CN111197173B - Electroplating preparation method of non-noble metal single-atom-doped two-dimensional material - Google Patents
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Abstract
The invention belongs to the technical field of two-dimensional material preparation, and particularly relates to an electroplating preparation method of a non-noble metal-doped two-dimensional material. The method comprises the following specific steps: preparing an electrode containing a single layer or a few layers of two-dimensional materials; preparing a non-noble metal doped two-dimensional material by an electroplating method: the electroplating system is a three-electrode system, a graphite rod is used as an anode, a two-dimensional material is used as a cathode, and saturated calomel is used as a reference electrode; the electrolyte is saturated transition metal hydroxide solution, and the concentration range of free metal ions in the system is controlled within 10 by adjusting the pH value range of the solution‑10~10‑6g/ml; and (3) preparing the two-dimensional materials with different doping concentrations by electrodeposition for 0.1-24 hours. The method is simple and easy to implement, the reaction can be carried out at room temperature, the species and the concentration of the doped ions can be accurately adjusted, and the prepared non-noble metal doped two-dimensional material has higher electro-catalytic hydrogen evolution and electro-catalytic carbon dioxide reduction performance.
Description
Technical Field
The invention belongs to the technical field of two-dimensional material preparation, and particularly relates to an electroplating preparation method of a monoatomic-doped two-dimensional material.
Background
Molybdenum disulfide has good catalytic activity in electrocatalytic hydrogen evolution electrocatalytic reactions, but is limited by the defects of poor active site density, poor reaction activity, poor electric transport and the like. Increasing the number of active sites, increasing the site activity of the material and increasing the conductivity of the material are important methods for increasing its catalytic performance. The introduction of the heteroatom can regulate the activity of the active site, increase the number of the active sites or improve the conductivity of the material.
The transition metal as a doping atom can regulate the electrocatalytic performance of the two-dimensional material, and can obviously improve the electrocatalytic hydrogen evolution and electrocatalytic carbon dioxide reduction performance of the two-dimensional material. The method for preparing transition metal doped two-dimensional materials commonly used at present mainly comprises two major categories, namely a direct synthesis method, wherein a precursor containing doping elements is added in the synthesis process, and the transition metal doped two-dimensional materials are directly prepared by a one-step method, specifically comprising a hydrothermal method, a solvothermal method, a chemical vapor deposition method and the like; the other is a post-processing method, and doping modification is carried out on the prepared two-dimensional material, and the method comprises an ion implantation method, a coprecipitation method and the like. The existing direct synthesis and post-treatment methods can not control the doping site and concentration and need higher reaction temperature.
The electroplating method is also used for preparing transition metal doped two-dimensional materials at present, but because the reduction potential of most metal ions is lower, nano particles or metal films are formed on the surfaces of the materials by low-potential short-time reduction under the concentration of conventional electrolyte.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides an electroplating preparation method of a simple-process, accurate and controllable single-atom-doped two-dimensional material, wherein the prepared two-dimensional material has no nano-particle deposition and has higher electro-catalytic performance.
The invention provides an electroplating preparation method of a monatomic doped two-dimensional material, which comprises the following specific steps:
(1) preparing a two-dimensional material electrode by adopting a direct growth or transfer method;
(2) then preparing a non-noble metal doped two-dimensional material by adopting an electroplating method: a three-electrode system is adopted, a two-dimensional material is used as a working electrode, a graphite rod is used as a counter electrode, and saturated calomel is used as a reference electrode; the electrolyte is a saturated non-noble metal hydroxide aqueous solution, the pH of the system is adjusted to 9-14, and the concentration of free metal ions in the system is controlled to be 10-10~10-6g/ml; carrying out electrodeposition under magnetic stirring by adopting a chronopotentiometry (0 to-1V vs. RHE) and a cyclic voltammetry (0 to-1V vs. RHE), wherein the electrodeposition time is 0.1-24 h;
(3) and after the electroplating is finished, the two-dimensional material electrode is washed by deionized water and dried by nitrogen.
