CN109225270B - Ni3S2@ NiV-LDH heterostructure bifunctional electrocatalyst, preparation method and application - Google Patents
Ni3S2@ NiV-LDH heterostructure bifunctional electrocatalyst, preparation method and application Download PDFInfo
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Abstract
The invention provides Ni3S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst comprises the following steps: soaking a clean conductive matrix in an NiV-LDH precursor solution, and carrying out hydrothermal reaction to obtain an NiV-LDH/NF nanosheet array; soaking the NiV-LDH/NF nano sheet array in a uniform solution containing a sulfur source, and carrying out hydrothermal reaction to obtain Ni3S2The @ NiV-LDH heterostructure bifunctional electrocatalyst. The invention also provides the Ni3S2The @ NiV-LDH heterostructure bifunctional electrocatalyst. The invention directly prepares the electrode material, avoids using a binder, enables the material to fully expose active sites on the surface of the electrode material, and simultaneously solves the problem that the existing electrocatalyst can not simultaneously show excellent performance and stability on both OER and HER.
Description
Technical Field
The invention belongs to the technical field of electrocatalysts, and particularly relates to Ni3S2A @ NiV-LDH heterostructure bifunctional electrocatalyst, a preparation method and application.
Background
The exhaustion of the traditional fossil energy and the problem of environmental pollution become more serious, and people are forced to seek a novel alternative energy. Hydrogen energy is a clean, efficient, and pollution-free energy source. In consideration of the fact that the water storage capacity on the earth is extremely rich and the water is decomposed to generate hydrogen and oxygen, the technology for producing hydrogen and oxygen by electrolyzing water is favored by people. The water electrolysis process is divided into two half reactions: hydrogen evolution reaction and oxygen evolution reaction, noble metal oxide (IrO)2、RuO2) And the noble metal Pt are considered to be the most effective water-splitting OER and HER catalysts, but their expensive price and low reserves restrict large-scale production and wide application.
Recently, layered double hydroxides (abbreviated as LDHs) are a class of materials having a specific layered structure, which have been noticed and applied in OER due to their unique two-dimensional layered structure, controllability of composition and content of layered elements, and exchangeability of inter-layered anions, but have poor or almost no HER properties, and powder samples are easily curled during the test process, resulting in their properties being affected, Ni3S2Is a metallic sulfide with good conductivity, and is introduced with Ni3S2The nanomaterial can improve the conductivity of the material.
This patent uses a high efficiency, simple and low cost hydrothermal process to prepare Ni3S2The @ NiV-LDH heterostructure electrode material effectively improves the electrocatalytic full-hydrolytic performance of the material.
Disclosure of Invention
The invention introduces a conductive matrix, directly prepares an electrode material, avoids using a binder, enables the material to fully expose active sites on the surface of the electrode material, solves the problem that the conventional electrocatalyst can not simultaneously show excellent performance and stability on both OER and HER, and provides Ni3S2A preparation method of a @ NiV-LDH heterostructure bifunctional electrocatalyst.
(1) Immersing the conductive substrate into an acetone solution for ultrasonic cleaning for 5-20 min, then transferring the conductive substrate into 2-4 mol/L hydrochloric acid for ultrasonic cleaning for 5-20 min, finally alternately washing the conductive substrate with ethanol and ultrapure water for 2-3 times, and then performing vacuum drying at 25-35 ℃ for 10-14 h;
(2) preparing a precursor solution, wherein the precursor solution comprises an aqueous solution of nickel salt with the concentration of (0.05-0.2) mol/L, vanadium salt with the concentration of (0.0125-0.1) mol/L, ammonium fluoride with the concentration of (0.01-0.1) mol/L and urea with the concentration of (0.125-0.35) mol/L, and magnetically stirring at room temperature for 20-40 min to obtain a clear solution A. Transferring the clear solution A and the conductive matrix treated in the step (1) into a high-temperature high-pressure hydrothermal kettle, and then reacting for 6-18 h at 90-150 ℃, wherein the reaction filling ratio should be controlled at 20-80%. And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled conductive substrate after the reaction, collecting a product after 3 times of washing and 3 times of alternate alcohol washing, and drying in vacuum for 3-5 hours at the temperature of 25-35 ℃.
