CN111560621A - NiSe/Ni3S2Composite, preparation method and self-supporting electrode prepared from composite - Google Patents
NiSe/Ni3S2Composite, preparation method and self-supporting electrode prepared from composite Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 title claims description 71
- 239000002131 composite material Substances 0.000 title abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 74
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 49
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 229910000990 Ni alloy Inorganic materials 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 239000000243 solution Substances 0.000 abstract description 4
- 150000001408 amides Chemical class 0.000 abstract 1
- 125000004014 thioethyl group Chemical group [H]SC([H])([H])C([H])([H])* 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 36
- 238000012360 testing method Methods 0.000 description 9
- 229910021607 Silver chloride Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000010411 electrocatalyst Substances 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- -1 Transition Metal Chalcogenides Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/069—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of at least one single element and at least one compound; consisting of two or more compounds
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention belongs to the technical field of electrode manufacturing, and particularly relates to NiSe/Ni3S2The composite, the preparation method and the prepared self-supporting electrode comprise the following steps: (1) synthesis of NiSe/NF: adding Se powder into mixed solution of glycerol and ethanol, and slowly adding NaBH into the solution4Stirring for 10-30 min, loading a piece of treated NF and the solution into an autoclave, reacting at 250 ℃ for 12h, naturally cooling, and washing the obtained product (NiSe) with deionized water and ethanol for several times alternately, (2) NiSe/Ni3S2The synthesis of (2): adding thioethyl into mixed solution of ethylene glycol and ethanolThen adding the NiSe/NF obtained in the step (1) after the amide and the urea are reacted for 2 to 8 hours at the temperature of 100 ℃ and 200 ℃ in a high pressure kettle, cooling and washing to obtain the NiSe/Ni3S2. The invention can efficiently separate oxygen under the alkaline condition.
Description
Technical Field
The invention belongs to the technical field of electrode manufacturing, and particularly relates to NiSe/Ni3S2A composite, a preparation method and a self-supporting electrode prepared by the composite.
Background
Electrocatalytic decomposition of water is a novel energy technology, and water decomposition involves two key half-reactions: a Hydrogen Evolution Reaction (HER) and an Oxygen Evolution Reaction (OER) occur at the cathode and anode, respectively. The key problem hindering practical application is the slow thermodynamics and kinetics of OER due to the proton coupled four electron transfer process and the formation of O-O bonds. Therefore, the emphasis on improving the efficiency of water decomposition should be on developing an excellent electrocatalyst so that the reaction rate can be improved while minimizing the OER kinetic overpotential. Noble metal catalysts (e.g. IrO)2And RuO2) Are the most advanced electrocatalysts for OER, however, the scarcity and high price of these rare metal based catalysts inevitably limits their widespread use. Transition Metal Chalcogenides (TMC), which are 3d transition metal compounds, have different oxidation states and are electrocatalysts currently being studied more in the field of electrochemical energy storage and conversion technology. Wherein nickel selenide (such as Ni0.85Se, NiSe) is added2And Ni3Se2) Giving great hope. However, these TMC materials have limited conductivity and insufficiently exposed electroactive sites in alkaline media, resulting in poor OER catalytic performance, and thus further improvements are needed in the art.
Disclosure of Invention
The invention aims to provide NiSe/Ni capable of efficiently separating oxygen under alkaline conditions3S2A composite, a preparation method and a self-supporting electrode prepared by the composite.
Based on the purpose, the invention adopts the following technical scheme:
NiSe/Ni3S2And (c) a complex.