Then, characterization and catalytic performance test are carried out.
In the invention, the two-dimensional material is transition metal chalcogenide (TMD), nitrogen-doped reduced graphene oxide (NRGO) or transition metal carbon family compound (MXene).
In the present invention, the transition metal chalcogenide is MX2Wherein M is Ti, Zr, Hf, V, Nb, Ta, Mo, W, Re or Pt; x is S, Se or Te; the transition metal carbon family compound MXene, wherein M is Mo, Ti, V, Nb or Ta.
In the invention, the two-dimensional material electrode is prepared by adopting a liquid phase stripping, mechanical stripping or chemical vapor deposition method.
In the invention, the non-noble metal is Fe, Co, Ni, Cu or Zn.
In the invention, the electrolyte adopts a saturated non-noble metal hydroxide solution; carrying out electrodeposition under magnetic stirring, and controlling the magnetic stirring speed to be 100-600 r/min.
In the invention, in the reaction system, the metal hydroxide precipitate and the two-dimensional material electrode are isolated by filter paper, ion semipermeable membrane or other modes.
The invention relates to the preparation of monoatomic doped two-dimensional materials by means of electrochemical deposition, based on the principle that metal hydroxides (such as cobalt hydroxide) are sparingly soluble in water, according to which KspThe concentration of free cobalt ions in the saturated aqueous solution of cobalt hydroxide was calculated to be 4.2X 10-6mol/L, the concentration of free cobalt ions can be adjusted and controlled to reach the concentration range (10) required by the single-atom electroplating by controlling the pH of the system-10~10-6g/ml), and then applying a reduction potential on the surface of the two-dimensional material to prepare the monoatomic doped two-dimensional material.
Compared with the prior art, the invention has the beneficial effects that:
(1) the electroplating method is adopted, the required equipment is simple, and only an electrochemical workstation or a common direct-current power supply is needed;
(2) the method is different from a coprecipitation method and an impregnation method in that the reaction temperature is room temperature, and no additional temperature is needed;
(3) the preparation process is simple, and the monoatomic doped two-dimensional material can be prepared in situ. The new method for preparing the monatomic doped two-dimensional material is applied to the large-scale preparation of the monatomic doped electro-catalytic material and the expansion of electronic devices of the monatomic doped two-dimensional material.
Drawings
FIG. 1 is a schematic diagram of an apparatus for electroplating to prepare a monatomic Co-doped NRGO. The H-shaped reaction tank is used for electroplating reaction, and filter paper is used as a diaphragm in the middle.
FIG. 2 is Co 2p of Co-NRGO3/2X-ray photoelectron spectroscopy.
In FIG. 3, (a) is a transmission electron microscope image of Co-NRGO with a 50 nm scale; (b) is a transmission electron microscope image of Co-NRGO with a scale of 5 nm.
FIG. 4, (a-d) HAADF-STEM images and corresponding EDX images of Co-NRGO, (b) element C; (c) n element; (d) co element; the scale is 20 nm.
FIG. 5 is a polarization curve for NRGO and Co-NRGO.
FIG. 6 (a) Faraday efficiencies FE of NRGO and Co-NRGO CO at different operating potentialsCOCurrent densities for NRGO and Co-NRGO at different potentials to produce CO; (c) the yield of reduced NRGO and Co-NRGO to CO at different potentials.
FIG. 7 is a schematic diagram of the method of the present invention.
Detailed Description
The invention is further elucidated with reference to the drawing.
