CN109974317B - Solar energy absorption system with composite absorption mechanism and preparation method thereof - Google Patents
Solar energy absorption system with composite absorption mechanism and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a solar energy absorption system with a composite absorption mechanism and a preparation method thereof, which solve the problem that no absorption material capable of effectively realizing multiple composite absorption mechanisms exists in the prior art. The invention comprises a substrate layer and graphene doped SiO plated on the substrate layer2Sol; the base layer is a stainless steel plate after high-temperature oxidation; the graphene-doped SiO2The raw material composition of the sol comprises: silicate ester, ethanol, acid, deionized water and graphene. The invention combines a plurality of absorption mechanisms such as intrinsic absorption, light trap absorption, amorphous phase carbon defect absorption and the like, has higher selective absorption coefficient and excellent performance.
Description
Technical Field
The invention relates to a solar energy absorption system, in particular to a solar energy absorption system with a composite absorption mechanism and a preparation method thereof.
Background
Solar energy is a clean renewable energy source, has great development potential, and is widely concerned by people in the current society with environmental pollution and resource shortage. As one of the important ways for solar energy utilization, the solar energy heat conversion technology has the advantages of wider available spectrum (300-2500nm), strong applicability, wide working temperature distribution (60-1000 ℃) and the like. However, due to the limitations of high manufacturing cost, high energy consumption, low photo-thermal conversion efficiency, etc., the development of materials with high selective absorption ratio is still a serious challenge in the research field.
The intensity of solar radiation of different wavelengths received by the earth's surface is not uniform and is influenced by many factors, such as season, latitude, terrain, and weather. From the solar radiation intensity distribution curve of fig. 1, we can see that the solar radiation is mainly distributed in the 300-2500nm band, wherein the high radiation region is about 300-800nm band, and when the wavelength exceeds 2500nm, the thermal radiation loss of the material itself is relatively serious, and the energy loss is significant. In view of this objective phenomenon, in order to improve the photothermal conversion efficiency of solar energy, the solar selective absorbing material must have a high absorption rate α (formula 1) in the region of 300-; and a low emissivity in the region of wavelengths greater than 2500nm (equation 2).
Wherein R isλIs the reflectivity of the surface of the material; i issλThe radiation intensity of solar energy at a certain wavelength is shown as AM1.5(ISO, ASTMG179-03) as a standard spectrum; i isBλThe Planckian black body radiation power of an ideal black body substance at a certain wavelength is measured at a certain temperature.
In the prior art, no absorption material capable of effectively realizing a multiple composite absorption mechanism exists, the selectivity coefficient is low, and the solar heat collector can not be effectively applied to various solar heat utilization devices.
Disclosure of Invention
The invention aims to solve the problem that no absorption material capable of effectively realizing multiple composite absorption mechanisms exists in the prior art, and provides a solar energy absorption system with a composite absorption mechanism and a preparation method thereof, wherein the solar energy absorption system has high selectivity coefficient and can be applied to various solar energy heat utilization devices.
The invention is realized by the following technical scheme:
a solar energy absorption system with a composite absorption mechanism comprises a substrate layer and graphene-doped SiO coated on the substrate layer2Sol;
the base layer is a stainless steel plate after high-temperature oxidation;
the graphene-doped SiO2The raw material composition of the sol comprises: silicate ester, ethanol, acid, deionized water and graphene.
The invention plates the SiO doped with graphene on the surface of the stainless steel which is in the sub-wavelength structure after high-temperature oxidation2Sol, the graphene-doped SiO2The sol is made of SiO2As the skeleton of the gel coating, the doped graphene effectively reduces the roughness of the sub-wavelength structure and simultaneously retains the light trap effect and Fe2O3The intrinsic absorption effect of the composite material achieves the effects of improving the absorptivity α of the surface of the material and reducing the emissivity, so that the selectivity coefficient S (S is α /) is remarkably increased, the aim of more efficiently utilizing solar heat is finally achieved, and the composite material has great application potential in the field of solar heat power generation.
The invention combines a plurality of absorption mechanisms such as intrinsic absorption, light trap absorption, amorphous phase carbon defect absorption and the like, has higher selective absorption coefficient and excellent performance.
