CN112725827A - Preparation method of black phosphorus alkene modified iron oxide composite photoelectrode - Google Patents
Preparation method of black phosphorus alkene modified iron oxide composite photoelectrode Download PDFInfo
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Abstract
The invention relates to the technical field of materials, in particular to a preparation method of a black phosphorus alkene modified iron oxide composite photoelectrode. According to the invention, a surface modification method is adopted, and a small amount of black phosphorus alkene is loaded on the titanium-treated iron oxide photoelectrode, so that on one hand, the energy level structure of the black phosphorus alkene matched with the iron oxide is very beneficial to the separation and transmission of photon-generated carriers; on the other hand, phosphorus-oxygen groups generated on the surface of the black phosphorus alkene can effectively bridge the black phosphorus alkene and the iron oxide nanoparticles, and the combination of the black phosphorus alkene and the iron oxide nanoparticles is more compact, so that the separation and the transmission of photon-generated carriers are further promoted.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a preparation method of a black phosphorus alkene modified iron oxide composite photoelectrode.
Background
Since Fujishima and Honda of professor Fujishima of tokyo university in 1972 discovered the phenomenon of hydrogen production by water decomposition through photoelectrocatalysis on a single-crystal titanium dioxide electrode, the technology of hydrogen production by water decomposition through solar photoelectrocatalysis with semiconductor nano materials as catalysts has become one of the most concerned research directions all over the world. The hydrogen production by decomposing water by solar photoelectrocatalysis is a special heterogeneous catalysis, which refers to a process that a semiconductor photoelectrode (catalyst) realizes the decomposition of water under the combined action of an external electric field and sunlight. The method has the characteristics of high hydrogen production efficiency compared with a photocatalytic system, moderate cost and environmental protection, and thus the method is widely concerned by researchers.
Among the numerous photoelectrode materials, iron oxide is considered to be the most promising one, mainly thanks to its suitable visible light absorption band gap (2.0-2.2eV), excellent photoelectrochemical stability, low production cost and non-toxicity. However, at the same time, iron oxide also has fatal defects, such as low conductivity, short hole diffusion distance and service life, slow surface oxygen evolution reaction kinetics speed and the like, so that the activity of the iron oxide for decomposing water by photoelectrocatalysis is severely limited. At present, the photoelectrocatalysis performance of the iron oxide photoelectrode cannot meet the requirements of practical application.
In order to effectively solve the problems, in the last decades, researchers have successively designed and developed various effective modification strategies, such as morphology control, element doping, heterojunction construction, surface treatment, and the like. Among these, titanium treatment is the most used and most effective one. Therefore, in the invention, titanium-treated iron oxide with higher photoelectrocatalysis activity is selected as a black phosphorus alkene-loaded carrier in the next step to obtain an iron oxide photoelectrode with more excellent performance.
On the other hand, as a novel two-dimensional material with excellent conductivity and adjustable band gap, the black phosphorus alkene has shown huge application potential in the aspects of photoelectric detection, gas sensing, chemical catalysis, energy storage and the like in recent years. Meanwhile, due to the excellent oxygen evolution reaction capability of the black phosphorus alkene, the application of the black phosphorus alkene in the field of hydrogen production by solar photoelectric catalytic water decomposition is also very widely concerned. At present, composite photo-electrodes such as black phosphene/bismuth vanadate, black phosphene/titanium dioxide and the like are successfully prepared, and show excellent photo-catalytic activity. However, for the iron oxide photoelectrode, few studies and reports on the photoelectrocatalytic behavior of the black phosphene are available. Therefore, it is necessary to intensively study and analyze the synthesis, performance, operation mechanism, and the like of the black phospholene-modified iron oxide photoelectrode.
Disclosure of Invention
The invention aims to solve the problem that the hydrogen production performance of the existing iron oxide photoelectrode by water decomposition through photoelectrocatalysis cannot meet the requirement of practical application.
The invention also aims to provide a preparation method of the black phosphorus alkene modified iron oxide composite photoelectrode. The method disclosed by the invention is simple and easy to prepare, easy to control conditions, low in cost, non-toxic and environment-friendly, and provides possibility for large-scale production of high-performance iron oxide electrode materials.
