CN110767462A - Bimetal nickel-cobalt telluride supercapacitor electrode material and preparation method thereof - Google Patents
Bimetal nickel-cobalt telluride supercapacitor electrode material and preparation method thereof Download PDFInfo
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- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000007772 electrode material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 32
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 16
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- -1 nano-needle Substances 0.000 claims abstract description 6
- 239000002135 nanosheet Substances 0.000 claims abstract description 6
- 239000002071 nanotube Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002073 nanorod Substances 0.000 claims abstract description 5
- 239000012467 final product Substances 0.000 claims abstract description 3
- 238000005342 ion exchange Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000007774 positive electrode material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 abstract description 7
- 238000004146 energy storage Methods 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 239000011232 storage material Substances 0.000 abstract description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract 1
- 239000010931 gold Substances 0.000 abstract 1
- 229910052737 gold Inorganic materials 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 239000006260 foam Substances 0.000 description 15
- 229910052759 nickel Inorganic materials 0.000 description 15
- 239000000835 fiber Substances 0.000 description 9
- 229910021389 graphene Inorganic materials 0.000 description 9
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 7
- 229910052714 tellurium Inorganic materials 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 150000004771 selenides Chemical class 0.000 description 2
- SITVSCPRJNYAGV-UHFFFAOYSA-L tellurite Chemical compound [O-][Te]([O-])=O SITVSCPRJNYAGV-UHFFFAOYSA-L 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- YTBWYQYUOZHUKJ-UHFFFAOYSA-N oxocobalt;oxonickel Chemical compound [Co]=O.[Ni]=O YTBWYQYUOZHUKJ-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Images
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
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Abstract
A bimetal nickel-cobalt telluride supercapacitor electrode material and a preparation method thereof belong to the technical field of energy storage materials. Using urea as precipitant and Ni2+And Co2+Free Ni in the mixed solution2+And Co2+Growing a nickel-cobalt precursor on a conductive substrate, and then putting the conductive substrate with the nickel-cobalt precursor into a reducing aqueous solution containing sodium tellurite and hydrazine hydrate, wherein Te is4+After being reduced by hydrazine hydrate, the bimetal nickel cobalt telluride is formed through ion exchange reaction; by adjusting Ni2+And Co2+And (3) mixing the solvent of the solution to obtain nickel-cobalt precursors with different morphologies, and regulating and controlling the morphology of the bimetal nickel-cobalt telluride by regulating the concentration of sodium tellurite in the reducing aqueous solution and regulating the reaction time. Final product of gold and silverThe shape of the nickel-cobalt telluride on the conductive substrate is one or more of nano-sheet, nano-needle, nano-tube and nano-rod. The invention improves the electrochemical performance.
Description
The technical field is as follows:
the invention belongs to the technical field of energy storage materials, relates to a transition metal compound electrode material, and particularly relates to a bimetal nickel-cobalt telluride supercapacitor electrode material and a preparation method thereof.
Background art:
the super capacitor, as one type of energy storage device, has the advantages of ultra-high power density, fast charge/discharge rate, long cycle life, high safety, and the like. However, commercial supercapacitors have much lower energy densities than batteries and fuel cells. Therefore, it is very desirable to increase the energy density without losing the power density, and the preparation of the hybrid supercapacitor is one of the effective methods for solving the above problems. The hybrid supercapacitor consists of a battery-type electrode and a capacitor electrode. Among them, the battery type electrode brings high energy, and the capacitor type electrode provides high power and long life. In recent years, nickel or cobalt oxide/hydroxide has been the focus of research as a battery-type material with high theoretical specific capacity, but the application of nickel or cobalt oxide/hydroxide is limited by low conductivity and poor electrochemical stability, and the research finds that the bimetallic nickel-cobalt compound has higher conductivity and more active sites than the corresponding monometallic compound, and shows better electrochemical performance. In addition, tellurium is used as a semimetal, theoretically, the telluride has higher conductivity than an oxide, and the electrochemical performance of the bimetal nickel-cobalt telluride is expected to be further improved when the bimetal nickel-cobalt telluride is used as an electrode material.
