CN111719165B - Method for preparing Bi nanosheet by electrochemical stripping method - Google Patents
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Abstract
The invention discloses a method for preparing Bi nanosheets by an electrochemical stripping method, and belongs to the technical field of preparation of micro/nano materials. The invention adopts an electrochemical stripping method to prepare Bi nanosheets, Pt sheet electrodes are used as anodes, metal Bi blocks are used as cathodes, NaI solution is used as supporting electrolyte solution, and N is2Under protection, stripping the bulk metal Bi under the condition of 10-30V voltage. The prepared Bi nanosheet has high purity, and the CO is subjected to electrocatalytic reduction in a wider potential range2The Faraday efficiency of the formic acid can reach more than 94 percent, and the current density under lower electrolytic potential (-0.5V vs. RHE) can also reach 50mA/cm2The above. Compared with the Bi nanosheets prepared by a mechanical method, the Bi nanosheets with more uniform shapes and sizes and more surface active sites can be obtained more easily by an electrochemical stripping method, and the method is simple to operate, low in energy consumption, very economical and practical and has good industrial prospects.
Description
Technical Field
The invention relates to a method for preparing Bi nanosheets by an electrochemical stripping method, and belongs to the technical field of preparation of micro/nano materials.
Background
The low-cost and low-toxicity Bi is very potential reduction CO2Electrocatalyst for the production of formic acid, which is selective for CO2·-The intermediate shows a weak affinity for CO2Side reaction of RR-formation of H2The reaction of (HER) is inherently inert. Although the metal Bi electrocatalytic reduces CO2The selectivity of formic acid production is close to 100%, but the catalytic current density is not ideal. In order to further improve the Bi-based material in CO2The catalytic performance in the reduction reaction needs reasonable structural design and surface interface regulation and control on the material from the nanometer scale.
Bi and black phosphorus have similar layered crystal structures, each layer has a warped honeycomb-like structure, and the layers are supported by each other mainly through weak van der Waals force. Based on the structural characteristics of Bi, a proper method is selected to hopefully obtain the two-dimensional Bi nanosheet with the nanoscale thickness. At present, the traditional top-down mechanical stripping method or the bottom-up chemical synthesis method cannot be used for successfully preparing the single-layer or few-layer Bi nanosheets. It has been reported that the Bi nano-sheet is prepared by performing ultrasonic treatment on Bi powder in isopropanol solution added with a small amount of NaOH, but the process needs to be completed in a glove box, the preparation condition is harsh, the ultrasonic treatment time is as long as 30h, the Bi nano-sheet is easily oxidized by performing ultrasonic treatment under alkaline condition, the obtained product needs to be soaked in hydrazine hydrate for one night to remove a surface oxidation layer [ Wenjun Zhang, Yi Hu, Zhong Jin, et al, liquid-phase exposed ultra-thin Bi nano-sheets: (inorganic composites of enhanced electrochemical CO nano-catalytic)2 reduction on two-dimensional metal nanostructure[J].Nano Energy,2018,53:808-816]。
The electrochemical stripping method is based on that under the condition that an electrolyte solution is electrified, specific ions can be inserted into the layers of the layered two-dimensional material due to the directional migration of the ions, and the expansion separation of the layers is realized under the action of bubbles generated by an electrode, so that the required two-dimensional nano material is stripped. A great number of reports have been made on the preparation of graphene, phospholene and transition metal disulfur compounds by electrochemical exfoliation [ Sheng Yang, Panpan Zhang, Xinliang Feng, et al. Graphite is a precursor of a two-dimensional material, the most researches are carried out at present, and metal Bi is a two-dimensional layered material similar to the graphite, but the melting point of the metal Bi is low (271.3 ℃), and the metal Bi cannot stably exist in an acid-base solution and an oxygen-containing atmosphere, so that the direct synthesis of the metal Bi with the nano structure is difficult to realize.
