CN115156548B - Nano belt-like Cu 3 P/Cu material and preparation method thereof - Google Patents
Nano belt-like Cu 3 P/Cu material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a nano strip Cu 3 The preparation method of the P/Cu specifically comprises the following steps: dispersing black phosphorus in an organic solvent under the anhydrous and anaerobic condition to obtain a mixed solution A; ultrasonic stripping is carried out on the mixed solution A by utilizing a liquid phase stripping method, and then an upper layer solution is collected to obtain black phosphorus nano-sheet dispersion liquid; carrying out hydrothermal reaction on the black phosphorus nano-sheet dispersion liquid subjected to ultrasonic stripping and copper acetylacetonate, cleaning, centrifuging and drying to obtain nano-ribbon Cu 3 P/Cu material; the preparation process is controllable, and the Cu composite material is prepared 3 The interface effect of P/Cu improves the electronic structure of the material, thereby effectively improving the electrocatalytic reaction activity; and prepared Cu 3 The P/Cu material is in nano-ribbon distribution, is not easy to agglomerate and has high specific surface area.
Description
Technical Field
The application relates to the technical field of preparation and conversion of new energy materials, in particular to nano strip Cu 3 P/Cu material and its preparation method are provided.
Background
Metal phosphides are a class of interstitial compounds formed by filling non-metallic elemental phosphorus with a large atomic radius into a lattice of metal atoms. Because of its special structure, phosphide exhibits higher stability, reactivity, etc., than other nitrides, oxides, sulfides, etc. The metal phosphide has wide application in the fields of photoelectricity, magnetism and energy storage. Copper-based materials have obvious advantages in oxidation-reduction performance compared with Co, fe, ni and the like, so research on copper phosphide materials becomes a research hot spot.
Currently, cu 3 The preparation method of the P/Cu nano-micron material has less research; in the prior art, cu 3 The preparation method of the P/Cu is generally as follows: firstly, preparing a precursor of Cu, and preparing a copper-based carrier; then, sodium hypophosphite is used as a phosphorus source to generate phosphine (extremely toxic) in the high-temperature process for preparing Cu by phosphating 3 P, cu is prepared by controlling the phosphating time 3 P/Cu, the method has poor controllability and safety, and can cause agglomeration of materials in the high-temperature phosphating process, so that Cu with high specific surface area is difficult to obtain 3 P/Cu composite.
In view of this, the present application is specifically proposed.
Disclosure of Invention
To solve one of the technical defects, embodiments of the present application provide a nano-ribbon Cu 3 P/Cu preparation method and nano strip Cu 3 P/Cu material. The preparation process is controllable, and the Cu composite material is prepared 3 The interface effect of P/Cu improves the electronic structure of the material, thereby effectively improving the electrocatalytic reaction activity; and prepared Cu 3 The P/Cu material is in nano-ribbon distribution, is not easy to agglomerate and has high specific surface area.
In order to achieve the above purpose, the present application adopts the following technical scheme:
nano strip Cu 3 The preparation method of the P/Cu specifically comprises the following steps:
dispersing black phosphorus in an organic solvent under the anhydrous and anaerobic condition to obtain a mixed solution A;
ultrasonic stripping is carried out on the mixed solution A by utilizing a liquid phase stripping method, and then an upper layer solution is collected to obtain black phosphorus nano-sheet dispersion liquid;
carrying out hydrothermal reaction on the black phosphorus nano-sheet dispersion liquid subjected to ultrasonic stripping and copper acetylacetonate, cleaning, centrifuging and drying to obtain nano-ribbon Cu 3 P/Cu material.
Preferably, the organic solvent is N-methylpyrrolidone or N, N-dimethylformamide.
Preferably, black phosphorus is dispersed in an organic solvent under anhydrous and anaerobic conditions to obtain a mixed solution A, and the method comprises the following steps:
weighing black phosphorus in a glove box without water and oxygen;
placing the weighed black phosphorus in a closed container;
adding an organic solvent into a closed container to obtain a mixed solution.