Further, the graphene-doped SiO is calculated by weight2The raw material composition of the sol comprises:
80-90 parts of silicate with the content of 99.0%, 1270-1350 parts of ethanol with the content of 99.9%, 6-9 parts of hydrochloric acid with the content of 36-38%, 10-15 parts of deionized water, 1-5 parts of graphene and 1-5 parts of a dispersing agent.
Further, the graphene-doped SiO is calculated by weight parts2The raw material composition of the sol comprises:
86 parts of silicate ester with the content of 99.0 percent; 1290 parts of ethanol with the content of 99.9 percent; 7 parts of hydrochloric acid with the content of 36.0-38.0 percent; 2 parts of graphene; and 2 parts of a commercial dispersant.
Further, the substrate layer is in a sub-wavelength structure.
A method of making a solar absorption system having a composite absorption mechanism, comprising:
(1) separately preparing graphene-doped SiO2Sol and a substrate layer;
(2) SiO doping graphene2The sol is plated on the substrate layer;
(3) performing heat treatment under the condition of high-purity nitrogen;
the graphene-doped SiO2The preparation process of the sol comprises the following steps: dispersing silicate ester and graphene in ethanol at the same time, and hydrolyzing and condensing the silicate ester in the ethanol under the catalysis of acid to obtain the graphene/graphene composite material;
the preparation process of the substrate layer comprises the following steps: and (3) treating the stainless steel plate at high temperature, and cleaning and drying to obtain a layered structure with a sub-wavelength structure.
The reaction equation of the hydrolysis condensation in the present invention is as follows:
hydrolysis and condensation: si (OC)2H5)4+4H2O→Si(OH)4+C2H5OH
Si(OH)4→SiO2+2H2O
The invention relates to graphene-doped SiO2In the preparation process of the sol, the reaction condition is mild, the requirements on equipment and experimental conditions are low, the energy consumption is saved, no liquid pollutant is discharged in the whole process, and the method is environment-friendly; the treatment of the substrate material and the preparation process of the coating are simple, the equipment requirement is low, and the harsh experimental conditions such as vacuum and the like do not need to be provided.
Further, the specific preparation method of the invention is as follows:
1. graphene doped SiO2Preparation of the Sol
a) Adding silicate ester, ethanol, hydrochloric acid, deionized water, graphene and a commercial dispersing agent into a reaction bottle according to the measurement, stirring for 2 hours at the temperature of 30 ℃, and then placing the reaction bottle in a constant-temperature water bath for aging for 7 days at the temperature of 25 ℃;
b) the sol comprises the following components in parts by weight: 80-90 parts of silicate with the content of 99.0%, 1270-1350 parts of ethanol with the content of 99.9%, 6-9 parts of hydrochloric acid with the content of 36-38%, 10-15 parts of deionized water, 1-5 parts of graphene (in an oxidized state), and 1-5 parts of commercial dispersant with the same mass as the graphene; as the most preferable of the above components, the components are composed of, in parts by weight: 86 parts of silicate ester with the content of 99.0 percent; 1290 parts of ethanol with the content of 99.9 percent; 7 parts of hydrochloric acid with the content of 36.0-38.0 percent; 2 parts of graphene; and 2 parts of a commercial dispersant.
2. Treatment of stainless steel substrates
a) The substrate is a 4k mirror polished stainless steel plate with the thickness of 1mm, and the material is stainless steel of types 304, 306, 316L and the like;
b) washing the stainless steel sheet with mirror surface polishing with clear water to remove insoluble impurities such as dust on the surface, placing in a sealed container containing acetone, performing ultrasonic treatment in an ultrasonic cleaning tank, taking out, washing with ethanol, and wiping;
c) and (2) placing the cleaned stainless steel sheet in a muffle furnace, treating at the high temperature of 1000 ℃ of 800-.