Through search, Chinese patents related to the synthesis of transition metal telluride are as follows: a preparation method (CN108636428A) of metal telluride as a bifunctional electrolytic water catalyst; a preparation method of a metal chalcogenide nano-sieve material (CN 103910340A); a method for synthesizing various metal selenide and telluride semiconductor materials (CN 1384047A). The transition metal tellurides with different morphologies can be prepared on different substrates by the method, but the preparation method of the nickel-cobalt double-metal telluride is not reported at present.
The method prepares the bimetal nickel-cobalt telluride with four shapes of sheet, tube, needle and bar for the first time by a simple solvothermal method. Specifically, urea is used as a precipitant to precipitate Ni2+And Co2+Forming a nickel-cobalt precursor to grow on the conductive substrate, and tellurite sodium and hydrazine hydrate to tellurite the nickel-cobalt precursor to form nickel-cobalt telluride. The morphology of the product is regulated and controlled by the type of the solvent, the concentration of sodium tellurite and the reaction time. The nickel-cobalt telluride has high conductivity (3.30 multiplied by 10)4S m-1) High hydrophilicity, large specific surface area and abundant electrochemical active sites,the electrochemical performance of the material is better when the material is used as a self-supporting supercapacitor electrode material. Under a three-electrode system, the nano-tube-shaped nickel-cobalt telluride electrode material has a current density of 1A g-1The specific capacity reaches 945F g-1At 20A g-1Can still maintain 571F g at the current density of-1. After 5000 times of cyclic charge and discharge, the capacity retention rate still reaches 92 percent. After forming a hybrid supercapacitor with activated carbon, 820W kg-1The energy density can reach 48.3Wh kg under the power density-1. The energy density value as a key performance index of the super capacitor is obviously superior to that of bimetal nickel-cobalt oxide, sulfide and selenide. The patent provides a new idea for high-performance supercapacitor electrode materials and has a good application prospect in the energy field.
The invention content is as follows:
the invention aims to provide a preparation method of a bimetal nickel-cobalt telluride used for a super capacitor electrode material. The method is simple, and the prepared electrode material has good electrochemical performance.
The technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a bimetal nickel cobalt telluride electrode material is characterized by comprising the following steps: using urea as precipitant and Ni2+And Co2+Free Ni in the mixed solution2+And Co2+Growing a nickel-cobalt precursor on a conductive substrate, and then putting the conductive substrate with the nickel-cobalt precursor into a reducing aqueous solution containing sodium tellurite and hydrazine hydrate, wherein Te is4+After being reduced by hydrazine hydrate, the bimetal nickel cobalt telluride is formed through ion exchange reaction.
The preparation process comprises the following steps:
(1) growing nickel-cobalt precursor on conductive substrate
Firstly, Ni is added2+And Co2+Dissolving the mixture into a solvent according to the molar ratio of 1:2, adding urea, and magnetically stirring for 15 minutes to form a uniform solution; then placing the solution and the conductive substrate cleaned in advance in a high-pressure reaction kettle, and reacting for 5-8h at 120 ℃; cooling to room temperature, taking out the conductive substrate, and adding BCleaning with alcohol and deionized water for several times, and drying in an oven at 70 ℃ overnight to obtain the conductive substrate loaded with the nickel-cobalt precursor;
(2) preparation of nickel cobalt telluride on conductive substrates
Uniformly mixing a sodium tellurite aqueous solution and hydrazine hydrate, placing the mixture into a high-pressure reaction kettle, placing the conductive substrate loaded with the nickel-cobalt precursor prepared in the step (1) into the mixed aqueous solution, and reacting for 8-15h at 180 ℃; after cooling to room temperature, the conductive substrate was taken out, washed several times with ethanol and deionized water, and dried in a vacuum oven.
Preferably, Ni is added to the solution of step (1) in an amount of 0.3 to 1mmol per 0.3 to 1mmol of Ni2+Corresponding to 25-60ml of solvent and 1.0-4mmol of urea, wherein the solvent is ethanol or a mixed solution of ethanol, and the volume ratio of the ethanol to the water in the mixed solution is 1: 0-5;
preferably, the concentration of the sodium tellurite aqueous solution in the step (2) is 0.1-10 mM; the dosage of hydrazine hydrate is: every 70ml of sodium tellurite aqueous solution corresponds to 2-10ml of 80% hydrazine hydrate.