The NiSe/Ni3S2The preparation method comprises the following steps:
(1) synthesis of NiSe/NF: se powder is added into the mixed solution of glycerol and ethanol, and NaBH is added4Uniformly stirring to obtain a mixed solution, mixing the pretreated NF with the mixed solution in a high-pressure kettle, reacting at the temperature of 150 ℃ and 250 ℃ for 10-14h, cooling and washing to obtain a piece of NiSe/NF;
（2）NiSe/Ni3S2the synthesis of (2): adding thioacetamide and urea into the mixed solution of ethylene glycol and ethanol, then adding NiSe/NF obtained in the step (1), reacting for 2-8h at the temperature of 100 ℃ and 200 ℃ in a high-pressure kettle, cooling and washing to obtain NiSe/Ni3S2。
Further, in the step (1), the Se powder: glycerol: ethanol NaBH4The mass-volume ratio of the glycol to the ethanol to the thioacetamide to the urea in the step (2) is 0.1974g, 5ml to 15 ml to 0.1892 g, the mass-volume ratio of the glycol to the ethanol to the thioacetamide to the urea in the step (2) is 25ml to 0.1503-0.4509g to 0.06g, and the specification of the pretreated NF is 0.5cm × 1cm × 4 cm.
Further, the pretreatment method of NF in the step (1) is prepared by the following steps: soaking NF in dilute hydrochloric acid for 20-30min, soaking in acetone for 20-30min, ultrasonic treating in ionized water at 40-50KHz for 15-25min, and vacuum drying.
Further, the cooling temperature is room temperature, and washing is performed by alternately washing with deionized water and ethanol for 3-5 times.
Further, the Se powder in the step (1) is 150-300 mesh powder.
Furthermore, the mass percent of the ethylene glycol in the step (2) is 96-98%, and the mass percent of the ethanol is 99.6-99.8%.
One kind of the NiSe/Ni3S2And (5) manufacturing the self-supporting electrode.
NiSe/Ni prepared by the invention3S2As a novel compound, the NiSe/Ni with the interface effect is synthesized by using a two-step method3S2Simple process, easy operation, the NiSe/Ni3S2The compound is used as an electrode to carry out an electrocatalytic oxygen evolution test in a 1M KOH solution, can reach a current density of 100 mA cm & lt-2 & gt at a lower overpotential (340 mV), and has long-term circulation stability and electrocatalytic reaction activity.
Drawings
FIG. 1 shows a series of NiSe/Ni compounds with different compounding ratios3S2XRD pattern of the electrode;
FIG. 2 shows NiSe/Ni with different compounding ratios3S2Graph of LSV testing of electrodes.
Detailed Description
Example 1:
NiSe/Ni3S2A compound; the NiSe/Ni3S2The preparation method comprises the following steps:
(1) synthesis of NiSe/NF: se powder is added into the mixed solution of glycerol and ethanol, and NaBH is added4Uniformly stirring to obtain a mixed solution, mixing the pretreated NF with the mixed solution in a high-pressure kettle, reacting for 10 hours at 150 ℃, cooling to room temperature, and alternately washing for 3 times by using deionized water and ethanol to obtain a piece of NiSe/NF;
（2）NiSe/Ni3S2the synthesis of (2): adding thioacetamide and urea into the mixed solution of ethylene glycol and ethanol, then adding NiSe/NF obtained in the step (1), reacting for 2 hours at 100 ℃ in a high-pressure kettle, cooling to room temperature, and alternately washing for 3 times by using deionized water and ethanol to obtain NiSe/Ni3S2。
The Se powder in the step (1): glycerol: ethanol NaBH4: the mass-to-volume ratio of (1) is 0.1974g, 5ml, 15 ml, 0.1892 g; se powder is 150-300 mesh powder. The ethylene glycol in the step (2): ethanol: thioacetamide: the mass volume ratio of the urea is 25ml to 0.1503g of 0.06g, wherein the specification of the pretreated NF is 0.5cm × 1cm × 4 cm, the mass percent of the ethylene glycol is 96 percent, and the mass percent of the ethanol is 99.6 percent.
The NF pretreatment method in the step (1) is prepared by the following steps: soaking NF in dilute hydrochloric acid for 20min, soaking in acetone for 20min, ultrasonic treating in ionized water at 40KHz for 15min, and vacuum drying.
The NiSe/Ni3S2And (5) manufacturing the self-supporting electrode.