3. Preparation of a Selective absorbing coating
a) Graphene-doped SiO using dip-lift coater2The sol is plated on the surface of the stainless steel after high-temperature oxidation, the pulling speed is 180-280mm/min, the humidity between the plated films is kept below 30%, the temperature is controlled to be about 30 ℃, and as the most preferable step of the step, the pulling speed is selected to be 250 mm/min;
b) the prepared coating is subjected to heat treatment at the temperature of not more than 450 ℃ in a tube furnace, and the atmosphere in a tube cavity is replaced by high-purity nitrogen in advance to prevent the loss caused by oxidation of the graphene component at high temperature.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. compared with the absorbing material prepared by the similar method, the solar selective absorbing material prepared by the invention combines multiple absorption mechanisms such as intrinsic absorption, light trap absorption, amorphous carbon defect absorption and the like, and has higher selective absorption coefficient and excellent performance.
2. In the preparation process, the reaction condition is mild, the requirements on equipment and experimental conditions are low, the energy consumption is saved, no liquid pollutant is discharged in the whole process, the environment is protected, the preparation process is simple, the equipment requirement is low, and the harsh experimental conditions such as vacuum and the like do not need to be provided;
3. the solar selective absorbing material is suitable for various solar heat conversion devices below 400 ℃.
Drawings
FIG. 1 is a graph of the AM1.5(ISO, ASTMG179-03) solar radiation spectrum.
FIG. 2 is a graph showing the reflectance of the stainless steel substrate of the present invention in the wavelength region of 300-2500 nm.
FIG. 3 is a graph showing the reflectance of the stainless steel substrate of the present invention in a 2.5-25 μm wavelength band.
FIG. 4 is a surface topography of the present invention and a stainless steel substrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1
A preparation method of a solar energy absorption system with a composite absorption mechanism comprises the following specific processes:
uniformly dispersing graphene powder with the same mass into 1270 parts of 99.9% ethanol by using 2 parts of a commercial dispersant BYK-190, adding 80 parts of 99.0% silicate ester, uniformly mixing, adding 8 parts of 36.0-38.0% hydrochloric acid serving as a catalyst, and reacting in a water bath at 30 ℃ for 12 hours for later use. And washing the mirror-polished 316L stainless steel sheet by using clear water, removing insoluble impurities such as dust on the surface, then placing the stainless steel sheet in a sealed container containing acetone, carrying out ultrasonic treatment in an ultrasonic cleaning tank for 30min, taking out the stainless steel sheet, washing the stainless steel sheet by using ethanol, and wiping the stainless steel sheet clean. And (3) placing the cleaned stainless steel sheet in a muffle furnace, treating at the high temperature of 1000 ℃ for 2h, cooling the stainless steel sheet to room temperature along with the furnace after the treatment is finished, taking out the stainless steel sheet, washing with ethanol again to remove the surface, drying at the temperature of 80 ℃, and placing the stainless steel sheet in a dryer for later use. And plating the graphene-doped silica sol on the surface of the stainless steel after high-temperature oxidation by using a dipping-pulling film plating machine, wherein the pulling speed is 200mm/min, the humidity between films is kept below 30%, and the temperature is controlled to be about 30 ℃. The prepared coating is subjected to heat treatment at 400 ℃ in a tube furnace, and the atmosphere in a tube cavity is replaced by high-purity nitrogen in advance to prevent the loss caused by oxidation of the graphene component at high temperature.
Example 2
A preparation method of a solar energy absorption system with a composite absorption mechanism comprises the following specific processes:
uniformly dispersing graphene powder with the same mass in 1290 parts of ethanol with the content of 99.9% by using 2 parts of a commercial dispersant BYK-2012, adding 86 parts of silicate with the content of 99.0%, uniformly mixing, adding 7 parts of 36.0-38.0% hydrochloric acid serving as a catalyst, and reacting in a water bath at 30 ℃ for 12 hours for later use. And (3) washing the 316 stainless steel sheet with the mirror surface polished by clear water to remove insoluble impurities such as dust on the surface, then placing the 316 stainless steel sheet in a sealed container containing acetone, carrying out ultrasonic treatment in an ultrasonic cleaning tank for 30min, taking out the 316 stainless steel sheet, washing the 316 stainless steel sheet by using ethanol and wiping the 316 stainless steel sheet clean. And (3) placing the cleaned stainless steel sheet in a muffle furnace, treating at the high temperature of 900 ℃ for 2h, cooling the stainless steel sheet to room temperature along with the furnace after the treatment is finished, taking out the stainless steel sheet, washing with ethanol again to remove the surface, drying at the temperature of 80 ℃, and placing the stainless steel sheet in a dryer for later use. And plating the graphene-doped silica sol on the surface of the stainless steel after high-temperature oxidation by using a dipping-pulling film plating machine, wherein the pulling speed is 250mm/min, the humidity between films is kept below 30%, and the temperature is controlled to be about 30 ℃. The prepared coating is subjected to heat treatment at 450 ℃ in a tube furnace, and the atmosphere in a tube cavity is replaced by high-purity nitrogen in advance to prevent the loss caused by oxidation of the graphene component at high temperature.
