CN108517534B - CVD method for preparing multifunctional nickel-doped molybdenum disulfide in-situ electrode - Google Patents

CVD method for preparing multifunctional nickel-doped molybdenum disulfide in-situ electrode Download PDF

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CN108517534B
CN108517534B CN201810196377.7A CN201810196377A CN108517534B CN 108517534 B CN108517534 B CN 108517534B CN 201810196377 A CN201810196377 A CN 201810196377A CN 108517534 B CN108517534 B CN 108517534B
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molybdenum disulfide
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黄妞
闫术芳
丁玉岳
孙小华
孙盼盼
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China Three Gorges University CTGU
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Abstract

The invention provides a CVD preparation method of a multifunctional nickel-doped molybdenum disulfide in-situ electrode, which is characterized in that nickel salt and molybdenum chloride are dissolved in a volatile non-aqueous solvent to obtain a Ni-Mo precursor solution; coating the precursor solution on a substrate, drying, and placing in Ar + S atmosphere or N2CVD vulcanization in + S atmosphere. The product obtained by the technical scheme of the invention has the advantages of low equipment requirement, low cost of required raw materials, easy control of reaction conditions, simple production process, good consistency of the formed product, small environmental pollution and the like, and can be used as a multifunctional electrocatalyst for HER, OER and ORR.