In order to realize the purpose of the invention, the following technical scheme is mainly adopted:
a preparation method of a black phosphorus alkene modified iron oxide composite photoelectrode comprises the following steps:
(1) and cleaning the FTO glass.
(2) Putting the cleaned FTO conductive glass into a reaction kettle in a mode that the conductive surface faces upwards, and adding an iron oxide precursor solution into the reaction kettle; and heating the reaction kettle at 100 ℃ for 4h, and taking out the FTO conductive glass after the reaction kettle is heated and cooled.
(3) And putting the FTO conductive glass into a titanium acetylacetonate oxide (TOPD) solution, performing ultrasonic treatment, then putting the FTO conductive glass into a muffle furnace, annealing for 2h at 550 ℃, and annealing for 15min at 750 ℃ to obtain the titanium-treated iron oxide photoelectrode.
(4) And (3) dropwise adding a black phosphorus alkene solution on the iron oxide photoelectrode treated by titanium, and putting the iron oxide photoelectrode into a vacuum drying oven to be heated for 20min at the temperature of 150 ℃, so as to obtain the black phosphorus alkene modified iron oxide composite photoelectrode.
The preparation method comprises the following steps: in the step (1), the step of cleaning the FTO glass comprises the following steps: firstly, cleaning stains on the surface of the FTO glass by using a hand sanitizer or a liquid detergent, then sequentially putting the FTO glass into deionized water and absolute ethyl alcohol for ultrasonic cleaning for 15 minutes respectively, and finally drying the FTO glass for later use.
The preparation method comprises the following steps: in the step (2), the preparation method of the iron oxide precursor solution comprises the following steps: 2.025 g (75mM) FeCl were weighed3·6H2O and 0.9 g (50mM) C6H12O6Dissolving the mixture in 100mL of deionized water, and magnetically stirring for 15 minutes to obtain the product; after the hydrothermal reaction is finished and the reaction kettle is naturally cooled to room temperature, the FTO glass needs to be taken out of the reaction kettleDischarging and washing with deionized water;
the preparation method comprises the following steps: in the step (3), the following steps are carried out: the concentration of the TOPD solution is 2.5mM, the volume is 5mL, and the ultrasonic time is 5 min; the temperature rise rate of the whole annealing stage is controlled at 10 ℃/min;
the preparation method comprises the following steps: in the step (4), the dropping amount of the black phosphorus alkene solution is 50 mu L; the preparation method of the black phosphorus alkene solution comprises the following steps: 500mg of red phosphorus, 1g of tin powder and 100mg of iodine were sealed in a vacuum quartz glass ampoule having a length of 100mm, an inner diameter of 8mm and a wall thickness of 1mm, and then the sealed ampoule was heated from room temperature to 600 ℃ at a slow heating rate for 7 hours and then held at 600 ℃ for 5 to 10 hours. Finally, a 4 mm-sized bulk black phosphorus single crystal was obtained, which was bulk black phosphorus. Then 25mg of block black phosphorus is dissolved in 50mL of isopropanol solution and is subjected to ultrasonic treatment for 8h, and then the solution is centrifuged at 9000r/min for 10min to obtain a supernatant.
The composite iron oxide photoelectrode with more excellent photoelectric catalytic performance is prepared by the method.
The invention has the beneficial effects that:
according to the invention, a surface modification method is adopted, and a small amount of black phosphorus alkene is loaded on the titanium-treated iron oxide photoelectrode, so that on one hand, the energy level structure of the black phosphorus alkene matched with the iron oxide is very beneficial to the separation and transmission of photon-generated carriers; on the other hand, phosphorus-oxygen groups generated on the surface of the black phosphorus alkene can effectively bridge the black phosphorus alkene and the iron oxide nanoparticles, and the combination of the black phosphorus alkene and the iron oxide nanoparticles is more compact, so that the separation and the transmission of photon-generated carriers are further promoted.
In addition, the preparation method is very simple, and has the characteristics of mild experimental conditions, simple process, low energy consumption and environmental friendliness.