Preferably, the dosage ratio of the black phosphorus to the organic solvent in the mixed solution is (1-2) mg:4mL.
Preferably, the reaction conditions for ultrasonic stripping of the mixed solution A by the liquid phase stripping method are as follows: the temperature is 3-7 ℃, and the ultrasonic treatment is carried out for 8-12 hours.
Preferably, the black phosphorus nanoplatelet dispersion is subjected to a hydrothermal reaction with copper acetylacetonate, comprising:
adding the black phosphorus nano-sheet dispersion liquid and copper acetylacetonate into a reaction kettle, introducing nitrogen gas, sealing, and performing hydrothermal reaction.
Preferably, the hydrothermal reaction conditions are: heating to 180-220 ℃ at the speed of 3-5 ℃/min, and preserving heat for 10-14 h.
Preferably, the product after the hydrothermal treatment is cooled, washed by a cleaning agent and centrifugally separated, and then dried to obtain the nano-ribbon Cu 3 P/Cu material.
Preferably, the drying condition is that the vacuum drying is carried out for 10-14 h at 55-65 ℃.
According to a first aspect of the present application, there is provided a nanoribbon Cu 3 The P/Cu material is prepared by adopting the preparation method; the Cu is 3 The P/Cu material presents a nano belt shape, the width of the nano belt is 180nm-220nm, the phosphide has high conductivity, and the interface effect at the interface of the composite material causes the change of the coordination mode at the interfaceCausing redistribution of the electronic structure at the interface.
The application has the following beneficial effects:
1. the black phosphorus is dispersed in an organic solvent under the anhydrous and anaerobic condition to obtain a mixed solution A; after ultrasonic stripping is carried out on the mixed solution A by utilizing a liquid phase stripping method, the stripped black phosphorus nano-sheet provides a nano-sheet template and a P source for a target product; carrying out hydrothermal reaction on the black phosphorus nano sheet dispersion liquid subjected to ultrasonic stripping and copper acetylacetonate; because the phosphorus has stronger binding capacity to metal ions, the phosphorus is easy to combine with Cu 2+ Forming Cu-P bond and Cu in hydrothermal process 3 P, then Cu in the reaction process 2+ With P in an organic solvent to form Cu, thereby forming Cu 3 P/Cu material realizes high-porosity composite Cu by controlling black phosphorus stripping conditions and hydrothermal reaction conditions 3 Preparation of P/Cu.
2. Cu synthesized by the present application 3 The P/Cu material presents a nano belt shape, the width of the nano belt is 180-220 nm, the thickness of the nano belt shape is thinner, and the catalytic reaction belongs to surface reaction, so that the exposure of the active site of the catalyst can be improved, the utilization rate of the active site of the catalyst is effectively improved, and the reaction activity is increased; in addition, the reaction process composite material Cu 3 The interface effect in P/Cu improves the electronic structure of the material, thereby effectively improving the electrocatalytic reaction activity. That is, due to Cu 3 The existence of P/Cu interface, the coordination mode at the interface is different from that of the bulk materials, so the electronic structure at the interface is different from that of the bulk materials, and the existence of heterojunction interface is also considered as an important means for improving the activity of the catalyst.
3. The method provides a reaction template and a P source based on stripped BP, and the generated target product has the characteristic of controllable morphology, thereby being a safe and environment-friendly synthesis method. The shape of the nano belt is favorable for full exposure of active sites, the effective utilization rate of the materials is increased, meanwhile, the interface effect of the two materials in the generation process can improve the coordination environment of a single material, the electronic structure of a target material is regulated, and the intrinsic activity of the active sites is improved.