(3) Weighing a proper amount of Thioacetamide (TAA) and adding the Thioacetamide (TAA) into 20-40 ml of deionized water, wherein the concentration of the TAA is (1-2) mol/l, transferring the dried conductive matrix obtained in the step (2) and the TAA solution into a high-temperature high-pressure hydrothermal kettle together, and reacting for 0.5-2 h at 100-200 ℃, wherein the reaction filling ratio is controlled to be 20-80%.
The conductive substrate in the step (1) is any one of foamed nickel or carbon cloth.
The nickel salt in the step (2) is one of nickel nitrate hexahydrate, nickel sulfate hexahydrate or nickel chloride hexahydrate as the nickel source.
The vanadium salt in the step (2) is vanadium chloride.
The invention has the beneficial effects that:
(1) ni prepared by the invention3S2The @ NiV-LDH heterostructure is completed by simple hydrothermal reaction, and has the advantages of simple steps, short reaction time, environmental friendliness and strong repeatability.
(2) Ni proposed by the invention3S2The preparation method of the @ NiV-LDH composite structure is characterized in that a nanosheet array structure grows on a conductive substrate, and the nanosheet array structure is directly prepared into an electrode material which can be directly used for electrocatalytic performance testing.
Drawings
FIG. 1 shows Ni prepared in example 5 of the present invention3S2The X-ray diffraction (XRD) pattern of the @ NiV-LDH/NF composite structure;
FIG. 2 shows Ni prepared in example 5 of the present invention3S2Scanning Electron Microscope (SEM) picture of @ NiV-LDH/NF composite structure;
FIG. 3 shows Ni prepared in example 5 of the present invention3S2A Transmission Electron Microscope (TEM) photograph of the @ NiV-LDH/NF composite structure;
FIG. 4 shows Ni prepared in example 5 of the present invention3S2The HER performance graph of @ NiV-LDH/NF composite material;
FIG. 5 shows Ni prepared in example 5 of the present invention3S2The OER performance graph of the @ NiV-LDH/NF composite material.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific embodiments:
example 1:
the conductive substrate is foamed nickel, and the nickel salt is nickel nitrate hexahydrate.
(1) Immersing the conductive substrate in an acetone solution for ultrasonic cleaning for 10min, then transferring the conductive substrate to 2mol/L hydrochloric acid for ultrasonic cleaning for 10min, finally alternately washing the conductive substrate for 3 times by using ethanol and ultrapure water respectively, and then drying the conductive substrate for 10h in vacuum at 35 ℃;
(2) preparing a precursor solution, wherein the precursor solution comprises nickel nitrate hexahydrate with the concentration of 0.05mol/L, vanadium chloride with the concentration of 0.0125mol/L, ammonium fluoride with the concentration of 0.05mol/L and urea with the concentration of 0.125) mol/L, and magnetically stirring for 20min at room temperature to obtain a clear solution A. Transferring the clear solution A and the conductive matrix treated in the step (1) into a high-temperature high-pressure hydrothermal kettle, and then reacting for 18 hours at 100 ℃, wherein the reaction filling ratio should be controlled at 40%. And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled conductive substrate after the reaction, collecting a product after 3 times of washing and 3 times of alternate alcohol washing, and drying for 3 hours in vacuum at the temperature of 35 ℃.
(3) Weighing a proper amount of Thioacetamide (TAA) and adding the thioacetamide into 20ml of deionized water, wherein the concentration of the TAA is 2mol/l, then transferring the conductive matrix dried in the step (2) and the TAA solution into a high-temperature high-pressure hydrothermal kettle together, and then reacting for 2h at 100 ℃, wherein the reaction filling ratio should be controlled at 40%.
Example 2:
the conductive substrate is foamed nickel, and the nickel salt is nickel nitrate hexahydrate.