Drawings
FIG. 1 is a flow chart of the preparation of a black phosphorus alkene/ferric oxide composite photoelectrode.
FIG. 2 is a Scanning Electron Microscope (SEM) image and a high-resolution transmission electron microscope (HRTEM) image of example 3. (a) And (b) respectively treating titanium with iron oxide (Ti-Fe) by Scanning Electron Microscope (SEM)2O3) Photoelectrode and loadThe morphology of the titanium-treated iron oxide photoelectrode of black phosphene (Ti-Fe2O3/BP) was characterized and analyzed. (c) For further characterization and analysis of the Ti-Fe2O3/BP microstructure using High Resolution Transmission Electron Microscopy (HRTEM).
FIG. 3 is a graph of photocurrent density versus applied bias (J-V) performance of a black phosphene/iron oxide composite photoelectrode. (a) The photocurrent density graphs of the composite photoelectrode of example 1, example 2 and example 3; (b) is Ti-Fe in example 32O3Graph comparing the photocurrent density of Ti-Fe2O3/BP photoelectrode.
FIG. 4 is an X-ray photoelectron spectroscopy (XPS) chart in example 3. (a) Is Ti-Fe2O3P2P XPS spectrum of/BP photoelectrode; (b) is Ti-Fe2O3And Ti-Fe2O3O1s XPS spectrum of/BP photoelectrode; (c) is Ti-Fe2O3And Ti-Fe2O3Fe2p XPS spectrum of/BP photoelectrode; (d) is Ti-Fe2O3And Ti-Fe2O3Ti 2p XPS spectrum of/BP photoelectrode.
Fig. 5 is a graph showing the separation efficiency of photogenerated carriers at the surface interface and the bulk phase in example 3. (a) Is a surface; (b) is a bulk phase.
Fig. 6 is a schematic diagram of the energy level structure and the operation mechanism in embodiment 3.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified. Preparing a black phosphorus alkene modified iron oxide photoelectrode: placing FTO conductive glass into a reaction kettle in a mode that a conductive surface faces upwards, and adding a precursor solution (weighing 2.025 g FeCl)3·6H2O and 0.9 g C6H12O6Dissolving the mixture in 100mL of deionized water, and magnetically stirring for 15 minutes to obtain the product); heating the reaction kettle at 100 ℃ for 4 hours, and taking out the FTO conductive glass after the reaction kettle is heated and cooled; putting the FTO conductive glass into titanium oxide acetylacetonate (TOPD) solution, performing ultrasonic treatment for 5min, putting the FTO conductive glass into a muffle furnace, and performing ultrasonic treatmentAnnealing at 550 ℃ for 2h, and then annealing at 750 ℃ for 15min to obtain the titanium-treated iron oxide photoelectrode.
The following example embodiments are all between iron oxide and black phospholene loaded iron oxide photoelectrode.
Example 1: and (3) dropwise adding 30 mu L of black phosphorus alkene solution on the sample treated by the titanium, and putting the sample treated by the titanium into a vacuum drying oven to be heated for 10min at 200 ℃, thereby obtaining the black phosphorus alkene modified iron oxide composite photoelectrode.
Example 2: and (3) dropwise adding 100 mu L of black phosphorus alkene solution on the sample treated by the titanium, and putting the sample treated by the titanium into a vacuum drying oven to heat for 30min at 100 ℃, thereby obtaining the black phosphorus alkene modified iron oxide composite photoelectrode.
Example 3: and (3) dropwise adding 50 mu L of black phosphorus alkene solution on the sample treated by the titanium, and putting the sample treated by the titanium into a vacuum drying oven to be heated for 20min at the temperature of 150 ℃, so as to obtain the black phosphorus alkene modified ferric oxide composite photoelectrode.