Description of the drawings:
the accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:
FIG. 1 shows Cu prepared in example one 3 High angle annular dark field scanning transmission electron microscopy (HAADF-STEM) images of P/Cu material;
FIG. 2 is a Cu film prepared according to example one 3 Cu element distribution diagram of the P/Cu material;
FIG. 3 is a Cu film prepared according to example one 3 P element distribution diagram of P/Cu material;
FIG. 4 shows Cu prepared in example one 3 XRD pattern of P/Cu material;
FIG. 5 is a High Resolution Transmission (HRTEM) diagram of a Cu3P/Cu material with nanoribbon structures prepared.
Detailed Description
In order to make the technical solutions and advantages of the embodiments of the present application more apparent, the following detailed description of exemplary embodiments of the present application is given with reference to the accompanying drawings, and it is apparent that the described embodiments are only some of the embodiments of the present application and not exhaustive of all the embodiments. It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other.
Example 1
(1) 20mg of Black Phosphorus (BP) was weighed into a 50mL centrifuge tube in a glove box free of aqueous oxygen, and 40mL of N-methylpyrrolidone (NMP) was added to the centrifuge tube; air and water should be avoided in the mixing process of the black phosphorus and the N-methyl pyrrolidone to prevent the black phosphorus from being oxidized, and the mixture is sealed and taken out of the glove box after being mixed.
(2) Placing the sample prepared in the step (1) into ultrasonic waves for stripping by utilizing a liquid phase stripping method, maintaining the temperature at 5 ℃, carrying out ultrasonic treatment for 10 hours, centrifuging at 2000/min, and collecting an upper solution to obtain black phosphorus nano-sheet dispersion liquid with smaller particle size; the surface energy of black phosphorus is improved through ultrasonic stripping; is favorable for subsequent hydrothermal reaction.
(3) 1mmol of ethyl is weighedAdding copper acetylacetonate into a 50ml reaction kettle, adding the black phosphorus nanosheet dispersion liquid obtained in the step (2) into the reaction kettle, introducing nitrogen for 30min, and sealing. Carrying out a hydrothermal reaction under the following conditions: heating to 200 ℃ at the speed of 3 ℃/min, and preserving heat for 12 hours to obtain Cu 3 P/Cu。
(4) Cooling to room temperature, directly transferring to centrifuge tube, centrifuging at 10000r/min, removing supernatant, adding N-methylpyrrolidone NMP, centrifuging at the same speed for 3 times, vacuum drying at 60deg.C for 12 hr to obtain nanometer strip Cu 3 P/Cu target material.
Example two
(1) 10mg of Black Phosphorus (BP) was weighed into a 50mL centrifuge tube in a glove box free of aqueous oxygen, and 40mL of N-methylpyrrolidone (NMP) was added to the centrifuge tube; air and water should be avoided in the mixing process of the black phosphorus and the N-methyl pyrrolidone to prevent the black phosphorus from being oxidized, and the mixture is sealed and taken out of the glove box after being mixed.
(2) Placing the sample prepared in the step (1) into ultrasonic waves for stripping by utilizing a liquid phase stripping method, maintaining the temperature at 5 ℃, carrying out ultrasonic treatment for 10 hours, centrifuging at 2000/min, and collecting an upper solution to obtain black phosphorus nano-sheet dispersion liquid with smaller particle size; the surface energy of black phosphorus is improved through ultrasonic stripping; is favorable for subsequent hydrothermal reaction.
(3) 1mmol of copper acetylacetonate is weighed, added into a 50ml reaction kettle, and the black phosphorus nano-sheet dispersion liquid obtained in the step (2) is added into the reaction kettle, nitrogen is introduced for 30min, and the reaction kettle is sealed. Carrying out a hydrothermal reaction under the following conditions: heating to 200 ℃ at the speed of 3 ℃/min, and preserving heat for 12 hours to obtain Cu 3 P/Cu。
Cooling to room temperature, directly transferring to centrifuge tube, centrifuging at 10000r/min, removing supernatant, adding N-methylpyrrolidone NMP, centrifuging at the same speed for 3 times, vacuum drying at 60deg.C for 12 hr to obtain nanometer strip Cu 3 P/Cu target material.