The absorption system prepared in this example was compared with the stainless steel substrate after high temperature treatment disclosed in this example, and the results are shown in fig. 2 to 4.
In FIG. 2, S1Is a reflectivity curve of the stainless steel substrate after high temperature treatment in the wave band of 300-2The reflectivity curve of the absorber system of the invention is in the 300-2500nm wave band; in FIG. 3, S1Is a reflectivity curve of the stainless steel substrate after high-temperature treatment in a wave band of 2.5-25 mu m, S2The absorber system of the invention has a reflectance curve in the 2.5-25 μm band. The absorptivity of the composite absorption system can be calculated to be as high as 0.93 by the curves of fig. 2 and fig. 3 and the formulas shown by combining the formulas 1 and 2, the emissivity at 200 ℃ is as low as 0.205, and the selective absorption coefficient can reach 4.54.
In FIG. 4, a is the surface morphology of the stainless steel substrate after the high temperature treatment, b is the surface morphology of the absorption system of the present invention, and it can be observed from a in FIG. 4 that Fe is generated on the surface of the stainless steel after the high temperature treatment2O3The size of the surface relief of the crystal varies from hundreds of nanometers to one micron, and the crystal plays a role of a 'trap' for light with the wavelength lower than the corresponding width. After the introduction of the coating, the "light trap" structure remains, as shown in fig. 4 b. The coating "backfills" the recessed portions, reducing roughness,the emissivity decreases.
Example 3
A preparation method of a solar energy absorption system with a composite absorption mechanism comprises the following specific processes:
uniformly dispersing graphene powder with the same mass into 1330 parts of 99.9% ethanol by using 2 parts of a commercial dispersant BYK-2012, adding 90 parts of 99.0% silicate ester, uniformly mixing, adding 9 parts of 36.0-38.0% hydrochloric acid serving as a catalyst, and reacting in a water bath at 30 ℃ for 12 hours for later use. And (3) washing the 304 stainless steel sheet with the mirror surface polished by clear water, removing insoluble impurities such as dust on the surface, then placing the steel sheet in a sealed container containing acetone, carrying out ultrasonic treatment in an ultrasonic cleaning tank for 30min, taking out the steel sheet, washing the steel sheet by ethanol, and wiping the steel sheet clean. And (3) placing the cleaned stainless steel sheet in a muffle furnace, treating at the high temperature of 800 ℃ for 2h, cooling the stainless steel sheet to room temperature along with the furnace after the treatment is finished, taking out the stainless steel sheet, washing with ethanol again to remove the surface, drying at the temperature of 80 ℃, and placing the stainless steel sheet in a dryer for later use. And plating the graphene-doped silica sol on the surface of the stainless steel after high-temperature oxidation by using a dipping-pulling film plating machine, wherein the pulling speed is 220mm/min, the humidity between films is kept below 30%, and the temperature is controlled to be about 30 ℃. The prepared coating is subjected to heat treatment at 450 ℃ in a tube furnace, and the atmosphere in a tube cavity is replaced by high-purity nitrogen in advance to prevent the loss caused by oxidation of the graphene component at high temperature.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. The solar energy absorption system with the composite absorption mechanism is characterized by comprising a substrate layer and graphene-doped SiO plated on the substrate layer2Sol;
the substrate layer is a stainless steel plate after high-temperature oxidation, and the substrate layer is of a sub-wavelength structure;
the graphene-doped SiO is calculated by weight2The raw material composition of the sol comprises:
80-90 parts of silicate with the content of 99.0%, 1270-1350 parts of ethanol with the content of 99.9%, 6-9 parts of hydrochloric acid with the content of 36-38%, 10-15 parts of deionized water, 1-5 parts of graphene and 1-5 parts of a dispersing agent.