Fig. 1 is a flow chart of preparation of a black phosphorus alkene loaded iron oxide composite photoelectrode. Firstly, FTO conductive glass attached with an FeOOH film is put into TOPD solution for ultrasonic treatment, and then the FTO conductive glass is converted into a titanium-treated iron oxide photoelectrode through high-temperature annealing. Finally, the black phosphorus alkene solution is dripped on the surface of the iron oxide photoelectrode treated by the titanium, so that the black phosphorus alkene modified iron oxide composite photoelectrode (Ti-Fe) is successfully prepared2O3/BP)。
FIG. 2 is a SEM topographic comparison map, HRTEM image of example 3. Wherein FIGS. 2a and 2b respectively treat titanium with iron oxide (Ti-Fe) using a Scanning Electron Microscope (SEM)2O3) Photoelectrode and black phosphorus alkene-loaded titanium-treated iron oxide photoelectrode (Ti-Fe)2O3BP) were characterized and analyzed. FIG. 2c is a graph of Ti-Fe using a High Resolution Transmission Electron Microscope (HRTEM)2O3Further characterization and analysis of the microstructure of the/BP. As shown in fig. 2a and 2b, black phosphene was successfully supported on the surface of the iron oxide photoelectrode. Fig. 2c further demonstrates the successful fabrication of the black phospholene/iron oxide composite photoelectrode.
FIG. 3 is a graph of photocurrent density versus applied bias (J-V) performance of the composite photoelectrode of example 1, example 2 and example 3. The performance test isIn a quartz cell of three-electrode system, from a xenon cold light source (luminous power 100 mW/cm) equipped with an AM 1.5G analog filter2) As a sunlight simulation light source, a CHI 660E type electrochemical workstation is used as a data acquisition device. FIG. 3a shows that 50. mu.L of black phosphorus alkene is dropped on the composite photoelectrode (Ti-Fe)2O3BP (50 μ L)) had the best photocatalytic activity and a photocurrent density of 3.02mA/cm at 1.23V vs. rhe22.91mA/cm higher than 20 μ L photoelectrode respectively2And 2.20mA/cm for a 100. mu.L photoelectrode2. Meanwhile, as can be seen from FIG. 3b, Ti-Fe2O3The photocurrent density of the/BP (50 mu L) composite photoelectrode is also higher than that of the titanium-treated iron oxide photoelectrode (Ti-Fe)2O3) A photocurrent density of only 1.93mA/cm at 1.23V vs. rhe2. The result shows that the load of the black phosphorus alkene can effectively improve the photoelectrocatalysis water decomposition performance of the titanium modified iron oxide photoelectrode.
FIG. 4 is an XPS spectrum of example 3. The use of XPS for Ti-Fe2O3And Ti-Fe2O3The electronic structure and chemical composition of the/BP two electrodes are characterized and researched. As shown in FIG. 4a, the appearance of the P-P peak confirms that the black phospholene is present in Ti-Fe2O3The existence of the/BP photoelectrode further illustrates the successful preparation of the iron oxide/black phospholene composite photoelectrode. In addition, the P-O peak in FIG. 4a and PO in FIG. 4b4 3-The appearance of the peak indicates that the black phospholene prepared in the present invention is partially oxidized and a large amount of phosphorus-oxygen PO exists on the surface4 3-A group. While the shift in the position of the Fe2p peak in FIG. 4c and the Ti 2p peak in FIG. 4d indicates PO on the black phospholene surface4 3-The groups can play a role of bridging so that the black phosphorus alkene is more tightly combined with the ferric oxide.
FIG. 5 shows the surface and bulk charge separation efficiency of example 3. Relative to Ti-Fe2O3Photoelectrode of Ti-Fe2O3the/BP photoelectrode exhibits higher separation efficiency both in bulk and at the surface of the electrode. This indicates that Ti-Fe benefits from the matching energy level structure of the black phosphene with iron oxide and the formation of phosphorus-oxygen groups2O3The preparation of the/BP heterojunction can remarkably accelerate the separation and transmission of photo-generated charges, so that the performance of the photoelectrocatalysis water decomposition of the/BP heterojunction is improved.
