in an inert gas (nitrogen or argon) atmosphere.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
The overall scheme and steps of example 1 are the same as those of the above specific implementation process, and are described in more detail as follows:
1. adopting a polished metal Al sheet as a substrate and an infrared reflecting layer at the same time;
2. preparing an antireflection layer by adopting a sol-gel method, wherein the selected material is silicon dioxide nano sol;
3. the graphene absorption layer is prepared by a method of drying after solution coating, and the method further comprises the following steps:
3.1 concentration of the aqueous solution of graphene oxide obtained in step S1 was 10 mg. m L-1；
3.2 in step S2, selecting a low-surfactant solution as ethanol, wherein the volume ratio of the ethanol to the graphene oxide aqueous solution is 10: 1;
3.3 the coating method adopted in the step S3 is spin coating, the rotating speed is 2000-6000 rpm, and the coating times are 50-1000;
3.4 the reduction treatment method adopted in step S4 is high-temperature heat treatment, and the sample covered with the graphene oxide absorption layer is annealed at 300 ℃ for 1h in an argon atmosphere. The thickness of the obtained graphene absorption layer is 50 nm;
4. and performing spectral selectivity measurement on the prepared graphene-based selective absorption film, wherein the sunlight absorption rate is measured and recorded by a UV-NIR spectrophotometer, and the thermal radiation emissivity is measured and recorded by a thermal imaging emissivity correction method under black body reference. The obtained graphene-based selective absorption film had a solar light absorption rate of 0.87 (fig. 2) and a thermal radiation emissivity of 0.03.
Example 2
Example 2 is essentially the same as example 1, except that the resulting graphene absorber layer is thick.
1. Adopting a polished metal Al sheet as a substrate and an infrared reflecting layer at the same time;
2. preparing an antireflection layer by adopting a sol-gel method, wherein the selected material is silicon dioxide nano sol;
3. the graphene absorption layer is prepared by a method of drying after solution coating, and the method further comprises the following steps:
3.1 concentration of the aqueous solution of graphene oxide obtained in step S1 was 10 mg. m L-1；
3.2 in step S2, selecting a low-surfactant solution as ethanol, wherein the volume ratio of the ethanol to the graphene oxide aqueous solution is 10: 1;
3.3 the coating method adopted in the step S3 is spin coating, the rotating speed is 2000-6000 rpm, and the coating times are 50-1000;
3.4 the reduction treatment method adopted in step S4 is high-temperature heat treatment, and the sample covered with the graphene oxide absorption layer is annealed at 300 ℃ for 1h in an argon atmosphere. The thickness of the obtained graphene absorption layer is 100 nm;
4. and performing spectral selectivity measurement on the prepared graphene-based selective absorption film, wherein the sunlight absorption rate is measured and recorded by a UV-NIR spectrophotometer, and the thermal radiation emissivity is measured and recorded by a thermal imaging emissivity correction method under black body reference. The solar light absorption rate of the obtained graphene-based selective absorption film was 0.92 (fig. 3), and the thermal radiation emissivity was 0.04.
Example 3
Example 3 is essentially the same as example 1, except that the resulting graphene absorber layer is thick.
1. Adopting a polished metal Al sheet as a substrate and an infrared reflecting layer at the same time;
2. preparing an antireflection layer by adopting a sol-gel method, wherein the selected material is silicon dioxide nano sol;
3. the graphene absorption layer is prepared by a method of drying after solution coating, and the method further comprises the following steps:
3.1 concentration of the aqueous solution of graphene oxide obtained in step S1 was 10 mg. m L-1；
3.2 in step S2, selecting a low-surfactant solution as ethanol, wherein the volume ratio of the ethanol to the graphene oxide aqueous solution is 10: 1;
3.3 the coating method adopted in the step S3 is spin coating, the rotating speed is 2000-6000 rpm, and the coating times are 50-1000;
3.4 the reduction treatment method adopted in step S4 is high-temperature heat treatment, and the sample covered with the graphene oxide absorption layer is annealed at 300 ℃ for 1h in an argon atmosphere. The thickness of the obtained graphene absorption layer is 150 nm;
4. and performing spectral selectivity measurement on the prepared graphene-based selective absorption film, wherein the sunlight absorption rate is measured and recorded by a UV-NIR spectrophotometer, and the thermal radiation emissivity is measured and recorded by a thermal imaging emissivity correction method under black body reference. The solar light absorption rate of the obtained graphene-based selective absorption film was 0.89 (fig. 4), and the thermal radiation emissivity was 0.06.
