CN114322339A - Solar selective absorption Ni @ SiO2Preparation method and application of nano-microspheres - Google Patents
Solar selective absorption Ni @ SiO2Preparation method and application of nano-microspheres Download PDFInfo
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- JVYLIMILBNDJRH-UHFFFAOYSA-L dichloronickel;tetrahydrate Chemical compound O.O.O.O.Cl[Ni]Cl JVYLIMILBNDJRH-UHFFFAOYSA-L 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- 239000012280 lithium aluminium hydride Substances 0.000 claims description 3
- -1 lithium aluminum hydride Chemical compound 0.000 claims description 3
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 3
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
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- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 claims description 2
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
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- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/40—Solar thermal energy, e.g. solar towers
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Abstract
The invention relates to solar selective absorption Ni @ SiO2A preparation method and application of nano-microspheres, belonging to the technical field of optical materials. Firstly, Ni nano-particles are prepared by using reduction reaction and corresponding ligands, and then Ni @ SiO is prepared by using a sol-gel method2Solar selective absorption nano-microspheres. The method can prepare the thermally stable powder selectively absorbed by solar energy, has high solar energy absorptivity (about 0.913) and low thermal emissivity (about 0.085), is excellent powder selectively absorbed by solar energy, and has great application potential in the field of high-temperature solar photothermal conversion.
Description
Technical Field
The invention relates to solar selective absorption Ni @ SiO2A preparation method and application of nano-microspheres, belonging to the technical field of optical materials.
Background
The sunlight transmits energy to the earth through electromagnetic radiation, wherein about 99.9 percent of the energy is concentrated in the 300-2500nm band, namely the ultraviolet-visible-near infrared region, and the improvement of the electromagnetic absorption of the 300-2500nm band is very important. Objects above absolute zero radiate energy outwards, thus requiring materials with low emissivity in the mid and far infrared regions. The solar selective absorption coating is a coating with high absorptivity in an ultraviolet-visible-near infrared region and low emissivity in a middle-far infrared region, and is widely applied to the field of solar photothermal conversion. The solar selective absorbing coating prepared by the coating method has the advantages of large production scale, high production cost performance and the like, and is suitable for industrial production.
The traditional metal ceramic solar selective absorption powder has poor thermal stability in a high-temperature environment, and long-term high-temperature environment can cause metal nanoparticles to diffuse to cause particle sintering and metal on a substrate to migrate to functional powder to form binary or ternary metal oxide in an absorption layer. This results in the poor absorption and utilization effect of the coating on solar energy, and therefore, it is very important for the solar energy selective absorption powder to improve the thermal stability of the solar energy selective absorption powder and to improve the absorptivity of the ultraviolet-visible-near infrared band and to reduce the emissivity of the mid-infrared band.
Disclosure of Invention
The invention aims to overcome the defects and provide the solar selective absorption Ni @ SiO2The nano-microsphere can effectively inhibit Ni nano-particles from sintering and avoid forming binary or multi-element oxides in an absorption layer, and is excellent solar selective powder.
The technical scheme of the invention is that the solar selective absorption Ni @ SiO2The preparation method of the nano-microsphere comprises the steps of firstly preparing Ni nano-particles by utilizing a reduction reaction and corresponding ligands, then dissolving the obtained Ni nano-particles in polyvinylpyrrolidone PVP for surface modification, and adding SiO into the PVP2Precursor and ethylenediamine, and Ni @ SiO is prepared by adopting a sol-gel method2Solar selective absorption nano-microspheres.
Further, the steps are as follows:
(1) preparing Ni nano microspheres: firstly, uniformly stirring a dispersing agent, Ni salt and deionized water in a reaction container, then introducing nitrogen to remove oxygen in a system, adding a reducing agent under the protection of the nitrogen, carrying out reduction reaction, and separating and drying by using a centrifugal machine to obtain Ni nano particles;
(2)Ni@SiO2synthesizing the solar selective absorption nano microspheres: dissolving the Ni nano particles prepared in the step (1) in polyvinylpyrrolidone PVP for surface modification, and then centrifuging; dispersing the modified Ni nano-particles in deionized water, and adding SiO into the deionized water2The precursor and ethylenediamine react under the action of ultrasound and then are centrifuged; washing to obtain Ni @ SiO2Solar selective absorption nano-microspheres.