Description

CVD method for preparing multifunctional nickel-doped molybdenum disulfide in-situ electrode
Technical Field
The invention relates to an in-situ electrode and preparation thereof, belonging to the field of energy storage and conversion materials and devices.
Background
Molybdenum disulfide MoS2As a novel graphite-like material, the material is widely applied to the fields of hydrodesulfurization, lithium ion batteries, supercapacitors, hydrogen production by water electrolysis, dye-sensitized solar cells and the like. Mo and S atoms at the edges of the molybdenum disulfide layer have high catalytic activity due to coordination unsaturation, and S atoms in the layer which are saturated in coordination are basically inert. Research shows that molybdenum disulfide can effectively improve the catalytic performance of hydrodesulfurization and hydrogen production by electrolyzing water by doping transition metal elements such as cobalt and nickel. The research of England Environ Sci, 2015,8, 1594-1601) finds that the nickel incorporation greatly improves the hydrogen proton adsorption capacity of the surrounding sulfur atoms, and Δ GH 0The voltage is reduced from about 1.83eV to-0.28 eV. The larger adsorption capacity is intended to improve the catalytic hydrogen production (HER) performance of nickel-doped molybdenum disulfide in alkalinity (low hydrogen proton concentration).
The research shows that NiSx、NiOxHas the performance of electrocatalytic oxygen absorption (OER) and electrocatalytic oxygen reduction (ORR). If nickel is doped into molybdenum disulfide, a Ni-S bond exists in the nickel-doped molybdenum disulfide, and if pre-oxidation is carried out in the OER test process, a Ni-O bond exists. Thus, nickel doped molybdenum disulfide is intended to have OER and ORR properties.
However, this preparation of doped MoS2Wet chemical methods such as hydrothermal method, solvent thermal method, chemical bath and the like are mostly adopted, and most prepared samples are powder and still need to be prepared into slurry or ink for coating and film forming, so that the process complexity and the cost are increased.
Disclosure of Invention
In view of the above, the present invention is directed to an in-situ preparation method of Ni-doped MoS2The method of the electrode has the advantages of low equipment requirement, low cost of required raw materials, easy control of reaction conditions, simple production process, good consistency of formed products, small environmental pollution and the like, can be used for multifunctional electrocatalysts of HER, OER and ORR, and has great significance for batch production of in-situ electrodes.
Therefore, the invention provides a method for preparing in-situ Ni-doped MoS by film-forming Ni-Mo precursor liquid and then carrying out atmosphere vulcanization2A method of chemical vapor deposition of an electrode comprising the steps of:
firstly, under the condition of stirring at room temperature, dissolving nickel salt and molybdenum chloride in polar volatile solvents such as ethanol and the like to obtain Ni-Mo precursor solution, wherein the sum of the concentrations of Ni atoms and Mo atoms is 200-900 mM. The significance of this step is: almost no water molecule exists in the precursor liquid, so that molybdenum chloride is prevented from being hydrolyzed; uniformly dispersing reaction reagents to obtain a precursor liquid which is uniformly mixed with Ni and Mo without precipitates on an atomic scale for preparing uniform Ni-doped MoS2The array lays a good foundation.
And secondly, dripping or spin-coating the precursor on a substrate, such as carbon cloth, graphite paper, copper or nickel foil, drying in dry air or rapidly drying on a hot table at 70-100 ℃, wherein the step is as follows: the ethanol is quickly volatilized to leave a precursor film layer formed by uniformly mixing Ni salt and molybdenum chloride, so that uniform Ni-doped MoS can be obtained after the subsequent chemical vapor deposition reaction2And (3) a membrane. Thirdly, the precursor film in the second step is put in Ar + S atmosphere or N2Sintering at 500-800 ℃ for 30 min-3 h in + S atmosphere, cooling along with the furnace and taking out to obtain the Ni-doped MoS2And (4) in-situ electrode. Taking a chlorine salt of Ni as an example, the CVD doping reaction in sintering at 500-800 ℃ for 0.5-3 h is as follows:
Figure GDA0001646118220000021
the preparation principle of the Ni-doped molybdenum disulfide in-situ electrode is that ① utilizes the uniform mixing property of Ni and Mo atoms in Ni-Mo precursor liquid and the easy uniform film forming property of Ni-Mo ethanol precursor liquid, and ② utilizes CVD reaction at 500-800 ℃ to prepare Ni-doped molybdenum disulfide.
Drawings
FIG. 1 shows the linear voltammetric scans (LSV) of (a) HER, (b) OER, (c) ORR for Ni-doped molybdenum disulfide in-situ electrodes prepared in example 1.
Figure 2 OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulphide in situ electrode prepared in example 2.
Figure 3 OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulphide in situ electrode prepared in example 3.
Figure 4 OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulphide in situ electrode prepared in example 4.
Figure 5 (a) HER, (b) OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulfide in situ electrode prepared in example 5.
Figure 6 (a) HER, (b) OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulfide in situ electrode prepared in example 6.
Figure 7 XRD of Ni doped molybdenum disulphide in situ electrode prepared in example 6.
Figure 8 (a) HER, (b) OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulfide in situ electrode prepared in example 7.
Figure 9 (a) HER, (b) OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulfide in situ electrode prepared in example 8.
Figure 10 OER linear voltammetric scan (LSV) of the Ni doped molybdenum disulphide in situ electrode prepared in example 9.
FIG. 11 shows the linear voltammetric scans (LSV) of (a) HER, (b) OER, (c) ORR for Ni-doped molybdenum disulfide in-situ electrodes prepared in example 10.
Fig. 12 SEM of Ni-doped molybdenum disulfide in-situ electrode prepared in example 10, wherein a is low magnification SEM image; b is a low-magnification SEM image.
Detailed Description
Description of the drawings:
the method for testing HER, OER and ORR performance LSV in the embodiment of the invention comprises the following steps: ni-doped MoS2The in-situ electrode is a working electrode, the carbon rod is used as a counter electrode, the saturated Hg/HgO electrode is used as a reference electrode, the electrolyte is 1M KOH aqueous solution, and the scanning speed is 5mV s-1. Wherein HER test is saturated with nitrogen and OER and ORR test are saturated with oxygen. The potential of the corrected Reversible Hydrogen Electrode (RHE) was-0.842V relative to the saturated Hg/HgO electrode.
Example 1:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, the concentration of the nickel chloride is 40mM, the concentration of the molybdenum chloride is 360mM, and the ratio of the nickel atoms to the sum of the number of the nickel atoms and the number of the molybdenum atoms is 10%. Soaking the precursor solution in carbon paper, taking out, and drying at 80 deg.C for 10 min. The coated substrate is placed in a tube furnace and passed through N2After the residual air in the tube furnace is exhausted by vacuumizing repeatedly for three times, N is conducted again2The flow rate of gas is 2SCCM, 1g of sulfur powder is placed in the upper portion of the tube furnace, and as the temperature in the tube furnace is raised, the sulfur powder is evaporated to form sulfur vapour, and in the N portion2Reacting for 3h at 550 ℃ under the atmosphere of + S, naturally cooling and taking out. FIG. 1 is graphs of (a) HER, (b) OER, (c) ORR linear voltammetric sweep (LSV) of Ni-doped molybdenum disulfide in-situ electrode prepared in example 1. As can be seen from FIG. 1(a), the current density when the electrode passes through the electrode was 10mA/cm2Only 0.14V overpotential is needed for hydrogen production in the alkaline aqueous solution; when the electrode passes through the current density of 200mA/cm2When hydrogen is produced, the overpotential of only 0.26V is needed, and the electrode prepared by the embodiment has excellent hydrogen production performance. As can be seen from fig. 1(b), the electrode prepared in this example has oxygen evolution performance, the initial potential of oxygen evolution is 1.55V, and the overpotential of oxygen evolution is 1.55-1.23 ═ 0.32V. As can be seen from FIG. 1(c), the electrode prepared in this example has oxygen reduction performance, and the current density can reach 7.5mA/cm under the condition of no rotation2。
Example 2:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms and molybdenum atoms is 10%. Soaking the precursor solution in carbon paper, taking out, and drying at 80 deg.C for 10 min. Putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing Ar gas with the flow of 2SCCM, putting 1g of sulfur powder on the upper part of the tube furnace, evaporating the sulfur powder to form sulfur steam along with the temperature rise in the tube furnace, reacting for 45min at 800 ℃ in Ar + S atmosphere, naturally cooling and taking out. Figure 2 is a plot of OER linear voltammetric scan (LSV) of the Ni-doped molybdenum disulfide in-situ electrode prepared in example 2. As can be seen from the graph, the electrode prepared in this example has oxygen evolution performance, the initial potential of oxygen evolution is 1.55V, and the overpotential of oxygen evolution is 0.32V.
Example 3:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms and molybdenum atoms is 10%. Soaking the precursor solution in carbon paper, taking out, and drying at 80 deg.C for 10 min. Putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing Ar gas with the flow of 1SCCM, putting 0.5g of sulfur powder on the upper part of the tube furnace, evaporating the sulfur powder to form sulfur vapor along with the temperature rise in the tube furnace, reacting for 45min at 800 ℃ in Ar + S atmosphere, naturally cooling, and taking out. Figure 3 is a plot of OER linear voltammetric scan (LSV) of the Ni-doped molybdenum disulfide in-situ electrode prepared in example 3. As can be seen from the figure, the electrode prepared in this example has good oxygen evolution performance, the initial potential of oxygen evolution is 1.50V, and the overpotential of oxygen evolution is 0.27V.
Example 4:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms and molybdenum atoms is 10%. Soaking the carbon paper in the precursor solution, taking out, drying at 80 deg.C for 10min, dripping the precursor solution on the surface of the substrate, drying at 80 deg.C for 10min, placing the coated substrate in a tube furnace, introducing N2After the residual air in the tube furnace was exhausted by repeating the evacuation three times, Ar gas was introduced at a flow rate of 1SCCM and 2g of sulfur was charged in the upper part of the tube furnaceAnd (3) evaporating the sulfur powder to form sulfur vapor along with the temperature rise in the tube furnace, reacting for 45min at 800 ℃ in Ar + S atmosphere, naturally cooling and taking out. Figure 4 is a plot of OER linear voltammetric scans (LSV) of the Ni-doped molybdenum disulfide in-situ electrode prepared in example 4. As can be seen from the figure, the electrode prepared in this example has good oxygen evolution performance, the initial potential of oxygen evolution is 1.53V, and the overpotential of oxygen evolution is 0.30V.
Example 5:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the nickel chloride is 10mM, the concentration of the molybdenum chloride is 190mM, and the ratio of the nickel atoms to the sum of the number of the nickel atoms and the number of the molybdenum atoms is 5%. Soaking the precursor solution in carbon paper, taking out, and drying at 80 deg.C for 10 min. The coated substrate is placed in a tube furnace and passed through N2After the residual air in the tube furnace is exhausted by vacuumizing repeatedly for three times, N is conducted again2The flow rate of gas is 1SCCM, 1g of sulfur powder is placed in the upper portion of the tube furnace, and as the temperature in the tube furnace is raised, the sulfur powder is evaporated to form sulfur vapour, and in the N portion2Reacting for 1h at 600 ℃ under the atmosphere of + S, naturally cooling and taking out. FIG. 5 is graphs of (a) HER and (b) OER linear voltammetric scans (LSV) of Ni-doped molybdenum disulfide in-situ electrodes prepared in example 5. It can be seen from the figure that the electrode prepared in this example has good HER and OER properties.