Ni2+And Co2+Is added in the form of nitrate.
The invention adjusts Ni2+And Co2+And (3) mixing the solvent of the solution to obtain nickel-cobalt precursors with different morphologies, and regulating and controlling the morphology of the bimetal nickel-cobalt telluride by regulating the concentration of sodium tellurite in the reducing aqueous solution and regulating the reaction time. The appearance of the final product bimetal nickel cobalt telluride on the conductive substrate is one or more of nano sheets, nano needles, nano tubes and nano rods.
The bimetallic nickel-cobalt telluride electrode material can be used as a super capacitor electrode material.
The invention relates to 3 basic principles:
(1) the reason why the bimetal nickel-cobalt telluride is selected as the electrode material is that the bimetal nickel-cobalt telluride has high conductivity, super-hydrophilicity and abundant electrochemical active sites, and can realize high electrochemical performance.
(2) Through the selection of the solvent and the control of the reaction concentration and the reaction time, the nickel-cobalt telluride with various shapes is formed, including nano sheets, nano needles, nano tubes and nano rods. The unique nano structure increases the specific surface area of the electrode material, ensures sufficient electrode electrolyte contact and realizes rapid ion/electron transmission.
(3) The electrode material active substance directly grows on the conductive substrate and directly serves as the electrode material, a conductive agent and an adhesive do not need to be added, the interface contact resistance is reduced, and the electrochemical performance is favorably improved.
Drawings
FIG. 1 is a flow chart of the preparation of nickel cobalt telluride.
FIGS. 2a, b, c, d, e, f are SEM images of the electrode materials prepared in examples 1-6, respectively.
Fig. 3 is an XRD spectrum of the electrode material prepared in example 2.
FIGS. 4a, b, c, d are the current-voltage curves at different scan rates, the constant current charging and discharging curves at different current densities, the specific capacitance curves at different current densities and the specific capacitance curve at 5Ag for the electrode material prepared in example 2-1Capacity retention versus cycle number curve.
Fig. 5 is a graph of energy density versus power density for a hybrid supercapacitor assembled from the electrode material prepared in example 2.
Detailed Description
The present invention will be further described in the following examples, which are illustrative, not restrictive and are not intended to limit the scope of the invention.
Example 1.
Firstly, growing nickel-cobalt precursor on a nickel foam substrate, and firstly, 0.3mmol of Ni2+And 0.6mmol Co2+Dissolving in 60mL ethanol, adding 1.1mmol urea, and magnetically stirring for 15 min to obtain a uniform solution. And (3) placing the solution and the cleaned nickel foam in a high-pressure reaction kettle, and reacting for 8 hours at 120 ℃. After cooling to room temperature, the nickel foam was removed, washed several times with ethanol and deionized water, and dried in an oven at 70 ℃ overnight.
And preparing the nickel-cobalt telluride. 70ml of a 1mM sodium tellurite aqueous solution was prepared, and 5ml of hydrazine hydrate (80%) was added thereto and magnetically stirred for 30 minutes. And transferring the solution into a high-pressure reaction kettle, simultaneously putting nickel foam loaded with a nickel-cobalt precursor, and carrying out a tellurization reaction for 8 hours at 180 ℃. After cooling to room temperature, the nickel foam was taken out, washed several times with ethanol and deionized water, and vacuum dried in a vacuum oven at 70 ℃ for 12 h. And obtaining the electrode material of the nickel-cobalt-tellurium nanosheet loaded on the nickel foam. See a in fig. 2.
Example 2.
The procedure is as in example 1, except that the reaction time for the telluride formation is 12 hours. And obtaining the electrode material of the nickel-cobalt-tellurium nanotube loaded on the nickel foam. See b in fig. 2.
Example 3.
The procedure is as in example 1, except that the reaction time for the telluride formation is 15 hours. And obtaining the electrode material of the nickel-cobalt-tellurium nanotube loaded on the nickel foam. See c in fig. 2.
Example 4.