Further, the dispersant is one or more of sodium dodecyl sulfate, oleic acid, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate;
the reducing agent is specifically sodium borohydride, potassium borohydride or lithium aluminum hydride.
The Ni salt is specifically nickel nitrate hexahydrate, nickel sulfate hexahydrate, nickel chloride tetrahydrate or nickel acetate tetrahydrate.
Further, the SiO2The precursor is tetraethyl silicate and/or tetramethoxysilane and propyl orthosilicate.
Further, the step (1) is specifically as follows: boiling deionized water, and deoxidizing for later use; respectively pre-dispersing 25-30g of dispersing agent and 2.9-3g of Ni salt into 10mL of deionized water, then adding the uniformly dispersed dispersing agent and Ni salt into a reaction container containing 80mL of deionized water, and uniformly stirring at 300-400rpm magnetic force; introducing nitrogen to remove oxygen in the system, adding 29-30mg of reducing agent under the protection of nitrogen, reacting for 1-1.5h at 5-20 ℃, stopping the reaction, then performing deionization washing and centrifugation for a plurality of times, and drying for 22-26h at 40-50 ℃ in a vacuum oven under 0.08-0.1MPa to obtain the Ni nano particles.
Further, the step (2) is specifically as follows: 5 to 7g of polyvinylpyrrolidone, 100mL of deionized water and 0.9 to 1g of the stepMixing the Ni nanoparticles prepared in the step (1), magnetically stirring for 25-30min, and then centrifuging to disperse the Ni nanoparticles into 11-13mL of ethanol; 2-2.5mL of ethylenediamine and 0.55-0.56mL of SiO were added2Stirring and reacting the precursor for 70-80min at 300-400rpm magnetic stirring, and keeping the temperature at 5-20 ℃; finally, the Ni @ SiO is prepared by a plurality of times of deionization washing and centrifugation2Solar selective absorption nano-microspheres.
Further, the Ni @ SiO2The solar selective absorption nano-microspheres are dispersed in the dispersion liquid for storage.
Further, the Ni @ SiO2Dispersing the solar selective absorption nano microspheres in an ethanol solution for storage; the ethanol solution is absolute ethanol; when dispersing, the volume ratio of the microspheres to the ethanol solution is 1: 4-5.
Solar energy selective absorption Ni @ SiO prepared by the method2The application of the nano-microspheres is applied to a solar absorber.
Further, adding Ni @ SiO2The solar selective absorption nano microsphere dispersion liquid is used as a raw material, and is dried to form a film on a carrier at the temperature of 60-70 ℃ at the pulling speed of 2-3mm/s by a dip coating method to prepare the solar absorber.
Further, the dried film is subjected to annealing treatment by heat preservation for 3-3.5h at the heating rate of 10 ℃/min and 700 ℃ under the nitrogen atmosphere.
Further, the thickness of the film is 0.2 to 0.3mm when the film is formed.
Further, adding Ni @ SiO2The solar selective absorption nano microsphere dispersion liquid is used as an additive to be added into the coating, the addition amount is 30-40% of the mass of the coating, and a tape casting film forming method or other conventional film forming methods can be adopted.
The invention has the beneficial effects that: the method can prepare the powder with high solar energy selective absorption, the powder has high solar energy absorption rate (about 0.913) and low thermal emissivity (about 0.085), is excellent powder with solar energy selective absorption, and has great application potential in the field of solar energy photo-thermal conversion.
Drawings
FIG. 1 is Ni @, prepared in example 1SiO2TEM image of solar selective absorption nanospheres.
Fig. 2 is a schematic diagram of the change of the absorption rate of the coating AM1.5 with different Ni particle sizes prepared in example 1.