Example 2:
NiSe/Ni3S2A compound; the NiSe/Ni3S2The preparation method comprises the following steps:
(1) synthesis of NiSe/NF: se powder is added into the mixed solution of glycerol and ethanol, and NaBH is added4Uniformly stirring to obtain a mixed solution, mixing the pretreated NF with the mixed solution in a high-pressure kettle, reacting for 12 hours at 200 ℃, cooling to room temperature, and alternately washing for 4 times by using deionized water and ethanol to obtain a piece of NiSe/NF;
（2）NiSe/Ni3S2the synthesis of (2): adding thioacetamide and urea into the mixed solution of ethylene glycol and ethanol, then adding NiSe/NF obtained in the step (1), reacting for 6 hours at 150 ℃ in a high-pressure kettle, cooling to room temperature, and alternately washing for 4 times by using deionized water and ethanol to obtain NiSe/Ni3S2。
The Se powder in the step (1): glycerol: ethanol NaBH4The mass volume ratio of the ethylene glycol to the ethanol to the thioacetamide to the urea in the step (2) is 25ml to 0.3006g to 0.06g, the pretreated NF specification is 0.5cm × cm × cm, the mass percent of the ethylene glycol is 96-98%, and the mass percent of the ethanol is 99.7%.
The NF pretreatment method in the step (1) is prepared by the following steps: soaking NF in dilute hydrochloric acid for 25min, soaking in acetone for 25min, ultrasonic treating in ionized water at 45KHz for 20min, and vacuum drying.
The NiSe/Ni3S2And (5) manufacturing the self-supporting electrode.
Example 3:
NiSe/Ni3S2A compound; the NiSe/Ni3S2The preparation method comprises the following steps:
(1) synthesis of NiSe/NF: se powder is added into the mixed solution of glycerol and ethanol, and NaBH is added4Uniformly stirring to obtain a mixed solution, mixing the pretreated NF with the mixed solution in a high-pressure kettle, reacting for 14h at 250 ℃, cooling to room temperature, and alternately washing for 5 times by using deionized water and ethanol to obtain a piece of NiSe/NF;
（2）NiSe/Ni3S2the synthesis of (2): adding thioacetamide and urea into the mixed solution of ethylene glycol and ethanol, then adding NiSe/NF obtained in the step (1), reacting for 8 hours at 200 ℃ in a high-pressure kettle, cooling to room temperature, and alternately washing for 5 times by using deionized water and ethanol to obtain NiSe/Ni3S2。
The Se powder in the step (1): glycerol: ethanol NaBH4The mass volume ratio of the ethylene glycol to the ethanol to the thioacetamide to the urea in the step (2) is 25ml to 0.4509g to 0.06g, the specification of the pretreated NF is 0.5cm × cm × cm, the mass percent of the ethylene glycol is 98%, and the mass percent of the ethanol is 99.8%.
The NF pretreatment method in the step (1) is prepared by the following steps: soaking NF in dilute hydrochloric acid for 30min, soaking in acetone for 30min, ultrasonic treating in ionized water at 50KHz for 25min, and vacuum drying.
The NiSe/Ni3S2And (5) manufacturing the self-supporting electrode.
Test example 1:
the electrochemical test was carried out using a three-electrode system with Ag/AgCl, carbon rods and the electrode obtained in example 1 as reference, counter and working electrodes, respectively, in alkaline medium (1.0M KOH, p)H =14) at a scan rate of 5 mV s (LSV)-1. All potential values were converted to Reversible Hydrogen Electrode (RHE) scale: eRHE= EAg/AgCl+ 0.196V +0.0591 pH. The electrode can reach 100 mA cm under the overpotential of 390 mV-2The current density. Test example 2:
electrochemical testing A three-electrode system was used, with Ag/AgCl, carbon rods and the electrode prepared in example 2 as reference, counter and working electrodes, respectively, and a Linear Sweep (LSV) was performed in alkaline medium (1.0M KOH, pH =14) at a sweep rate of 5 mV s-1. All potential values were converted to Reversible Hydrogen Electrode (RHE) scale: eRHE= EAg/AgCl+ 0.196V +0.0591 pH. The electrode can reach 100 mA cm under 340 mV overpotential-2The current density.
