CN113772664B - Nickel black-graphene composite photo-thermal conversion film and preparation method thereof - Google Patents
Nickel black-graphene composite photo-thermal conversion film and preparation method thereof Download PDFInfo
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Abstract
A nickel black-graphene composite photo-thermal conversion film and a preparation method thereof relate to the structure, preparation and sea water desalination application of the nickel black-graphene composite photo-thermal conversion film. And simultaneously depositing graphene and nickel black on the wall surface of the foamed nickel hole by adopting a one-step electrochemical method to obtain the nickel black-graphene composite photo-thermal conversion film. The photo-thermal conversion efficiency is improved by combining the plasma resonance effect of the metal nickel black and the advantage of wide light absorption wavelength range of the graphene carbon material. The nickel black-graphene photo-thermal conversion film is used for sea water desalination under the illumination condition. Under the illumination intensity of 1sun, the light-steam energy conversion efficiency reaches 162.4 percent, and the steam permeability can reach 2.37kg/m 2 ·h。
Description
Technical Field
The invention belongs to the field of photo-thermal conversion and application thereof in sea water desalination.
Background
Fresh water resources are resources indispensable to human survival. Thus, more and more countries employ seawater desalination technology to alleviate the shortage of fresh water. However, a higher energy consumption is required in the sea water desalination process. Solar energy is used as an energy source necessary for living organisms, is ubiquitous and inexhaustible in life, and is often considered to be introduced into sea water desalination technology, so that the solar energy has a photo-thermal conversion effect and effectively reduces energy consumption. The problem of water resource shortage is solved by combining two most abundant resources on the earth, sustainable development is realized, and the method is a great trend of the future sea water desalination technology. Currently, commonly used solar thermal conversion materials are mainly classified into the following categories: various carbon materials, plasma metals, inorganic semiconductors, and organic polymers. A plasma metal material is used as a solar energy absorbing material due to its strong electromagnetic wave absorbing ability. At present, noble metals such as gold and silver have been widely studied, but the high cost severely limits the wide application. The economical nickel black can effectively replace expensive solar heat conversion materials to realize solar heat conversion. Meanwhile, graphene is an emerging two-dimensional material, has the characteristics of wide solar energy absorption wavelength range, good photo-thermal conversion performance and the like, and is widely applied to photo-thermal conversion. Therefore, the invention considers that the nickel black material and the graphene are combined together to form the photo-thermal composite material and is applied to the aspect of sea water desalination technology.
Disclosure of Invention
The invention aims to provide a nickel black-graphene composite photo-thermal conversion film and a preparation method thereof, which aim to improve photo-thermal conversion efficiency and sea water desalination by cooperatively playing the advantages of a metal material and a carbon material in photo-thermal conversion.
The method comprises the following steps:
the nickel black-graphene composite photo-thermal conversion film and the preparation method thereof are characterized by comprising the following specific steps:
(1) Adding a certain amount of ammonium sulfate and nickel sulfate into a solvent, and continuously stirring until the ammonium sulfate and the nickel sulfate are fully dissolved to form electrolyte;
(2) The foam nickel is used as a cathode, the graphite foil is used as an anode, and the distance between the electrodes is adjusted in the electrolyte;
(3) Under a certain direct current voltage, the gas and hydroxyl radicals generated by the electrolyte have intercalation on the graphite foil, so that the graphene is peeled off; the nickel ions play a role of a carrier, and reduce the graphene to nickel black while transferring the graphene to a cathode; thereby generating a uniform nickel black-graphene composite film on the cathode;
(4) Adjusting the concentration of the electrolyte, the deposition voltage and the deposition time to control the content of the nickel black-graphene composite material on the cathode;
the concentration of ammonium sulfate in the step (1) is 0-0.2M, and the concentration of nickel sulfate is 0-0.08M;
the electrode distance in the step (2) is 0.5-2 cm;
the voltage range in the step (3) is 5-15V;
the deposition time in the step (4) is 5-40 min;
(5) And after electrodepositing for a certain time, the nickel black-graphene photo-thermal conversion film is fully cleaned in deionized water, and is taken out and dried in an oven at 60 ℃ for 12 hours.
The formation principle of the nickel black-graphene composite photo-thermal conversion film is as follows: after the system is electrified, the gas and hydroxyl radicals generated by the electrolyte have intercalation effect on the graphite foil, so that the graphene is peeled off. The nickel ions play a role of charging salt, and reduce the graphene to nickel black while transferring the graphene to a cathode; thereby generating a uniform nickel black-graphene composite film on the cathode.
The invention adopts a one-step electrochemical method, the preparation process is simple, and the film is formed once; the nickel black on the surface of the carrier can realize the photo-thermal conversion effect under the effect of the plasma resonance effect, the graphene has a wide photo-absorption wavelength range, and the graphene can increase the generation of water vapor in the sea water desalination process to obtain more fresh water.