Disclosure of Invention
[ problem ] to
The traditional top-down mechanical stripping method or the bottom-up chemical synthesis method cannot be used for successfully preparing the single-layer or few-layer Bi nano-sheet. It has been reported that the Bi nanosheet can be prepared by performing ultrasonic treatment on Bi powder in an isopropanol solution added with a small amount of NaOH, but the preparation process needs to be completed in a glove box, the preparation condition is harsh, the ultrasonic treatment time is as long as 30 hours, the Bi nanosheet is easily oxidized by performing ultrasonic treatment under an alkaline condition, and the obtained product needs to be soaked in hydrazine hydrate overnight to remove a surface oxide layer. Therefore, it is necessary to search for a simple method for producing Bi nanosheets.
[ solution ]
Aiming at the problems, the invention provides a method for preparing Bi nanosheets by an electrochemical stripping method by combining the inherent layered structure and the chemical activity of metal Bi and other characteristics, and the invention is applied to N2Under protection, electrochemical stripping is carried out on the bulk metal Bi under the condition of normal pressure and oxygen content by taking the reductive NaI solution as a supporting electrolyte solution, and the prepared Bi nanosheet is high in purity.
The invention provides a method for preparing Bi nanosheets by an electrochemical stripping method, which uses a cheap and low-toxicity metal Bi block as a cathode, and is electrified and subjected to N2Under the protection of (3), the preparation of the Bi nano-sheet under the condition of normal pressure and oxygen is realized in the NaI electrolyte solution.
In one embodiment of the invention, the method for preparing Bi nanosheets by electrochemical stripping comprises the following steps:
(1) taking H-Cell as a reaction vessel, and adding NaI solution as supporting electrolyte solution into cathode and anode electrolytic cells of the H-Cell;
(2) using a metal Bi block as a cathode, a Pt sheet electrode as an anode and in N2Carrying out electrifying reaction under protection;
(3) and (3) separating and washing the precipitate obtained in the cathode electrolytic cell in the step (2), and drying in vacuum to obtain the Bi nanosheet.
In one embodiment of the present invention, the concentration of the NaI solution in the step (1) is 0.5 to 1.0 mol.L-1。
In one embodiment of the present invention, the size of the metal Bi block in the step (2) is 3 to 5mm3The purity is more than 99.99 percent.
In one embodiment of the present invention, the catholyte solution is required to be electrified for 15-30 min N before the step (2) is electrified2To drive out dissolved oxygen in the solution.
In one embodiment of the present invention, the energization condition in the step (2) is: the DC stabilized power supply provides 10-30V voltage.
In one embodiment of the present invention, the energization time in the step (2) is 2 to 5 hours.
In one embodiment of the present invention, the N is required to be continuously turned on during the power-on process in the step (2)2And carrying out air isolation protection.
In one embodiment of the present invention, the separation method in step (3) is vacuum filtration using a vacuum filter.
In one embodiment of the present invention, the washing method in step (3) is washing with ultrapure water for 2-5 times.
In one embodiment of the invention, the drying method in the step (3) is drying in an electric heating vacuum oven at 60-80 ℃ for 4-6 h.
In one embodiment of the invention, the method for preparing Bi nanosheets by electrochemical stripping comprises the following steps:
(1) preparing 0.5-1.0 mol.L-1N of (A)aI solution;
(2) 50mL of NaI solution as a supporting electrolyte solution was added to each of 100mLH-Cell cathode and anode electrolytic cells, and 20min N was passed through the cathode electrolytic Cell2；
(3) Taking a metal Bi block with the purity of 99.99 percent as a cathode, taking a Pt sheet electrode as an anode, providing 10-30V voltage by a direct current stabilized voltage power supply, and continuously maintaining N in a cathode electrolytic cell in the electrifying process2The airflow is protected by isolating air;
(4) and electrifying for 2-5 h, then carrying out vacuum filtration on the solution in the cathode electrolytic cell, fully washing the product with ultrapure water, collecting the product, and drying the product in an electrothermal vacuum drying oven at the temperature of 60-80 ℃ for 4-6 h to obtain the Bi nanosheet.