(1) Soaking foamed nickel with the size of 1cm x 5cm in an acetone solution, ultrasonically cleaning for 10min, then transferring to hydrochloric acid with the size of 2mol/L, ultrasonically cleaning for 10min, finally alternately washing for 3 times by using ethanol and ultrapure water respectively, and then carrying out vacuum drying for 10h at the temperature of 35 ℃;
(2) preparing a precursor solution, wherein the precursor solution comprises nickel nitrate hexahydrate with the concentration of 0.1mol/L, vanadium chloride with the concentration of 0.04mol/L, ammonium fluoride with the concentration of 0.05mol/L and urea aqueous solution with the concentration of 0.2mol/L, and magnetically stirring for 20min at room temperature to obtain a clear solution A. Transferring the clear solution A and the conductive matrix treated in the step (1) into a high-temperature high-pressure hydrothermal kettle, and then reacting for 14h at 120 ℃, wherein the reaction filling ratio should be controlled at 40%. And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled conductive substrate after the reaction, collecting a product after 3 times of washing and 3 times of alternate alcohol washing, and drying for 3 hours in vacuum at the temperature of 35 ℃.
(3) Weighing a proper amount of Thioacetamide (TAA) and adding the thioacetamide into 30ml of deionized water, wherein the concentration of the TAA is 2mol/l, then transferring the conductive matrix dried in the step (2) and the TAA solution into a high-temperature high-pressure hydrothermal kettle together, and then reacting for 1h at 120 ℃, wherein the reaction filling ratio should be controlled at 60%.
Example 3:
the conductive substrate is foamed nickel, and the nickel salt is nickel chloride hexahydrate.
(1) Immersing foamed nickel with the size of 1cm x 5cm into an acetone solution for ultrasonic cleaning for 5min, immersing the foamed nickel into hydrochloric acid with the size of 2mol/L for ultrasonic cleaning for 5min, finally alternately washing the foamed nickel for 3 times by using ethanol and ultrapure water respectively, and performing vacuum drying at the temperature of 30 ℃ for 10 times to obtain the processed foamed nickel;
(2) preparing a precursor solution, wherein the precursor solution comprises nickel chloride hexahydrate with the concentration of 0.1mol/L, vanadium chloride with the concentration of 0.05mol/L, ammonium fluoride with the concentration of 0.05mol/L and an aqueous solution of urea with the concentration of 0.2mol/L, and magnetically stirring for 20min at room temperature to obtain a clear solution A. Transferring the clear solution A and the foamed nickel treated in the step (1) into a high-temperature high-pressure hydrothermal kettle, and then reacting for 10 hours at 140 ℃, wherein the reaction filling ratio should be controlled at 30%. And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled conductive substrate after the reaction, collecting a product after 3 times of washing and 3 times of alternate alcohol washing, and drying for 3 hours in vacuum at the temperature of 35 ℃.
(3) Weighing an appropriate amount of Thioacetamide (TAA) and adding the thioacetamide into 30ml of deionized water, wherein the concentration of the TAA is 2mol/l, then transferring the conductive matrix dried in the step (2) and the TAA solution into a high-temperature high-pressure hydrothermal kettle together, and then reacting for 0.5h at 140 ℃, wherein the reaction filling ratio should be controlled at 60%.
Example 4:
the conductive matrix is foamed nickel, and the nickel salt is nickel sulfate hexahydrate.
(1) Immersing foamed nickel with the size of 1cm x 5cm into an acetone solution for ultrasonic cleaning for 5min, immersing the foamed nickel into hydrochloric acid with the size of 2mol/L for ultrasonic cleaning for 5min, finally alternately washing the foamed nickel for 3 times by using ethanol and ultrapure water respectively, and performing vacuum drying at the temperature of 30 ℃ for 10 times to obtain the processed foamed nickel;
(2) preparing a precursor solution, wherein the precursor solution comprises nickel sulfate hexahydrate with the concentration of 0.1167mol/L, vanadium chloride with the concentration of 0.067mol/L, ammonium fluoride with the concentration of 0.05mol/L and urea with the concentration of 0.2167mol/L, and magnetically stirring for 20min at room temperature to obtain a clear solution A. Transferring the clear solution A and the foamed nickel treated in the step (1) into a high-temperature high-pressure hydrothermal kettle, and then reacting for 15 hours at 150 ℃, wherein the reaction filling ratio should be controlled at 40%. And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled conductive substrate after the reaction, collecting a product after 3 times of washing and 3 times of alternate alcohol washing, and drying for 3 hours in vacuum at the temperature of 35 ℃.