FIG. 3 is a graph showing the reflectance of a coating with a Ni particle size of 40nm and the change in reflectance of the coating after heat treatment at 700 ℃ for 24 hours.
Detailed Description
Example 1
(1) Preparing Ni nano microspheres: boiling deionized water to remove oxygen for later use; to 80mL of water were added 10mL of sodium dodecyl sulfate (27.2g of an aqueous solution of sodium dodecyl sulfate), 1mL of oleic acid, and 10mL of Ni (NO)3)2·6H2O (2.9g of an aqueous solution prepared from nickel nitrate hexahydrate). After vigorously stirring at room temperature, 30mg of NaBH was added to the solution4. Controlling the reaction temperature to be 20 ℃, reacting for 1h, then carrying out deionization washing and centrifugation for a plurality of times, and drying for 24h at 40 ℃ under 0.08MPa in a vacuum oven to obtain the 40nm Ni nano particles.
The nickel nano particles with different sizes are influenced by temperature, can synthesize the nickel nano particles with about 40nm size at 20 ℃, can synthesize the nickel nano particles with about 60nm size at about 14 ℃, and can synthesize the nickel nano particles with about 80nm size at 5 ℃; the size of the synthesized nickel nanoparticles tends to increase as the temperature becomes lower.
(2)SiO2Synthesis of the Ni-coated microspheres: 6g of polyvinylpyrrolidone, 100mL of deionized water and 1g of Ni nanoparticles prepared in step (1) were mixed and magnetically stirred for 30 minutes, and then centrifugally dispersed in 12mL of ethanol. 2.2mL of Diethylamine (DEA) and 0.56mL of tetraethyl orthosilicate (TEOS) were rapidly added to the ethanol mixture containing nickel nanoparticles, and the nickel nanoparticles were coated under the action of ultrasound. Reacting for 70min to obtain nickel nano particles coated by silicon dioxide, and then centrifuging and washing by deionized water to obtain solar selective absorption Ni @ SiO2Nano-microspheres; dispersing the product in absolute ethyl alcohol, wherein the volume ratio of the microspheres to the ethyl alcohol solution is 1: 4-5 to obtain Ni @ SiO2Nano microsphere sol dispersion.
Ni @ SiO prepared from 40nm Ni nano microspheres2The TEM morphology of the solar selective absorption nanospheres is shown in fig. 1. Although there is a small amount of free SiO2It can be seen that mainly Ni @ SiO is also introduced2The microsphere, the obvious core-shell structure of which can be seen from fig. 1, confirms the formation of the silica-coated nickel nanoparticle structure.
Example 2
(1) Preparing Ni nano microspheres: boiling deionized water, and deoxidizing for later use; respectively pre-dispersing 30g of dispersing agent and 2.9g of Ni salt into 10mL of deionized water, then adding the uniformly dispersed dispersing agent and Ni salt into a reaction vessel containing 80mL of deionized water, and magnetically stirring uniformly at 300 rpm; introducing nitrogen to remove oxygen in the system, adding 30mg of reducing agent under the protection of nitrogen, reacting for 1h at 20 ℃, stopping the reaction, then performing deionization washing and centrifugation for a plurality of times, and drying for 22h at 50 ℃ under 0.08MPa in a vacuum oven to obtain the Ni nano particles.
The dispersant is specifically sodium dodecyl sulfate; the reducing agent is specifically sodium borohydride; the Ni salt is nickel sulfate hexahydrate; the SiO2The precursor is tetraethyl silicate.
(2)Ni@SiO2Synthesizing the solar selective absorption nano microspheres: mixing 7g of polyvinylpyrrolidone, 100mL of deionized water and 0.9g of Ni nanoparticles prepared in the step (1), magnetically stirring for 30min, and then centrifuging to disperse the Ni nanoparticles into 11mL of ethanol; 2.5mL of ethylenediamine and 0.55mL of SiO were added2Magnetically stirring and stirring the precursor at 400rpm for reaction for 70min, and keeping the temperature at 20 ℃; finally, the Ni @ SiO is prepared by a plurality of times of deionization washing and centrifugation2Solar selective absorption nano-microspheres.