Example 6:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms and molybdenum atoms is 10%. Soaking the precursor solution in carbon paper, taking out, and drying at 80 deg.C for 10 min. Putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing Ar gas with the flow of 1SCCM, putting 1g of sulfur powder on the upper part of the tube furnace, evaporating the sulfur powder to form sulfur steam along with the temperature rise in the tube furnace, reacting for 1h at 600 ℃ in Ar + S atmosphere, naturally cooling and taking out. FIG. 6 is graphs of (a) HER and (b) OER linear voltammetric scans (LSV) of Ni-doped molybdenum disulfide in-situ electrodes prepared in example 6. It can be seen from the figure that the electrode prepared in this example has good HER and OER properties. Figure 7 is an XRD of the Ni-doped molybdenum disulfide in-situ electrode prepared in example 6, comparing to a standard card, which indicates that the sample is molybdenum disulfide, indicating that nickel is about to be doped into molybdenum disulfide and nickel sulfide is not formed.
Example 7:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the nickel chloride is 90mM, the concentration of the molybdenum chloride is 360mM, and the ratio of the nickel atoms to the sum of the number of the nickel atoms and the number of the molybdenum atoms is 20%. Soaking the precursor solution in carbon paper, taking out, and drying at 80 deg.C for 10 min. Putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing Ar gas with the flow of 1SCCM, putting 1g of sulfur powder on the upper part of the tube furnace, evaporating the sulfur powder to form sulfur steam along with the temperature rise in the tube furnace, reacting for 1h at 600 ℃ in Ar + S atmosphere, naturally cooling and taking out. FIG. 8 is graphs of (a) HER and (b) OER linear voltammetric scans (LSV) of Ni-doped molybdenum disulfide in-situ electrodes prepared in example 7. It can be seen from the figure that the electrode prepared in this example has good HER and OER properties.
Example 8:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the nickel chloride is 80mM, the concentration of the molybdenum chloride is 720mM, and the ratio of the number of nickel atoms to the sum of the number of nickel atoms and molybdenum atoms is 10%. Soaking the precursor solution in carbon paper, taking out, and drying at 80 deg.C for 10 min. Putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing Ar gas with the flow of 1SCCM, putting 1g of sulfur powder on the upper part of the tube furnace, evaporating the sulfur powder to form sulfur steam along with the temperature rise in the tube furnace, reacting for 1h at 600 ℃ in Ar + S atmosphere, naturally cooling and taking out. FIG. 9 is graphs of (a) HER and (b) OER linear voltammetric scans (LSV) of Ni-doped molybdenum disulfide in-situ electrodes prepared in example 8. It can be seen from the figure that the electrode prepared in this example has good HER and OER properties.
Example 9
At room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms and molybdenum atoms is 10%. The precursor was applied dropwise to the surface of a flat graphite paper substrate and dried on a hot plate at 90 ℃ for 10 min. Putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing Ar gas with the flow of 1SCCM, putting 1g of sulfur powder on the upper part of the tube furnace, evaporating the sulfur powder to form sulfur steam along with the temperature rise in the tube furnace, reacting for 45min at 800 ℃ in Ar + S atmosphere, naturally cooling and taking out. Figure 10 is a plot of the OER linear voltammetric scan (LSV) of the Ni-doped molybdenum disulfide in-situ electrode prepared in example 9. It can be seen that the electrode prepared in this example has better OER performance.
Example 10:
at room temperature, nickel chloride and molybdenum chloride are dissolved in ethanol solution, wherein the concentration of the molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms and molybdenum atoms is 10%. The precursor was applied dropwise to the surface of a flat graphite paper substrate and dried on a hot plate at 90 ℃ for 10 min. Putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing Ar gas with the flow of 1SCCM, putting 1g of sulfur powder on the upper part of the tube furnace, evaporating the sulfur powder to form sulfur steam along with the temperature rise in the tube furnace, reacting at 500 ℃ for 30min under the Ar + S atmosphere, then reacting at 800 ℃ for 30min, naturally cooling, and taking out. FIG. 11 is graphs of (a) HER, (b) OER, (c) ORR linear voltammetric scan (LSV) of the Ni-doped molybdenum disulfide in-situ electrode prepared in example 10. It can be seen that the electrode prepared in this example has HER, OER, ORR functionalities and is intended to be used in electrolytic water reactors and metal air batteries. Figure 12 SEM image of Ni doped molybdenum disulfide in situ electrode prepared in example 10. It can be seen from the figure that the Ni-doped molybdenum disulfide in the electrode prepared in this example grows in a nano-sheet shape on the fiber rod of the carbon paper.

Claims (1)

1. A CVD preparation method of a multifunctional nickel-doped molybdenum disulfide in-situ electrode is characterized by comprising the following steps: dissolving nickel chloride and molybdenum chloride in ethanol solution at room temperature, wherein the concentration of the molybdenum chloride is 360mM, and the ratio of the nickel atoms to the sum of the nickel atoms and the molybdenum atoms is 10%, soaking the carbon paper in the precursor solution, taking out, and drying at 80 ℃ for 10min on a hot bench; putting the substrate with the coating into a tube furnace, introducing Ar gas, vacuumizing for three times repeatedly to discharge residual air in the tube furnace, introducing the Ar gas, wherein the flow rate is 1SCCM, 1g of sulfur powder is placed at the upper part of the tube furnace, the sulfur powder is evaporated to form sulfur steam along with the temperature rise in the tube furnace, reacting for 1h at 600 ℃ in Ar + S atmosphere, naturally cooling and taking out.
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