Firstly, growing nickel-cobalt precursor on a nickel foam substrate, firstly, 1mmol of Ni (NO)3)2·6H2O and 2mmol Co (NO)3)2·6H2Dissolving O in 25mL of mixed solution of ethanol and water, adding 4mmol of urea, and magnetically stirring for 15 minutes to obtain a uniform solution. And (3) placing the solution and the cleaned nickel foam in a high-pressure reaction kettle, and reacting for 5 hours at 120 ℃. After cooling to room temperature, the nickel foam was removed, washed several times with ethanol and deionized water, and dried in an oven at 70 ℃ overnight.
And preparing the nickel-cobalt telluride. 70ml of 5mM sodium tellurite aqueous solution was prepared, and 5ml of hydrazine hydrate (80%) was added thereto, followed by magnetic stirring for 30 minutes. And transferring the solution into a high-pressure reaction kettle, simultaneously adding nickel foam loaded with a nickel-cobalt precursor, and reacting for 12 hours at 180 ℃. After cooling to room temperature, the nickel foam was taken out, washed several times with ethanol and deionized water, and vacuum dried in a vacuum oven at 70 ℃ for 3 h. And obtaining the electrode material of the nickel-cobalt-tellurium nanoneedle loaded on the nickel foam. See d in fig. 2.
Example 5.
The procedure was as in example 1 except that the concentration of the sodium tellurite aqueous solution was 0.5 mM. And obtaining the electrode material of the nickel-cobalt-tellurium nano rod loaded on the nickel foam. See e in fig. 2.
Example 6.
Firstly, growing a nickel-cobalt precursor on a graphene fiber substrate, and firstly, 0.3mmol of Ni2+And 0.6mmol Co2+Dissolving in 60mL ethanol, adding 1.1mmol urea, and magnetically stirring for 15 min to obtain a uniform solution. And (3) putting the solution and the graphene fiber into a high-pressure reaction kettle, and reacting for 8 hours at 120 ℃. After cooling to room temperature, taking out the graphene fiber, washing the graphene fiber with ethanol and deionized water for several times, and drying the graphene fiber in an oven at 70 ℃ overnight.
And preparing the nickel-cobalt telluride. 70ml of a 10mM sodium tellurite aqueous solution was prepared, and 5ml of hydrazine hydrate (80%) was added thereto, followed by magnetic stirring for 30 minutes. Transferring the solution into a polytetrafluoroethylene lining, simultaneously putting graphene fibers loaded with nickel-cobalt precursors, putting the lining into a Geya reaction kettle, and reacting for 12 hours at 180 ℃. And after cooling to room temperature, taking out the graphene fiber, washing the graphene fiber with ethanol and deionized water for several times, and performing vacuum drying in a vacuum oven at 70 ℃ for 12 hours. And obtaining the electrode material of the nickel-cobalt-tellurium nanosheet loaded on the graphene fiber. See f in fig. 2.
Results of the implementation
Using the three-electrode electrochemical test, for examples 1, 3, 4, 5, at a current density of 1A g-1Specific capacity is 580Fg-1～683F g-1In the meantime. For the optimized electrode material example 2, at a current density of 1A g-1When the specific capacity reaches 945Fg-1And the cycle is 5000 times, the capacity retention rate is 92%, see figure 4. After the product of example 2 was combined with activated carbon to form a hybrid supercapacitor (i.e., the product of example 2 as a positive electrode material and activated carbon as a negative electrode material), 820W kg-1The energy density of the power can reach 48.3Wh kg-1See fig. 5. For example 7, at a current density of 0.8A cm-3When the specific capacity reaches 407F cm-3And the cycle is 1000 times, the capacity retention rate is 87%.
The relevant process parameters in the electrochemical test method are as follows: the nickel-cobalt telluride growing on the conductive substrate obtained by the method is directly used as an electrode material, 6M potassium hydroxide is used as electrolyte, and an Hg/HgO electrode and a platinum sheet/wire are used as a reference electrode and a counter electrode for three-electrode electrochemical test.