Drawings
Fig. 1 is an SEM image of a nickel black-graphene composite photothermal conversion film.
Figure 2 XRD pattern of nickel black-graphene composite photothermal conversion film.
Fig. 3 is a Raman diagram of the nickel black-graphene composite photo-thermal conversion film.
Description of the embodiments
In order to better explain the present invention, the present invention will be further described below by taking a nickel black-graphene composite photo-thermal conversion film as an example with reference to the accompanying drawings.
Early stage preparation of experiment:
1. preparation of a nickel black-graphene composite photo-thermal conversion film:
(1) Adding 1.32g of ammonium sulfate and 0.42g of nickel sulfate into 200ml of deionized water, and continuously stirring at room temperature until the ammonium sulfate and the nickel sulfate are fully dissolved to form an electrolyte solution;
(2) Connecting foam nickel on a cathode, connecting graphite foil on an anode, adjusting the distance between the connected electrodes, and placing the electrodes into electrolyte;
(3) Opening a switch of an externally applied direct current power supply, and adjusting experimental voltage and experimental time to adjust the content of the nickel black-graphene composite material on the foam nickel;
(4) And (3) cleaning the plated nickel black-graphene photo-thermal conversion film in deionized water, taking out, and drying in a 60 ℃ oven for 12 hours.
Fig. 1, 2 and 3 are SEM, XRD and Raman diagrams, respectively, of a nickel black-graphene composite photo-thermal conversion film. The existence of the graphene and the nickel black on the film surface can be clearly seen through an SEM image, and the characteristic peaks of the nickel and the graphene can be seen through XRD and a Raman image, so that the nickel black-graphene composite film can be effectively prepared.
2. The experimental process comprises the following steps:
the effective membrane area prepared above is 9cm 2 The nickel black-graphene composite photo-thermal conversion film is placed on an evaporation cup filled with NaCl solution with the concentration of 30g/L, and simulated sunlight with the light intensity of 1sun is adopted for irradiation. The initial weight and the final weight of the evaporation cup were weighed and the vapor permeability was calculated.
Example 1
Adding 1.32g of ammonium sulfate and 0.42g of nickel sulfate into 200ml of deionized water, and continuously stirring at room temperature until the ammonium sulfate and the nickel sulfate are fully dissolved to form an electrolyte solution; connecting foam nickel on a cathode, connecting graphite foil on an anode, adjusting the distance between the connected electrodes, and placing the electrodes into electrolyte; opening a switch of an externally-applied direct current power supply, and reacting for 10 minutes under 13V voltage; and (3) cleaning the plated nickel black-graphene photo-thermal conversion film in deionized water, taking out, and drying in a 60 ℃ oven for 12 hours. Placing on an evaporation cup under 1sun illumination, with light-steam energy conversion efficiency of 136.94% and steam permeability of 2.00 kg/m 2 ·h。
Example 2
Adding 1.32g of ammonium sulfate and 0.42g of nickel sulfate into 200ml of deionized water, and continuously stirring at room temperature until the ammonium sulfate and the nickel sulfate are fully dissolved to form an electrolyte solution; connecting foam nickel on a cathode, connecting graphite foil on an anode, adjusting the distance between the connected electrodes, and placing the electrodes into electrolyte; opening a switch of an externally-applied direct current power supply, and reacting for 20 minutes under 13V voltage; and (3) cleaning the plated nickel black-graphene photo-thermal conversion film in deionized water, taking out, and drying in a 60 ℃ oven for 12 hours. Placing on an evaporation cup under 1sun illumination, with light-steam energy conversion efficiency of 138.49% and steam permeability of 2.02 kg/m 2 ·h。
Example 3
Adding 1.32g of ammonium sulfate and 0.42g of nickel sulfate into 200ml of deionized water, and continuously stirring at room temperature until the ammonium sulfate and the nickel sulfate are fully dissolved to form an electrolyte solution; the foam nickel is connected with the cathode, the graphite foil is connected with the anode, and the mixture is connectedThe electrodes of which are well adjusted in distance and placed in electrolyte; opening a switch of an externally-applied direct current power supply, and reacting for 30 minutes under 13V voltage; and (3) cleaning the plated nickel black-graphene photo-thermal conversion film in deionized water, taking out, and drying in a 60 ℃ oven for 12 hours. Placing on an evaporation cup under 1sun illumination, with light-steam energy conversion efficiency of 162.48% and steam permeability of 2.37kg/m 2 ·h。
Example 4