Test example 3:
electrochemical testing A three-electrode system was used, with Ag/AgCl, carbon rods and the electrode prepared in example 3 as reference, counter and working electrodes, respectively, and a Linear Sweep (LSV) was performed in alkaline medium (1.0M KOH, pH =14) at a sweep rate of 5 mV s-1. All potential values were converted to Reversible Hydrogen Electrode (RHE) scale: eRHE= EAg/AgCl+ 0.196V +0.0591 pH. The electrode can reach 100 mA cm at an overpotential of 445 mV-2The current density.
Test example 4:
NiSe/Ni prepared in example 13S2(NiSe/Ni in FIG. 1)3S2-1) NiSe/Ni prepared in example 23S2(NiSe/Ni in FIG. 1)3S2-2) NiSe/Ni prepared in example 33S2(NiSe/Ni in FIG. 1)3S2-3) carrying out X-ray diffraction, and analyzing a diffraction pattern XRD pattern of the obtained product, wherein NiSe/Ni is prepared by the method disclosed by the invention as shown in figure 13S2And (c) a complex.
Test example 5:
NiSe/Ni prepared in example 13S2Electrode (NiSe/Ni in figure 2)3S2-1) NiSe/Ni prepared in example 23S2Electrode (NiSe/Ni in figure 2)3S2-2) NiSe/Ni prepared in example 23S2The electrode (NiSe/Ni 3S2-3 in FIG. 2) was subjected to LSV profile in 1M KOH solution, and as shown in FIG. 2, the NiSe/Ni3S2 electrode prepared in example 2 showed better electrocatalytic oxygen evolution performance than that of examples 1 and 3.
Claims (8)
1. NiSe/Ni3S2And (c) a complex.
2. NiSe/Ni as defined in claim 13S2The preparation method is characterized by comprising the following steps:
(1) synthesis of NiSe/NF: se powder is added into the mixed solution of glycerol and ethanol, and NaBH is added4Uniformly stirring to obtain a mixed solution, mixing the pretreated NF with the mixed solution in a high-pressure kettle, reacting at the temperature of 150 ℃ and 250 ℃ for 10-14h, cooling and washing to obtain a piece of NiSe/NF;
（2）NiSe/Ni3S2the synthesis of (2): adding thioacetamide and urea into the mixed solution of ethylene glycol and ethanol, then adding NiSe/NF obtained in the step (1), reacting for 2-8h at the temperature of 100 ℃ and 200 ℃ in a high-pressure kettle, cooling and washing to obtain NiSe/Ni3S2。
3. NiSe/Ni as claimed in claim 23S2The method for preparing (1), wherein the Se powder: glycerol: ethanol NaBH4The mass-volume ratio of the glycol to the ethanol to the thioacetamide to the urea in the step (2) is 0.1974g, 5ml to 15 ml to 0.1892 g, the mass-volume ratio of the glycol to the ethanol to the thioacetamide to the urea in the step (2) is 25ml to 0.1503-0.4509g to 0.06g, and the specification of the pretreated NF is 0.5cm × 1cm × 4 cm.
4. NiSe/Ni as claimed in claim 23S2The preparation method is characterized in that the NF pretreatment method in the step (1) comprises the following stepsThe preparation method comprises the following steps: soaking NF in dilute hydrochloric acid for 20-30min, soaking in acetone for 20-30min, ultrasonic treating in ionized water at 40-50KHz for 15-25min, and vacuum drying.
5. NiSe/Ni as claimed in claim 23S2The preparation method is characterized in that the cooling temperature is room temperature, and the washing is carried out for 3-5 times by using deionized water and ethanol alternately.
6. NiSe/Ni as claimed in claim 23S2The preparation method is characterized in that the Se powder in the step (1) is 150-300 mesh powder.
7. NiSe/Ni as claimed in claim 23S2The preparation method is characterized in that the mass percent of the glycol in the step (2) is 96-98%, and the mass percent of the ethanol is 99.6-99.8%.
8. A NiSe/Ni alloy as defined in any one of claims 1 to 73S2And (5) manufacturing the self-supporting electrode.
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