(3) And (3) weighing a proper amount of TAA, adding the TAA into 20ml of deionized water, wherein the concentration of the TAA is 2mol/l, transferring the NiV-LDH/NF nanosheet array prepared in the step two and the TAA solution into a high-temperature high-pressure hydrothermal kettle, and reacting for 2 hours at 100 ℃, wherein the reaction filling ratio is controlled to be 40%.
Example 5:
the conductive substrate is foamed nickel, and the nickel salt is nickel chloride hexahydrate.
(1) Immersing foamed nickel with the size of 1cm x 5cm into an acetone solution for ultrasonic cleaning for 5min, immersing the foamed nickel into hydrochloric acid with the size of 2mol/L for ultrasonic cleaning for 5min, finally alternately washing the foamed nickel for 3 times by using ethanol and ultrapure water respectively, and performing vacuum drying at the temperature of 30 ℃ for 10 times to obtain the processed foamed nickel;
(2) preparing a precursor solution, wherein the precursor solution comprises nickel chloride hexahydrate with the concentration of 0.1mol/L, vanadium chloride with the concentration of 0.025mol/L, ammonium fluoride with the concentration of 0.05mol/L and urea aqueous solution with the concentration of 0.25mol/L, and magnetically stirring for 20min at room temperature to obtain a clear solution A. Transferring the clear solution A and the foamed nickel treated in the step (1) into a high-temperature high-pressure hydrothermal kettle, and then reacting for 10 hours at 150 ℃, wherein the reaction filling ratio should be controlled at 40%. And after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled conductive substrate after the reaction, collecting a product after 3 times of washing and 3 times of alternate alcohol washing, and drying for 3 hours in vacuum at the temperature of 35 ℃.
(3) And (3) weighing a proper amount of TAA, adding the TAA into 20ml of deionized water, wherein the concentration of the TAA is 2mol/l, transferring the NiV-LDH/NF nanosheet array prepared in the step two and the TAA solution into a high-temperature high-pressure hydrothermal kettle together, and reacting for 0.5h at 160 ℃, wherein the reaction filling ratio is controlled to be 40%.
FIG. 1 shows Ni prepared in this example3S2The X-ray diffraction (XRD) pattern of the @ NiV-LDH/NF composite structure. The nickel foam and Ni appear in characteristic peaks of XRD pattern of product of the embodiment3S2And characteristic peaks of NiV-LDH, which indicates that the target product is obtained.
FIG. 2 shows Ni prepared in this example3S2Scanning Electron Microscope (SEM) picture of @ NiV-LDH/NF composite structure. The photograph shows that the foam nickel surface grows an array structure stacked by nano sheets.
FIG. 3 shows Ni prepared in this example3S2And a Transmission Electron Microscope (TEM) picture of the @ NiV-LDH/NF composite structure. The photograph shows the nano-particles embedded in the nano-sheets.
FIG. 4 shows Ni prepared in this example3S2The HER performance graph of the @ NiV-LDH/NF composite material. FIG. 4 shows that the composite material has good electrocatalytic hydrogen evolution performance inThe current density is 10mA/cm2When the voltage is higher than the threshold voltage, the overpotential is 200 mV.
FIG. 5 shows Ni prepared in this example3S2The OER performance graph of the @ NiV-LDH/NF composite material. FIG. 5 shows that the composite material has good electrocatalytic oxygen evolution performance and the current density is 50mA/cm2When the voltage is higher than the threshold voltage, the overpotential is 350 mV.
Claims (10)
1. Ni3S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized by comprising the following steps of:
soaking a clean conductive matrix in an NiV-LDH precursor solution, and carrying out hydrothermal reaction to obtain an NiV-LDH/NF nanosheet array; soaking the NiV-LDH/NF nano sheet array in a uniform solution containing a sulfur source, and carrying out hydrothermal reaction to obtain Ni3S2The @ NiV-LDH heterostructure bifunctional electrocatalyst.