2. The solar absorption system according to claim 1, wherein the graphene-doped SiO is in a form of a composite absorption mechanism2The raw material composition of the sol comprises:
86 parts of silicate ester with the content of 99.0 percent; 1290 parts of ethanol with the content of 99.9 percent; 7 parts of hydrochloric acid with the content of 36.0-38.0 percent; 2 parts of graphene; and 2 parts of a commercial dispersant.
3. A method for preparing a solar energy absorption system having a composite absorption mechanism, comprising:
(1) separately preparing graphene-doped SiO2Sol and a substrate layer;
(2) SiO doping graphene2The sol is plated on the substrate layer;
(3) performing heat treatment under the condition of high-purity nitrogen;
the graphene-doped SiO2The preparation process of the sol comprises the following steps: dispersing silicate ester and graphene in ethanol at the same time, and hydrolyzing and condensing the silicate ester in the ethanol under the catalysis of acid to obtain the graphene/graphene composite material;
the preparation process of the substrate layer comprises the following steps: and (3) treating the stainless steel plate at high temperature, and cleaning and drying to obtain a layered structure with a sub-wavelength structure.
4. The method of claim 3, wherein the graphene-doped SiO is applied by dip-coating and dip-coating2Sol-plated stainless steel plate after high-temperature oxidationAnd on the surface, the pulling speed is 180-280mm/min, and the humidity between the coating films is kept below 30%.
5. The method of claim 3, wherein the heat treatment temperature is less than 450 ℃.
6. The method for preparing the solar energy absorption system with the composite absorption mechanism according to claim 3, wherein the treatment temperature of the high-temperature treatment in the preparation process of the substrate layer is 800-1000 ℃.
7. The method for preparing a solar absorption system with a composite absorption mechanism as claimed in claim 3, wherein the graphene-doped SiO is2The preparation process of the sol comprises the following steps:
adding silicate ester, ethanol, hydrochloric acid, deionized water, graphene and a dispersing agent into a reaction bottle according to the measurement, stirring for 1.5-2.5 h at the temperature of 28-32 ℃, placing the mixture in a constant-temperature water bath, and aging to obtain the graphene-doped SiO2Sol;
the concrete metering of the components is as follows according to parts by weight:
80-90 parts of silicate with the content of 99.0%, 1270-1350 parts of ethanol with the content of 99.9%, 6-9 parts of hydrochloric acid with the content of 36-38%, 10-15 parts of deionized water, 1-5 parts of graphene and 1-5 parts of a dispersing agent.
8. The method for preparing a solar energy absorption system with a composite absorption mechanism according to claim 7, wherein the graphene is graphene in an oxidized state.
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| KR101097175B1 (en) * | 2010-07-09 | 2011-12-22 | 아주대학교산학협력단 | Saturable absorber comprising monolayer graphene and manufacturing method of the same |
| CN102798241A (en) * | 2012-08-31 | 2012-11-28 | 山东力诺新材料有限公司 | Solar selective absorption coating and preparation technology thereof |
| CN105498649B (en) * | 2015-12-24 | 2017-12-26 | 四川大学 | Graphene nano particle composite aerogel microballoon and preparation method thereof |
| CN109423068A (en) * | 2017-06-23 | 2019-03-05 | 北京国信优控系统技术有限公司 | Super-hydrophobic wear-resisting graphene composite coating and the solar energy heat collection pipe for applying it |
| CN109373618A (en) * | 2018-08-30 | 2019-02-22 | 江苏京展能源科技有限公司 | A kind of preparation method of selective solar composite coating for absorbing |
| CN109206017B (en) * | 2018-11-23 | 2022-03-25 | 天津市职业大学 | Graphene-doped glass coating liquid and preparation method thereof |
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