Claims (8)
1. A preparation method of a bimetal nickel cobalt telluride electrode material is characterized by comprising the following steps: using urea as precipitant and Ni2 +And Co2+Free Ni in the mixed solution2+And Co2+Growing a nickel-cobalt precursor on a conductive substrate, and then putting the conductive substrate with the nickel-cobalt precursor into a reducing aqueous solution containing sodium tellurite and hydrazine hydrate, wherein Te is4+After being reduced by hydrazine hydrate, the bimetal nickel cobalt telluride is formed through ion exchange reaction.
2. The method of claim 1, wherein the method comprises the steps of:
(1) growing nickel-cobalt precursor on conductive substrate
Firstly, Ni is added2+And Co2+Dissolving the mixture into a solvent according to the molar ratio of 1:2, adding urea, and magnetically stirring for 15 minutes to form a uniform solution; then placing the solution and the conductive substrate cleaned in advance in a high-pressure reaction kettle, and reacting for 5-8h at 120 ℃; after cooling to room temperature, taking out the conductive substrate, washing the conductive substrate with ethanol and deionized water for several times, and drying the conductive substrate in an oven at 70 ℃ overnight to obtain a conductive substrate loaded with a nickel-cobalt precursor;
(2) preparation of nickel cobalt telluride on conductive substrates
Preparing a sodium tellurite aqueous solution, uniformly mixing the sodium tellurite aqueous solution with hydrazine hydrate, placing the mixture into a high-pressure reaction kettle, placing the conductive substrate loaded with the nickel-cobalt precursor prepared in the step (1) into the mixed aqueous solution, and reacting for 8-15h at 180 ℃; after cooling to room temperature, the conductive substrate was taken out, washed several times with ethanol and deionized water, and dried in a vacuum oven.
3. The method for preparing a bimetallic nickel-cobalt-telluride electrode material as set forth in claim 2, wherein Ni is present in the solution in the step (1) in an amount of 0.3 to 1mmol per 0.3 to 1mmol of Ni2+Corresponding to 25-60ml of solvent and corresponding to 1.0-4mmoThe solvent is ethanol or a mixed solution of ethanol and water, and the volume ratio of the ethanol to the water in the mixed solution is 1: 0-5.
4. The method for preparing a bimetallic nickel-cobalt telluride electrode material as set forth in claim 2, wherein the concentration of the sodium tellurite aqueous solution in the step (2) is 0.1-10 mM; the dosage of hydrazine hydrate is: every 70ml of sodium tellurite aqueous solution corresponds to 2-10ml of 80% hydrazine hydrate.
5. The method for preparing a bimetallic nickel-cobalt-telluride electrode material as in claim 2, wherein Ni is2 +And Co2+Is added in the form of nitrate.
6. The method for producing a bimetallic nickel-cobalt-telluride electrode material as claimed in claim 1 or 2, characterized in that Ni is adjusted2+And Co2+Mixing solvents of the solution to obtain nickel-cobalt precursors with different morphologies, and adjusting and controlling the morphology of the bimetal nickel-cobalt telluride by adjusting the concentration of sodium tellurite in the reducing aqueous solution and adjusting the reaction time; the appearance of the final product bimetal nickel cobalt telluride on the conductive substrate is one or more of nano sheets, nano needles, nano tubes and nano rods.
7. A bimetallic nickel cobalt telluride electrode material prepared according to the method of any one of claims 1 to 6.
8. Use of a bimetallic nickel cobalt telluride electrode material prepared by a process as claimed in any one of claims 1 to 6 as a positive electrode material.
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| CN111524718A (en) * | 2020-04-11 | 2020-08-11 | 中南民族大学 | Method for preparing asymmetric supercapacitor by using hydrophilic carbon nanotube film and hyperbranched polymer as double templates |
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| CN114351183A (en) * | 2022-01-06 | 2022-04-15 | 武汉工程大学 | Tellurium-modified heterojunction catalytic material and preparation method and application thereof |
| CN114429866A (en) * | 2022-02-10 | 2022-05-03 | 杭州瑁昂科技有限公司 | Planar filtering electrochemical capacitor and preparation method thereof |
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| CN114725372A (en) * | 2022-04-24 | 2022-07-08 | 西安建筑科技大学 | Nickel-cobalt bimetallic telluride electrode material for sodium-ion battery and preparation method and application thereof |
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