Adding 1.32g of ammonium sulfate and 0.42g of nickel sulfate into 200ml of deionized water, and continuously stirring at room temperature until the ammonium sulfate and the nickel sulfate are fully dissolved to form an electrolyte solution; connecting foam nickel on a cathode, connecting graphite foil on an anode, adjusting the distance between the connected electrodes, and placing the electrodes into electrolyte; opening a switch of an externally-applied direct current power supply, and reacting for 40 minutes under 13V voltage; and (3) cleaning the plated nickel black-graphene photo-thermal conversion film in deionized water, taking out, and drying in a 60 ℃ oven for 12 hours. Placing on an evaporation cup under 1sun illumination, with light-steam energy conversion efficiency of 140.37% and steam permeability of 2.05 kg/m 2 ·h。
Comparative example 1:
the evaporation cup without the film containing NaCl solution with the concentration of 30g/L is irradiated by using the simulated sunlight with the light intensity of 1 sun. The initial weight and the end weight of the evaporation cup were weighed, the light-steam energy conversion efficiency was calculated to be 50.89%, and the steam permeability was calculated to be 0.75k g/m 2 ·h。
Comparative example 2:
adding 1.32g of ammonium sulfate into 200ml of deionized water, and continuously stirring at room temperature until the ammonium sulfate is fully dissolved to form an electrolyte solution; connecting foam nickel on a cathode, connecting two nickel plates on anodes on the left side and the right side of the foam nickel respectively, adjusting the distance between the connected electrodes, and placing the electrodes into electrolyte; opening an externally applied direct current power supply, and electrolyzing for 20 minutes under 15V voltage; and cleaning the plated nickel black photothermal conversion film in deionized water, taking out, and drying in a 60 ℃ oven for 12 hours. Under 1 sun's illumination, the light-steam energy conversion efficiency was 91.87%, and the steam permeability was 1.07kg/m 2 ·h。
Comparative example 3:
1.32g of ammonium sulfate was added to 200ml of deionized waterContinuously stirring the mixture in the sub-water at room temperature until the mixture is fully dissolved to form electrolyte solution; and respectively placing graphite foil on the cathode and the anode, peeling for 1 hour, and carrying out suction filtration on the obtained graphene to obtain a graphene film. Under 1 sun's light, the light-steam energy conversion efficiency was 81.20% and the steam permeability was 1.19kg/m 2 ·h。
Conclusion:
it can be seen from table 1 that the nickel black-graphene composite photo-thermal conversion film realizes a synergistic effect compared with the nickel black film and the graphene film, has a better effect in sea water desalination, and has the maximum photo-steam energy conversion efficiency and steam permeability when the electrolysis time is 30 min.
TABLE 1 effective membrane area of 9cm 2 Nickel black-graphene composite photo-thermal conversion film and steam permeability of comparative example under 1sun illumination
| Film and method for producing the same | Comparative example 1 (without film) | Comparative example 2 (Nickel black film) | Comparative example 3 (graphene film) | 10min | 20min | 30min | 40min |
| Permeability to steam (kg/m) 2 ·h） | 0.75 | 1.07 | 1.19 | 2.00 | 2.02 | 2.37 | 2.05 |
Claims (3)
1. The preparation method of the nickel black-graphene composite photo-thermal conversion film is characterized by comprising the following steps of:
(1) Adding a certain amount of ammonium sulfate and nickel sulfate into deionized water, and continuously stirring until the ammonium sulfate and the nickel sulfate are fully dissolved to form electrolyte with the concentration of ammonium sulfate of 0-0.2M and the concentration of nickel sulfate of 0-0.08M;
(2) Using foam nickel as a cathode and graphite foil as an anode, and adjusting the distance between electrodes in electrolyte to be 0.5-2 cm;
(3) Under the direct-current voltage of 5-15V, the gas and hydroxyl radicals generated by the electrolyte have intercalation effect on the graphite foil of the anode, so that the graphene is peeled from the anode into the electrolyte; meanwhile, nickel ions in the electrolyte transfer graphene stripped from the anode to the cathode under the action of an electric field force, and the nickel ions are reduced at the cathode; under the high current density generated by high voltage, the nickel-graphene composite deposition layer deposited on the cathode is burnt to form a nickel black-graphene composite photo-thermal conversion film;
(4) Adjusting the concentration of the electrolyte, the deposition voltage and the deposition time to control the component content of nickel black and graphene in the nickel black-graphene composite material on the cathode;
(5) And after electrodeposition for 5-40 minutes, the nickel black-graphene photo-thermal conversion film is fully cleaned in deionized water, and is taken out and dried in a 60 ℃ oven for 12 hours.
2. The method for preparing the nickel black-graphene photothermal conversion film according to claim 1, wherein graphene and nickel black are simultaneously deposited on the cathode by a one-step electrochemical method.
3. The nickel black-graphene composite photo-thermal conversion film obtained by the preparation method of claim 1 is applied to solar-driven seawater desalination and other water treatment processes.
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