Example 3
(1) Preparing Ni nano microspheres: boiling deionized water, and deoxidizing for later use; respectively pre-dispersing 28g of dispersing agent and 2.9g of Ni salt into 10mL of deionized water, then adding the uniformly dispersed dispersing agent and Ni salt into a reaction vessel containing 80mL of deionized water, and magnetically stirring uniformly at 350 rpm; introducing nitrogen to remove oxygen in the system, adding 30mg of reducing agent under the protection of nitrogen, reacting for 1.5h at 20 ℃, stopping the reaction, then performing deionization washing and centrifugation for several times, and drying for 22h at 45 ℃ in a vacuum oven under 0.1MPa to obtain the Ni nano particles.
(2)Ni@SiO2Synthesizing the solar selective absorption nano microspheres: mixing 6g of polyvinylpyrrolidone, 100mL of deionized water and 0.9g of Ni nanoparticles prepared in the step (1), magnetically stirring for 28min, and then centrifuging to disperse the Ni nanoparticles into 11mL of ethanol; 2.5mL of ethylenediamine and 0.56mL of SiO were added2Magnetically stirring and stirring the precursor at 350rpm for reacting for 75min, and keeping the temperature at 20 ℃; finally, the Ni @ SiO is prepared by a plurality of times of deionization washing and centrifugation2Solar selective absorption nano-microspheres.
The dispersant is sodium dodecyl benzene sulfonate; the reducing agent is lithium aluminum hydride; the Ni salt is nickel chloride tetrahydrate; the SiO2The precursor is propyl orthosilicate.
Application example 1Ni @ SiO2Nano microsphere coating film
The Ni @ SiO prepared in example 12Coating the nano microsphere sol dispersion solution on a chemically polished stainless steel foil of 40 × 40 cm; drying at 60 ℃, and finally annealing at 700 ℃ for 3h at the speed of 10 ℃/min in nitrogen to obtain Ni @ SiO2A solar energy absorber. The thickness of the absorbing coating was measured to be 0.3 mm.
The absorption rate of the coating AM1.5 with different Ni grain sizes is shown in figure 2; according to fig. 2, it can be seen that the Ni nanoparticles with the size of about 40nm synthesized at 20 ℃ have the best absorption rate in the ultraviolet-visible light-near infrared band, and the absorption rate of the coating in the ultraviolet-visible light-near infrared band is reduced as the size of the Ni nanoparticles is increased along with the reduction of the reduction reaction temperature, which may be because the absorption powder is more likely to generate mirror emission on the particle surface due to the closer the size of the absorption powder is to the wavelength of incident light, and is less likely to be absorbed by the powder;
the coating reflectivity of the solar absorber prepared by using the 40nm Ni nano-microspheres and the coating reflectivity after heat treatment at 700 ℃ for 24 hours are schematically shown in FIG. 3; according to the graph in FIG. 3, the coating has little influence on the absorption performance of the ultraviolet-visible light-near infrared band after being subjected to high temperature for a long time, and the prepared coating has good retention capability at high temperature.
Application example 2
The Ni @ SiO prepared in example 22The solar selective absorption nano-microsphere is used as a selective absorption additive to be added into the coating, the addition amount is 30 wt%, and then the film is formed on the carrier by tape casting.
Claims (10)
1. Solar selective absorption Ni @ SiO2The preparation method of the nano-microsphere is characterized by comprising the following steps: firstly, Ni nano-particles are prepared by utilizing reduction reaction and corresponding ligands, then the obtained Ni nano-particles are dissolved in polyvinylpyrrolidone PVP for surface modification, SiO is added into the PVP2Precursor and ethylenediamine, and Ni @ SiO is prepared by adopting a sol-gel method2Solar selective absorption nano-microspheres.