2. Ni according to claim 13S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized in that the NiV-LDH precursor solution is an aqueous solution containing a nickel source with the concentration of 0.05-0.2 mol/L, a vanadium source with the concentration of 0.0125-0.1 mol/L, ammonium fluoride with the concentration of 0.01-0.1 mol/L and urea with the concentration of 0.125-0.35 mol/L.
3. Ni according to claim 23S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized in that the nickel source is one of nickel nitrate hexahydrate, nickel sulfate hexahydrate and nickel chloride hexahydrate.
4. Ni according to claim 23S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized in that the vanadium source is vanadium chloride.
5. Ni according to claim 13S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized in thatThe conductive substrate is foamed nickel or carbon cloth.
6. Ni according to claim 13S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized in that the sulfur source is thioacetamide TAA.
7. Ni according to claim 13S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized in that the reaction temperature of hydrothermal reaction for preparing the NiV-LDH/NF nanosheet array is 90-150 ℃, the reaction time is 6-18 h, and the reaction filling ratio is controlled to be 20-80%; the reaction temperature of the hydrothermal reaction of the sulfur source and the NiV-LDH/NF nanosheet array is 100-200 ℃, the reaction time is 0.5-2 h, and the reaction filling ratio is controlled to be 20-80%.
8. Ni according to claim 13S2The preparation method of the @ NiV-LDH heterostructure bifunctional electrocatalyst is characterized by comprising the following specific steps of:
1) immersing the conductive substrate into an acetone solution for ultrasonic cleaning for 5-20 min, then transferring the conductive substrate into 2-4 mol/L hydrochloric acid for ultrasonic cleaning for 5-20 min, finally alternately washing the conductive substrate with ethanol and ultrapure water for 2-3 times, and then performing vacuum drying at 25-35 ℃ for 10-14 h;
2) preparing a precursor solution, wherein the precursor solution comprises an aqueous solution of nickel salt with the concentration of 0.05-0.2 mol/L, vanadium salt with the concentration of 0.0125-0.1 mol/L, ammonium fluoride with the concentration of 0.01-0.1 mol/L and urea with the concentration of 0.125-0.35 mol/L, and magnetically stirring at room temperature for 20-40 min to obtain a clear solution A; transferring the clear solution A and the conductive matrix treated in the step 1) into a high-temperature high-pressure hydrothermal kettle, and then reacting for 6-18 h at 90-150 ℃, wherein the reaction filling ratio should be controlled at 20-80%; after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled conductive substrate after the reaction, collecting a product after 3 times of washing and 3 times of alternate alcohol washing, and drying in vacuum for 3-5 hours at the temperature of 25-35 ℃;
3) weighing a proper amount of thioacetamide TAA, adding the thioacetamide TAA into 20-40 mL of deionized water, wherein the concentration of the TAA is 1-2 mol/L, transferring the dried conductive matrix obtained in the step 2) and the TAA solution into a high-temperature high-pressure hydrothermal kettle, and reacting for 0.5-2 h at 100-200 ℃, wherein the reaction filling ratio should be controlled at 20-80%.
9. Ni prepared by the method of any one of claims 1 to 83S2The @ NiV-LDH heterostructure bifunctional electrocatalyst.
10. Ni of claim 93S2The application of the @ NiV-LDH heterostructure bifunctional electrocatalyst as a catalyst for electrocatalytic full-hydrolysis.
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| "Ni基纳米材料的制备及其电催化性能研究";罗琼;《中国优秀硕士学位论文全文数据库工程科技I辑》;20170215(第02期);B020-834 * |
| "Tunable 3D hierarchical Ni3S2 superstructures as efficient and stable bifunctional electrocatalysts for both H2 and O2 generation";Lingyou Zeng et al.;《Journal of Materials Chemistry A》;20180208;第6卷(第10期);第4485-4493页 * |
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