Example 1: preparation of monatomic Co-doped MoS by electroplating method2
First, take 4 mg/ml MoS2NMP was subjected to ultrasonic stripping for 8 hours at an ultrasonic power of 150W; centrifuging at 5000 r/min, and electrophoresing MoS2Electrophoresis is carried out to the surface of graphite paper to prepare MoS2a/GP electrode;
secondly, the electrolyte is saturated cobalt hydroxide aqueous solution, and the pH is adjusted to 11.24; in a three-electrode system, a graphite rod is used as a counter electrode, saturated calomel is used as a reference electrode, and MoS2the/GP acts as the working electrode. Carrying out electrochemical deposition for 12 hours when the cathode potential is-0.38V (vs. RHE), wherein the magnetic stirring speed is 300 r/min;
thirdly, taking out the working electrode after the electrodeposition is finished,flushing with deionized water and blowing with nitrogen to obtain monatomic Co-doped MoS2；
Fourthly, the prepared material is characterized, and the single-atom Co-doped MoS is shown by means of an annular dark field-scanning transmission electron microscope, an X-ray photoelectron spectrometer and the like2Successful preparation;
and fifthly, testing the electrocatalytic performance of the material. The results show that MoS is doped by monoatomic Co2The electrocatalytic hydrogen evolution performance is obviously improved.
Example 2: preparation of monatomic Co-doped NRGO by electroplating method
Firstly, preparing nitrogen-doped reduced graphene oxide. Graphene Oxide (GO) solution is subjected to freeze drying to obtain graphene oxide powder, and then ammonia heat treatment is carried out at 500 ℃ to obtain nitrogen-doped reduced graphene oxide (NRGO). 4 mg of NRGO was dispersed in 2 ml (DMF: EtOH = v 1:1) of the mixed solution, and 80. mu.L of Nafion solution was added for sonication. 100 μ L of the dispersion was dropped on a 1 cm circle2Graphite paper surface to obtain 0.2 mg/cm2A loading amount of an electrode;
and secondly, preparing the non-noble metal doped nitrogen-doped reduced graphene oxide. The electrolyte is saturated cobalt hydroxide aqueous solution, and the pH is adjusted to 11.24; in the three-electrode system, a graphite rod is used as a counter electrode, saturated calomel is used as a reference electrode, and NRGO/GP is used as a working electrode (figure 1). Carrying out electrochemical deposition for 12 hours when the cathode potential is-0.38V (vs. RHE), wherein the magnetic stirring speed is 300 r/min;
thirdly, taking out the working electrode after the electrodeposition is finished, washing the working electrode by using deionized water, and drying the working electrode by using nitrogen to obtain the monatomic Co-doped NRGO;
fourthly, characterizing the prepared material, and showing the successful preparation of the monatomic Co-doped NRGO by an annular dark field-scanning transmission electron microscope and an X-ray photoelectron spectrometer (figures 3 and 4), wherein the doping concentration of the monatomic Co can reach 1.1 at.% (figure 2);
and fifthly, testing the electrocatalytic performance of the material. The results show that the electrocatalytic hydrogen evolution performance of the NRGO is significantly improved and the electrocatalytic carbon dioxide reduction performance is improved by the monoatomic Co doping (fig. 5 and 6).
Example 3: preparation of monatomic Fe-doped NRGO by electroplating method
Firstly, preparing nitrogen-doped reduced graphene oxide. 4 mg of NRGO was dispersed in 2 ml (DMF: EtOH = v 1:1) of the mixed solution, and 80. mu.L of Nafion solution was added for sonication. 100 μ L of the dispersion was dropped on a 1 cm circle2Graphite paper surface to obtain 0.2 mg/cm2A loading amount of an electrode;
and secondly, preparing the non-noble metal doped nitrogen-doped reduced graphene oxide. The electrolyte is a saturated ferrous hydroxide aqueous solution, and the pH is adjusted to 12; in the three-electrode system, a graphite rod is used as a counter electrode, saturated calomel is used as a reference electrode, and NRGO/GP is used as a working electrode. Carrying out electrochemical deposition for 1 hour when the cathode potential is-1V (vs. RHE), wherein the magnetic stirring speed is 300 r/min;
thirdly, taking out the working electrode after the electrodeposition is finished, washing the working electrode by using deionized water, and drying the working electrode by using nitrogen to obtain the monatomic Fe-doped NRGO;
fourthly, characterizing the prepared material, and showing the successful preparation of the single-atom Fe-doped NRGO by an annular dark field-scanning transmission electron microscope and an X-ray photoelectron spectrometer;
and fifthly, testing the electrocatalytic performance of the material. The result shows that the electrocatalytic hydrogen evolution performance of the NRGO is remarkably improved and the electrocatalytic carbon dioxide reduction performance is improved by doping with the monatomic Fe.