Fig. 6 is a schematic diagram of the energy level structure and the operation mechanism in embodiment 3. As can be seen, the valence band top of the black phosphorus alkene is significantly higher than that of the iron oxide, and the conduction band bottom is significantly lower than that of the iron oxide, which indicates that in Ti-Fe2O3In the/BP heterojunction, the black phosphorus alkene has an energy level structure matched with iron oxide, and the separation of photogenerated electrons and holes is greatly facilitated. Meanwhile, the phosphorus-oxygen group formed between the iron oxide and the black phosphene enables the connection between the iron oxide nanoparticles and the black phosphene to be tighter, so that the transmission speed of the photoproduction cavity is increased.
The above disclosure is only a preferred embodiment of the present invention, and the present invention shall be covered by the protection scope of the present invention by the replacement and modification according to the common knowledge and conventional means in the art without departing from the concept of the method of the present invention.
Claims (6)
1. A preparation method of a black phosphorus alkene modified ferric oxide composite photoelectrode is characterized by comprising the following specific steps:
(1) cleaning the FTO glass;
(2) putting the cleaned FTO conductive glass into a reaction kettle in a mode that the conductive surface faces upwards, and adding an iron oxide precursor solution into the reaction kettle; heating the reaction kettle at 100 ℃ for 4 hours, and taking out the FTO conductive glass after the reaction kettle is heated and cooled;
(3) putting the FTO conductive glass into a titanium acetylacetonate oxide (TOPD) solution, performing ultrasonic treatment, then putting the FTO conductive glass into a muffle furnace, annealing for 2h at 550 ℃, and annealing for 15min at 750 ℃ to obtain a titanium-treated iron oxide photoelectrode;
(4) and (3) dropwise adding a black phosphorus alkene solution on the iron oxide photoelectrode treated by titanium, and putting the iron oxide photoelectrode into a vacuum drying oven to be heated for 20min at the temperature of 150 ℃, so as to obtain the black phosphorus alkene modified iron oxide composite photoelectrode.
2. The method for preparing a black phosphorus alkene modified iron oxide composite photoelectrode according to claim 1, wherein in the step (1), the step of cleaning the FTO glass comprises the following steps: firstly, cleaning stains on the surface of the FTO glass by using a hand sanitizer or a liquid detergent, then sequentially putting the FTO glass into deionized water and absolute ethyl alcohol for ultrasonic cleaning for 15 minutes respectively, and finally drying the FTO glass for later use.
3. The method for preparing a black phosphorus alkene modified iron oxide composite photoelectrode according to claim 1, wherein in the step (2), the method for preparing the iron oxide precursor solution comprises the following steps: 2.025 g (75mM) FeCl were weighed3·6H2O and 0.9 g (50mM) C6H12O6Dissolving the mixture in 100mL of deionized water, and magnetically stirring for 15 minutes to obtain the product; after the hydrothermal reaction is finished and the reaction kettle is naturally cooled to the room temperature, the FTO glass needs to be taken out of the reaction kettle and washed clean by deionized water.
4. The method for preparing the black phosphorus alkene modified iron oxide composite photoelectrode as claimed in claim 1, wherein in the step (3), the TOPD solution has a concentration of 2.5mM, a volume of 5mL, and an ultrasonic time of 5 min; the heating rate of the whole annealing stage is controlled at 10 ℃/min.
5. The method for preparing a black phosphorus alkene modified iron oxide composite photoelectrode as claimed in claim 1, wherein in the step (4), the dropping amount of the black phosphorus alkene solution is 50 μ L.
6. The method for preparing the black phosphorus alkene modified iron oxide composite photoelectrode as claimed in claim 1 or 5, wherein the method for preparing the black phosphorus alkene solution is as follows: sealing 500mg of red phosphorus, 1g of tin powder and 100mg of iodine in a vacuum quartz glass ampoule bottle with the length of 100mm, the inner diameter of 8mm and the wall thickness of 1mm, heating the sealed ampoule bottle from room temperature to 600 ℃ at a slow heating rate for 7 hours, and keeping the temperature at 600 ℃ for 5-10 hours, so as to obtain a 4 mm-sized block black phosphorus single crystal which is block black phosphorus; then 25mg of block black phosphorus is dissolved in 50mL of isopropanol solution and is subjected to ultrasonic treatment for 8h, and then the solution is centrifuged at 9000r/min for 10min to obtain a supernatant.
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