Example 4
Example 4 is essentially the same as example 1, except for the polished metal sheet used, the thickness of the resulting graphene absorber layer, and the high temperature heat treatment process.
1. Adopting a polished metal W sheet as a substrate and an infrared reflecting layer at the same time;
2. preparing an antireflection layer by adopting a sol-gel method, wherein the selected material is silicon dioxide nano sol;
3. the graphene absorption layer is prepared by a method of drying after solution coating, and the method further comprises the following steps:
3.1 concentration of the aqueous solution of graphene oxide obtained in step S1 was 10 mg. m L-1；
3.2 in step S2, selecting a low-surfactant solution as ethanol, wherein the volume ratio of the ethanol to the graphene oxide aqueous solution is 10: 1;
3.3 the coating method adopted in the step S3 is spin coating, the rotating speed is 2000-6000 rpm, and the coating times are 50-1000;
3.4 the reduction treatment method adopted in step S4 is high-temperature heat treatment, and the sample covered with the graphene oxide absorption layer is annealed at 800 ℃ for 2h in an argon atmosphere. The thickness of the obtained graphene absorption layer is 120 nm;
4. and performing spectral selectivity measurement on the prepared graphene-based selective absorption film, wherein the sunlight absorption rate is measured and recorded by a UV-NIR spectrophotometer, and the thermal radiation emissivity is measured and recorded by a thermal imaging emissivity correction method under black body reference. The solar light absorptivity of the obtained graphene-based selective absorption film is 0.94 (figure 5), and the thermal radiation emissivity is 0.05;
5. the graphene-based selective absorption film is subjected to heat treatment at 800 ℃ for 96 hours in an argon atmosphere, and then spectral selectivity measurement is carried out, as shown in fig. 5, the solar light absorption rate is 0.92, and the thermal radiation emissivity is 0.13. The optimal value of visible spectrum selectivity PC is 0.04, and the use requirement is still met, which shows that the graphene-based selective absorption film has the long-time use performance of 800 ℃.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and those skilled in the art can make changes, modifications, substitutions and alterations to the above embodiments within the scope of the present invention and still cover the scope of the present invention.
Claims (10)
1. The graphene-based selective absorption film system is characterized by sequentially comprising an antireflection layer (4), an absorption layer (3), an infrared reflection layer (2) and a substrate layer (1) from top to bottom, wherein the absorption layer (3) is a graphene absorption layer and is composed of graphene or a graphene-based composite material.
2. The graphene-based selective absorption membrane system according to claim 1, wherein the graphene absorption layer (3) contains at least one of reduced graphene oxide, and graphene material.
3. The graphene-based selective absorption membrane system according to claim 1, wherein the thickness of the graphene absorption layer (3) is 10-500 nm, and the preferred range is 30-150 nm.
4. The graphene-based selective absorption film system according to claim 1, wherein the anti-reflection layer (4) is one or more of silicon dioxide, aluminum oxide, hafnium oxide and aluminum nitride.
5. The graphene-based selective absorption membrane system according to claim 1, wherein the infrared reflection layer (2) is composed of one of Al, W, Fe, Cu, Mo, Au, Ag metal films.
6. The graphene-based selective absorption membrane system according to claim 1, wherein the base layer (1) is made of the same material as the infrared reflection layer (2);
optionally, the material of the base layer (1) is different from the material of the infrared reflecting layer (2).
7. The method for preparing an absorption layer in a graphene-based selective absorption membrane according to any one of claims 1 to 6, comprising the steps of:
s1, oxidizing and stripping graphite powder to obtain a graphene oxide aqueous solution;
s2, mixing the graphene oxide aqueous solution with the low surface tension solution to obtain a mixed solution which is easy to coat and form a film;
s3, coating the mixed solution on the surface of the infrared reflection layer to obtain a graphene oxide absorption layer;
and S4, carrying out reduction treatment on the graphene oxide absorption layer to obtain the graphene absorption layer.
8. The method according to claim 7, wherein the low surface tension solution in step S2 is at least one of ethanol, acetone, isopropanol, and ethylene glycol.
9. The method according to claim 7, wherein the coating method in step S3 is at least one of spin coating, blade coating, drawing, spray coating, dipping, and stamping.
10. The method according to claim 7, wherein the reduction treatment in step S4 is one of a reducing agent fumigation method and a high-temperature heat treatment method.
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Application publication date: 20200710 |