Example III
(1) 15mg of Black Phosphorus (BP) was weighed into a 50mL centrifuge tube in a glove box free of aqueous oxygen, and 40mL of N-methylpyrrolidone (NMP) was added to the centrifuge tube; air and water should be avoided in the mixing process of the black phosphorus and the N-methyl pyrrolidone to prevent the black phosphorus from being oxidized, and the mixture is sealed and taken out of the glove box after being mixed.
(2) Placing the sample prepared in the step (1) into ultrasonic waves for stripping by utilizing a liquid phase stripping method, maintaining the temperature at 5 ℃, carrying out ultrasonic treatment for 10 hours, centrifuging at 2000/min, and collecting an upper solution to obtain black phosphorus nano-sheet dispersion liquid with smaller particle size; the surface energy of black phosphorus is improved through ultrasonic stripping; is favorable for subsequent hydrothermal reaction.
(3) 1mmol of copper acetylacetonate is weighed, added into a 50ml reaction kettle, and the black phosphorus nano-sheet dispersion liquid obtained in the step (2) is added into the reaction kettle, nitrogen is introduced for 30min, and the reaction kettle is sealed. Carrying out a hydrothermal reaction under the following conditions: heating to 200 ℃ at the speed of 3 ℃/min, and preserving heat for 12 hours to obtain Cu 3 P/Cu。
Cooling to room temperature, directly transferring to centrifuge tube, centrifuging at 10000r/min, removing supernatant, adding N-methylpyrrolidone NMP, centrifuging at the same speed for 3 times, vacuum drying at 60deg.C for 12 hr to obtain nanometer strip Cu 3 P/Cu target material.
FIG. 1 is a schematic diagram of a prepared nanoribbon structure Cu 3 HAADF-STEM diagram of P/Cu material; the figure shows that the material is in a nano-belt shape and is rich in pores, which is favorable for the exposure of active sites in the electrocatalytic reaction, the pores are favorable for the full contact with the reaction electrolyte, and the reaction mass transfer and charge transfer capacity is improved.
From FIGS. 2 and 3, cu can be seen 3 P/Cu is uniformly dispersed in a strip shape: nanoribbon structure Cu 3 And the Cu element of the P/Cu material is uniformly distributed and distributed with the P element. Specifically exfoliated BP nanoribbons as Cu 2+ In NMP solution containing BP, cu 2+ Forms Cu-P bond with BP surface, and forms Cu by nucleation and growth in hydrothermal process 3 P, then affected by the reaction temperature and reaction time, the content of phosphorus source and the air environment in the space of the reaction kettle, cu 2+ Reduction reaction in NMP to produce Cu, [ Cu ] 2+ -Cu 3 P(Cu + )-Cu]Form Cu 3 P/Cu nanobelts.
FIG. 4 is a schematic diagram of prepared nanoribbon Cu 3 XRD of P/Cu material, the prepared material is two-phase Cu 3 P/Cu, in combination with FIGS. 1, 2, 3, demonstrates a synthetic composite.
FIG. 5 is a schematic diagram of prepared nanoribbon Cu 3 The high-resolution transmission (HRTEM) diagram of the P/Cu material can obtain that Cu is respectively corresponding to the lattice spacing of 0.181nm and 0.200nm in the nano-belt structure 3 P and Cu phases, and the phases contain interfaces.
Based on the above, the embodiments of the present application realize high porosity composite Cu by controlling the time of black phosphorus stripping and the temperature of the hydrothermal reaction 3 P/Cu is prepared, the band width of the nano-band is about 200nm, the porosity and the shape of the nano-band can promote the mass transfer/charge process in the electrocatalytic process, and the composite material Cu 3 The interface effect in P/Cu improves the electronic structure of the material, thereby effectively improving the electrocatalytic reaction activity; in addition, by the scheme of the application, the nano Cu can be effectively avoided 3 P agglomeration phenomenon is generated; the method is simple and safe, and the process controllability is good.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present application without departing from the spirit or scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims and the equivalents thereof, the present application is intended to cover such modifications and variations.