The invention provides a Bi nanosheet prepared by the method.
The invention provides the application of the Bi nanosheet in electrocatalytic reduction of CO2Application in the reaction of preparing formic acid.
[ advantageous effects ]:
(1) the preparation method adopts an electrochemical stripping method to prepare the Bi nanosheets in an oxygen-containing atmosphere at normal pressure, and takes the metal Bi blocks as a cathode and the reductive NaI solution as a supporting electrolyte solution. The specific reaction principle is as follows: a large amount of Na in the electrolyte solution under the condition of electrification+Will intercalate into the interlayer of cathode metal Bi to increase the interlayer spacing of Bi and reduce the interlayer force, and H generated by the cathode2The explosion of the bubble can gradually strip the Bi nano-sheets from the bulk metal Bi. In order to prevent the stripped Bi nanosheets from being oxidized, a NaI solution with reducibility is selected as an electrolyte solution and is added in N2The preparation of the Bi nanosheets is carried out under protection, and the preparation method is simple to operate, low in energy consumption, economical and practical and has good industrial prospect.
(2) The Bi nanosheet prepared by the method has high purity, and the CO is subjected to electrocatalytic reduction in a wider potential range2The Faraday efficiencies of the formic acid preparation can reach more than 94 percent, and the current density under lower electrolytic potential (-0.5V vs. RHE) can also reach 50mA/cm2The above. Compared with Bi nanosheets prepared by a mechanical method, the morphology and the scale are easier to obtain by an electrochemical stripping methodThe size of the Bi nanosheet is more uniform, and the surface active sites are more.
Drawings
Fig. 1 is an XRD spectrum of the Bi nanoplate prepared in example 1.
Fig. 2 is an AFM photograph of the Bi nanoplates prepared in example 1.
FIG. 3 shows the Bi nanosheets prepared in example 1 being used for electrocatalytic reduction of CO2The Faraday efficiency and the current density change with the potential.
FIG. 4 shows Bi prepared in comparative example 14O5Br2XRD pattern of nanocrystals.
FIG. 5 shows Bi prepared in comparative example 22O3XRD pattern of nanocrystals.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
[ example 1 ]
(1) 50mL of 0.5 mol. L was added to each of the cathode and anode electrolytic cells of H-Cell (100mL standard)-1And introducing N into the cathode electrolytic cell for 20min2；
(2) In a size of 5mm399.99% purity metal Bi block as cathode, Pt sheet electrode as anode, DC regulated power supply providing 15V voltage, and continuously introducing N into cathode electrolytic cell during energization2；
(3) And electrifying for 2h, then performing vacuum filtration on the solution in the cathode electrolytic cell by using a vacuum filter, fully cleaning the precipitate by using ultrapure water, collecting the product, and drying the product in an electrothermal vacuum drying oven at the temperature of 80 ℃ for 4h to obtain the Bi nanosheet.
Characterization test:
XRD (X-ray diffraction) tests are carried out on the Bi nanosheets prepared in the embodiment, fig. 1 is an XRD (X-ray diffraction) map of the Bi nanosheets prepared in the embodiment, and PDF (Portable document Format) card comparison proves that the prepared products are Bi, and meanwhile, the prepared products are low in impurity peaks, high in purity, high in crystallinity and obvious in orientation growth.
Microstructure observation is carried out on the Bi nanosheets prepared in the embodiment by an Atomic Force Microscope (AFM), FIG. 2 is an AFM photograph of the Bi nanosheets prepared in the embodiment, and it can be seen from the image that the product is a nanosheet structure, the dispersibility of the Bi nanosheets is good, and the average thickness of the prepared Bi nanosheets is about 5.5 nm.