Claims (6)
1. A non-noble metal single-atom-doped two-dimensional material electroplating preparation method is characterized by comprising the following specific steps:
(1) preparing a two-dimensional material electrode by adopting a direct growth or transfer method;
(2) then preparing a non-noble metal doped two-dimensional material by adopting an electroplating method: a three-electrode system is adopted, a two-dimensional material is used as a working electrode, a graphite rod is used as a counter electrode, and saturated calomel is used as a reference electrode; the electrolyte uses a saturated non-noble metal hydroxide aqueous solution, the pH of the system is adjusted to 9-14,the concentration of free metal ions in the system is controlled to be 10-10~10-6g/ml; performing electrodeposition under magnetic stirring by adopting a chronopotentiometry or cyclic voltammetry, wherein the electrodeposition time is 0.1-24 h;
the non-noble metal is Fe, Co, Ni, Cu or Zn, wherein Fe is Fe (OH)2；
(3) And after the electroplating is finished, the two-dimensional material electrode is washed by deionized water and dried by nitrogen.
2. The method for preparing a non-noble metal monoatomic doped two-dimensional material according to claim 1, wherein the two-dimensional material is transition metal chalcogenide (TMD), nitrogen-doped reduced graphene oxide (NRGO) or transition metal carbon group compound (MXene).
3. The method of claim 2, wherein the transition metal chalcogenide is MX2Wherein M is Ti, Zr, Hf, V, Nb, Ta, Mo, W, Re or Pt; x is S, Se or Te; the transition metal carbon family compound MXene, wherein M is Mo, Ti, V, Nb or Ta.
4. The method of claim 1, wherein the metal hydroxide is cobalt hydroxide.
5. The method for preparing a non-noble metal monoatomic doped two-dimensional material according to claim 1, wherein the magnetic stirring speed is controlled to be 100 to 600 r/min.
6. The method for preparing the non-noble metal monatomic doped two-dimensional material by electroplating according to claim 1, wherein the metal hydroxide precipitate and the two-dimensional material electrode are isolated by means of filter paper or an ionic semipermeable membrane in the reaction system.
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| CN112774697B (en) * | 2020-09-07 | 2022-09-23 | 南京大学 | Monoatomic metal-molybdenum sulfide nano-composite and preparation method and application thereof |
| CN113394381B (en) * | 2021-06-10 | 2023-02-10 | 肇庆市华师大光电产业研究院 | Preparation method of layered double hydroxide composite material for positive electrode of lithium-sulfur battery |
| CN114457371B (en) * | 2021-11-05 | 2022-12-20 | 天津师范大学 | MXene loaded Ni nano-particle composite hydrogen evolution electrocatalyst and preparation method and application thereof |
| CN114371200B (en) * | 2021-12-31 | 2023-10-31 | 上海工程技术大学 | High-stain-resistance MXene-ERHG electrochemical sensor and preparation method thereof |
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| US7507320B2 (en) * | 2004-10-09 | 2009-03-24 | Academia Sinica | Single-atom tip and preparation method thereof |
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| CN107262117B (en) * | 2017-07-25 | 2020-06-19 | 华中师范大学 | Single-atom metal-doped few-layer molybdenum disulfide electrocatalytic material, synthesis method and electrocatalytic nitrogen fixation method thereof |
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