Claims (10)
1. Nano strip Cu 3 The preparation method of the P/Cu is characterized by comprising the following steps:
dispersing black phosphorus in an organic solvent under the anhydrous and anaerobic condition to obtain a mixed solution A;
ultrasonic stripping is carried out on the mixed solution A by utilizing a liquid phase stripping method, and then an upper layer solution is collected to obtain black phosphorus nano-sheet dispersion liquid;
carrying out hydrothermal reaction on the black phosphorus nano-sheet dispersion liquid subjected to ultrasonic stripping and copper acetylacetonate, cleaning, centrifuging and drying to obtain nano-ribbon Cu 3 P/Cu material.
2. The method for preparing nano-ribbon Cu3P/Cu according to claim 1, wherein the organic solvent is N-methylpyrrolidone or N, N-dimethylformamide.
3. The nanoribbon Cu of claim 1 3 The preparation method of the P/Cu is characterized in that black phosphorus is dispersed in an organic solvent under the anhydrous and anaerobic condition to obtain a mixed solution A, and the preparation method comprises the following steps:
weighing black phosphorus in a glove box without water and oxygen;
placing the weighed black phosphorus in a closed container;
adding an organic solvent into a closed container to obtain a mixed solution.
4. The nanoribbon Cu of claim 3 3 The preparation method of the P/Cu is characterized in that the dosage ratio of the black phosphorus to the organic solvent in the mixed solution is (1-2) mg:4mL.
5. The nanoribbon Cu of claim 1 3 The preparation method of the P/Cu is characterized in that the reaction conditions for carrying out ultrasonic stripping on the mixed solution A by utilizing a liquid phase stripping method are as follows: the temperature is 3-7 ℃, and the ultrasonic treatment is carried out for 8-12 hours.
6. The nanoribbon Cu of claim 1 3 The preparation method of the P/Cu is characterized in that the hydro-thermal reaction of the black phosphorus nano-sheet dispersion liquid and the copper acetylacetonate is carried out, and the preparation method comprises the following steps:
adding the black phosphorus nano-sheet dispersion liquid and copper acetylacetonate into a reaction kettle, introducing nitrogen gas, sealing, and performing hydrothermal reaction.
7. The nanoribbon Cu of claim 6 3 The preparation method of the P/Cu is characterized in that the dosage ratio of the copper acetylacetonate to the black phosphorus-containing nano-sheet dispersion liquid is 1mmol:30ml; the hydrothermal reaction conditions are as follows: heating to 180-220 ℃ at the speed of 3-5 ℃/min, and preserving heat for 10-14 h.
8. The nanoribbon Cu of claim 1 3 The preparation method of P/Cu is characterized in that the product after the hydrothermal treatment is cooled, washed by a cleaning agent, centrifugally separated and dried to obtain nano strip Cu 3 P/Cu material.
9. The nanoribbon Cu of claim 8 3 The preparation method of the P/Cu is characterized in that the drying condition is that the vacuum drying is carried out for 10-14 h under the condition of 55-65 ℃.
10. Nano strip Cu 3 P/Cu material, characterized in that it is prepared by the preparation method according to any one of claims 1 to 9; the Cu is 3 The P/Cu material presents a nano belt shape, the width of the nano belt is 180nm-220nm, and the phosphide has high conductivity.
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| 尤凯熹 ; 范涛健 ; 葛颜绮 ; 张晗 ; .二维纳米材料黑磷的光电特性研究进展.物理学进展.2018,(04),第19-30页. * |
| 殷宪国 ; .黑磷复合材料制备与应用技术研究进展.磷肥与复肥.2020,(03),第22-27页. * |
| 秦莉 ; 李瑞瑞 ; 何汇洋 ; 姜珊珊 ; 张鹏 ; .黑磷纳米片的制备及降解特性评价.沈阳药科大学学报.2020,(05),第5-9页. * |
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