[ example 2 ]
(1) 50mL of 1.0 mol. L was added to each of the cathode and anode electrolytic cells of H-Cell (100mL standard)-1NaI solution is introduced into the cathode electrolytic cell for 20min2；
(2) In a size of 5mm399.99% purity metal Bi block as cathode, Pt sheet electrode as anode, DC regulated power supply providing 30V voltage, and continuously introducing N into cathode electrolytic cell during electrification2；
(3) And electrifying for 3h, then carrying out vacuum filtration on the solution in the cathode electrolytic cell by using a vacuum filter, fully cleaning the precipitate by using ultrapure water, collecting the product, and drying the product in an electrothermal vacuum drying oven at 60 ℃ for 6h to obtain the Bi nanosheet.
[ example 3 ]
(1) 50mL of 0.7 mol. L was added to each of the cathode and anode electrolytic cells of H-Cell (100mL standard)-1And introducing N into the cathode electrolytic cell for 20min2；
(2) In a size of 5mm399.99% purity metal Bi block as cathode, Pt sheet electrode as anode, DC regulated power supply providing 10V voltage, and continuously introducing N into cathode electrolytic cell during electrification2；
(3) And electrifying for 4h, then carrying out vacuum filtration on the solution in the cathode electrolytic cell by using a vacuum filter, fully cleaning the precipitate by using ultrapure water, collecting the product, and drying the product in an electrothermal vacuum drying oven at 70 ℃ for 5h to obtain the Bi nanosheet.
[ example 4 ]
(1) 50mL of 0.9 mol. L was added to each of the cathode and anode electrolytic cells of H-Cell (100mL standard)-1And introducing N into the cathode electrolytic cell for 20min2；
(2) In a size of 5mm399.99% pure metal Bi block as cathodeThe Pt electrode is used as an anode, a DC stabilized voltage supply provides 25V voltage, and N is continuously introduced into the cathode electrolytic cell in the electrifying process2；
(3) And electrifying for 3h, then carrying out vacuum filtration on the solution in the cathode electrolytic cell by using a vacuum filter, fully cleaning the precipitate by using ultrapure water, collecting the product, and drying the product in an electrothermal vacuum drying oven at 60 ℃ for 6h to obtain the Bi nanosheet.
[ example 5 ]
(1) 50mL of 0.5 mol. L was added to each of the cathode and anode electrolytic cells of H-Cell (100mL standard)-1And introducing N into the cathode electrolytic cell for 20min2；
(2) In a size of 5mm399.99% purity metal Bi block as cathode, Pt sheet electrode as anode, DC regulated power supply providing 20V voltage, and continuously introducing N into cathode electrolytic cell during electrification2；
(3) And electrifying for 4h, then carrying out vacuum filtration on the solution in the cathode electrolytic cell by using a vacuum filter, fully cleaning the precipitate by using ultrapure water, collecting the product, and drying the product in an electrothermal vacuum drying oven at 60 ℃ for 6h to obtain the Bi nanosheet.
[ example 6 ] electrocatalytic reduction of CO2Preparation of formic acid
Electrocatalytic reduction of CO in Flow-Cell using samples prepared in example 12The preparation of HCOOH comprises the following specific processes: adding 10mg of Bi nano-sheets into a mixed solvent containing 50 mu L of 5% Nafion solution and 950 mu L of ethanol, performing ultrasonic treatment for 1h to prepare a catalyst dispersion liquid for later use, and loading a catalyst on hydrophobic carbon paper serving as a substrate, wherein the loading amount of the catalyst is about 1mg/cm2，CO2Flow rate of 45sccm, 1M KOH as electrolyte solution, electrolyte flow rate of 10mL/min, gas product (H)2CO) is detected by a gas chromatograph, a liquid product (HCOOH) is detected by a nuclear magnetic resonance spectrometer, the analysis of the applied potential and current density in the electrolysis process is completed by an electrochemical workstation, and the Faraday efficiency and the corresponding current density of the formic acid obtained by electrolysis are shown in figure 3 along with the variation trend of the electrolysis potential. From the results, it is clear that at a relatively low potential (C:)<0.8V vs. RHE), the Faraday efficiency of the formic acid can reach 98 percent, and the current density of the formic acid can reach 0.8V vs. RHEThe degree can reach 135mA/cm2。
Comparative example 1
(1) 50mL of 0.5 mol. L was added to each of the cathode and anode electrolytic cells of H-Cell (100mL standard)-1And introducing N into the cathode electrolytic cell for 20min2；
(2) In a size of 5mm399.99% purity metal Bi block as cathode, Pt sheet electrode as anode, DC regulated power supply providing 15V voltage, and continuously introducing N into cathode electrolytic cell during energization2；
(3) Electrifying for 2h, vacuum filtering the solution in the cathode electrolytic cell with a vacuum filter, fully cleaning the precipitate with ultrapure water, collecting the product, and drying in an electrothermal vacuum drying oven at 80 ℃ for 4h to obtain Bi4O5Br2And (4) nanocrystals.