2. The solar selective absorber Ni @ SiO of claim 12The preparation method of the nano-microsphere is characterized by comprising the following steps:
(1) preparing Ni nano microspheres: firstly, uniformly stirring a dispersing agent, Ni salt and deionized water in a reaction container, then introducing nitrogen to remove oxygen in a system, adding a reducing agent under the protection of the nitrogen, carrying out reduction reaction, and separating and drying by using a centrifugal machine to obtain Ni nano particles;
(2)Ni@SiO2synthesizing the solar selective absorption nano microspheres: dissolving the Ni nano particles prepared in the step (1) in polyvinylpyrrolidone PVP for surface modification, and then centrifuging; dispersing the modified Ni nano-particles in deionized water, and adding SiO into the deionized water2The precursor and ethylenediamine react under the action of ultrasound and then are centrifuged; washing to obtain Ni @ SiO2Solar selective absorption nano-microspheres.
3. The solar selective absorber Ni @ SiO of claim 22The preparation method of the nano-microsphere is characterized by comprising the following steps: the dispersant is specifically sodium dodecyl sulfate,One or more of oleic acid, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate;
the reducing agent is specifically sodium borohydride, potassium borohydride or lithium aluminum hydride.
4. The solar selective absorber Ni @ SiO of claim 22The preparation method of the nano-microsphere is characterized by comprising the following steps: the Ni salt is specifically nickel nitrate hexahydrate, nickel sulfate hexahydrate, nickel chloride tetrahydrate or nickel acetate tetrahydrate.
5. The solar selective absorber Ni @ SiO of claim 22The preparation method of the nano-microsphere is characterized by comprising the following steps: the SiO2The precursor is tetraethyl silicate and/or tetramethoxysilane and propyl orthosilicate.
6. The solar selective absorber Ni @ SiO of claim 22The preparation method of the nano-microsphere is characterized in that the step (1) is specifically as follows: boiling deionized water, and deoxidizing for later use; respectively pre-dispersing 25-30g of dispersing agent and 2.9-3g of Ni salt into 10mL of deionized water, then adding the uniformly dispersed dispersing agent and Ni salt into a reaction container containing 80mL of deionized water, and uniformly stirring at 300-400rpm magnetic force; introducing nitrogen to remove oxygen in the system, adding 29-30mg of reducing agent under the protection of nitrogen, reacting for 1-1.5h at 5-20 ℃, stopping the reaction, then performing deionization washing and centrifugation for a plurality of times, and drying for 22-26h at 40-50 ℃ in a vacuum oven under 0.08-0.1MPa to obtain the Ni nano particles.
7. The solar selective absorber Ni @ SiO of claim 22The preparation method of the nano-microsphere is characterized in that the step (2) is specifically as follows: mixing 5-7g of polyvinylpyrrolidone, 100mL of deionized water and 0.9-1g of Ni nanoparticles prepared in the step (1), magnetically stirring for 25-30min, and then centrifuging to disperse the Ni nanoparticles into 11-13mL of ethanol; 2-2.5mL of ethylenediamine and 0.55-0.56mL of SiO were added2Stirring and reacting the precursor for 70-80min at 300-400rpm magnetic stirring, and keeping the temperature at 5-20 ℃; finally, deionized water is washed for several timesWashing and centrifuging to obtain Ni @ SiO2Solar selective absorption nano-microspheres.
8. Solar selective absorption Ni @ SiO prepared by the process according to any one of claims 1 to 72The application of the nano-microsphere is characterized in that: the solar energy absorber is applied to a solar energy absorber.
9. Solar selective absorption Ni @ SiO prepared by the process according to any one of claims 1 to 72The application of the nano-microsphere is characterized in that: mixing Ni @ SiO2The solar selective absorption nano-microspheres are added into the coating as an additive, and a film is formed on the carrier to prepare the solar absorber.
10. Solar selective absorption Ni @ SiO prepared by the process according to any one of claims 1 to 72The application of the nano-microsphere is characterized in that: mixing Ni @ SiO2The solar selective absorption nano-microspheres are dispersed in a dispersing agent, and a film is formed by a sol-gel method to prepare the solar absorber.
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