Bi prepared for the comparative example4O5Br2XRD test of the nanocrystals, and FIG. 4 shows Bi prepared in this comparative example4O5Br2The XRD pattern of the nano-crystal is proved to be Bi by PDF card comparison4O5Br2But not Bi nanocrystals.
Comparative example 2
(1) 50mL of 0.5 mol. L was added to each of the cathode and anode electrolytic cells of H-Cell (100mL standard)-1NaOH solution and introducing N into the cathode electrolytic cell for 20min2；
(2) In a size of 5mm399.99% purity metal Bi block as cathode, Pt sheet electrode as anode, DC regulated power supply providing 15V voltage, and continuously introducing N into cathode electrolytic cell during energization2；
(3) Electrifying for 2h, vacuum filtering the solution in the cathode electrolytic cell with a vacuum filter, fully cleaning the precipitate with ultrapure water, collecting the product, and drying in an electrothermal vacuum drying oven at 80 ℃ for 4h to obtain Bi2O3And (4) nanocrystals.
Bi prepared for the comparative example2O3XRD test of the nanocrystals, and FIG. 5 shows Bi prepared in this comparative example2O3XRD (X-ray diffraction) spectrum of nanocrystalline is verified through PDF (Portable document Format) card comparisonIt is clear that the product prepared is Bi2O3But not Bi nanocrystals.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. The method for preparing the Bi nanosheets by the electrochemical stripping method is characterized in that a metal Bi block is used as a cathode, and the metal Bi block is electrified and N is added2Under the protection of (3), a Pt sheet electrode is used as an anode, and the preparation of the Bi nanosheet is realized in a NaI electrolyte solution.
2. The method according to claim 1, comprising in particular the steps of:
(1) taking H-Cell as a reaction vessel, and adding NaI solution as supporting electrolyte solution into cathode and anode electrolytic cells of the H-Cell;
(2) using a metal Bi block as a cathode, a Pt sheet electrode as an anode and in N2Carrying out electrifying reaction under protection;
(3) and (3) separating and washing the precipitate obtained in the cathode electrolytic cell in the step (2), and drying in vacuum to obtain the Bi nanosheet.
3. The method according to claim 2, wherein the concentration of the NaI solution in the step (1) is 0.5 to 1.0 mol-L-1。
4. The method according to claim 2, wherein the size of the metallic Bi block in the step (2) is 3 to 5mm3And the purity is more than 99.99 percent.
5. The method according to claim 2, wherein the catholyte solution is heated for 15 to 30min N before the step (2) of heating2To drive out dissolved oxygen in the solution.
6. The production method according to claim 2, wherein the energization condition in the step (2) is: the DC stabilized power supply provides 10-30V voltage.
7. The preparation method according to claim 2, wherein the time for electrifying in the step (2) is 2-5 h.
8. The preparation method of claim 2, wherein the drying method in the step (3) is drying in an electric heating vacuum oven at 60-80 ℃ for 4-6 h.
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| CN113638004B (en) * | 2021-08-09 | 2022-07-26 | 山东师范大学 | Preparation method and application of bimetallic catalyst |
| CN114672831B (en) * | 2022-04-29 | 2023-05-09 | 华中科技大学 | Atomic-level-thickness two-dimensional bismuth nanosheet material and preparation method and application thereof |
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