CN110828192B - Self-supporting high-rate performance electrode based on foamed nickel and preparation method thereof - Google Patents
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims abstract description 23
- 238000004070 electrodeposition Methods 0.000 claims abstract description 23
- 229910003424 Na2SeO3 Inorganic materials 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000011781 sodium selenite Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000007772 electrode material Substances 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 10
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 7
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 6
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 6
- 230000014759 maintenance of location Effects 0.000 abstract description 5
- 229910018143 SeO3 Inorganic materials 0.000 abstract 1
- 239000006260 foam Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 229910017709 Ni Co Inorganic materials 0.000 description 5
- 229910003267 Ni-Co Inorganic materials 0.000 description 5
- 229910003262 Ni‐Co Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000012467 final product Substances 0.000 description 4
- 239000011669 selenium Substances 0.000 description 4
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- -1 nickel and cobalt Chemical class 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PYHYDDIOBZRCJU-UHFFFAOYSA-N [Ni]=[Se].[Co] Chemical compound [Ni]=[Se].[Co] PYHYDDIOBZRCJU-UHFFFAOYSA-N 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
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- 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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- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
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- Electric Double-Layer Capacitors Or The Like (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses a self-supporting high-rate performance electrode based on foamed nickel and a preparation method thereof. The method firstly adopts an electrodeposition method to deposit Ni (OH) on the foamed nickel2‑Co(OH)2Then preparing Na by a hydrothermal method2SeO3Solution, finally adding Ni (OH)2‑Co(OH)2/NF in Na2SeO3Performing hydrothermal reaction selenization in the solution to prepare CoSe2A NiSe electrode. The preparation method is simple and easy to realize, and utilizes Ni (OH)2‑Co(OH)2Method of derivatizing selenization, modulation of CoSe2The shape and content of NiSe, the prepared self-supporting electrode has ultrahigh multiplying power performance of 15mA cm‑2The specific capacitance of the capacitor reaches 17.4F cm‑2And when the current density is increased up to 125mA cm‑2The specific capacitance is still as high as 11.6F cm‑2The specific capacitance retention rate is 67%, and the method is suitable for the super capacitor.
Description
Technical Field
The invention belongs to the technical field of self-supporting electrodes, and relates to a self-supporting high-rate performance electrode based on foamed nickel and a preparation method thereof.
Background
As a novel electrochemical energy storage device, the super capacitor has the advantages of low production cost, simple and efficient production method, green and environment-friendly production process, high charging and discharging efficiency, high power density, long cycle life, wide use temperature range, high charging and discharging speed and the like, and has wide application prospect in the fields of hybrid electric vehicles, aerospace, mobile communication, standby power systems and the like. The performance of the super capacitor is determined by the electrode to a great extent, and the composition and structure of the electrode material are particularly important. The foam nickel has the advantages of a cross-linked network structure, high porosity, high specific surface area, low density, good conductivity and the like, and is often used as a substrate material in an electrode material.
Transition metals, particularly nickel and cobalt, are widely used for research and development of energy storage electrode materials due to their excellent electrochemical properties and abundant natural resources. Ni-Co hydroxides and sulfides have been the focus of research in recent years. ZHou et al synthesized Ni (OH) with hexagonal microcrystalline structure by hydrothermal in-situ growth method2@Co(OH)2The material is a hollow nano hexagon with a core-shell structure, and the current density is 1A g-1In the case of (2), the specific capacitance of the electrode material was 369F g-1After 2500 cycles, the specific capacitance retention rate can be kept at 96.4%, but the electrode can only show good specific capacitance under low current density and can not break through the good performance under high current density (D.Zhou, et al.Ni (OH)2@Co(OH)2hold nanohexagons, Controllable synthesis, face-selected reactive growth and capacity property, Nano Energy 2014,5, 52-59). He topic combination firstly synthesizes a lamellar Ni-Co precursor network, and a large amount of S is generated by hydrothermal anion exchange in the vulcanization process2-Plays a dual role (sulfur source and etchant) responsible for the formation of rich networks of edge sites, S2-Anchored at Ni-Co precursor sites to form Ni3S2/CoNi2S4. Current density of 2A g-1At present, the specific capacitance of the electrode material is 2435F g-1When the current density increased to 20A g-1In this case, the specific capacitance retention rate is 80%, but sulfide is not only toxic but also easily oxidized, so that the electrode stability is poor (W.He, et al3S2/CoNi2S4 3D-network structureforsuperhighenergydensityasymmetric supercapacitors,Advanced Energy Materials,2017,7,1700983)。
Since elemental selenium has lower toxicity and nickel cobalt selenide has better conductivity than other nickel cobalt chalcogen compounds, Ni-Co seleniumThe compound multifunctional material has recently received more and more attention, and electrochemical properties can be greatly improved by preparing a binder-free selenide having various components through in-situ growth. Wang et al firstly prepare a graphene network on foamed nickel by using a vapor deposition method, and then perform a two-step hydrothermal method to obtain NiCo2.1Se3.3NSs/3D G/NF electrode. The current density was 1mA cm-2The specific capacitance of the electrode was 742.4F g-1And when the current density reaches 10mA cm-2When the specific capacitance is 471.78F g-1But at 10mA cm-2When the capacitance is only 83.5 percent after 1000 cycles, the electrode has poor stability, and the electrode material can not keep high specific capacitance under high current density (Y.Wang, et al. Ni-Co selected nano sheet/3D graphene/nickel foam binder-free electrode for high-performance capacitor, ACS applied. Mater. interfaces,2019,11, 7946-.
Lin et al prepare CoSe by two-step hydrothermal method2/Ni0.85Se electrode, which is electrochemically activated before electrochemical test, at a current density of 10C cm-2When the specific capacitance is 3.25 Ccm-2When the current density is 100 Ccm-2When the specific capacitance is reduced to 2.0C cm-2The retention of specific capacitance is yet to be further improved (J.Lin, et al. core-branched CoSe)2/Ni0.85Se nanotube arrays onNi foam with remarkable electrochemicalperformance for hybrid supercapacitors,Journal of Materials Chemistry A,2018,6,19151-19158.)。
Disclosure of Invention
The invention aims to provide a self-supporting high-rate performance electrode based on foamed nickel and a preparation method thereof.
The technical scheme for realizing the purpose of the invention is as follows:
the preparation method of the self-supporting high-rate performance electrode based on the foamed nickel comprises the following specific steps:
Step 3, dissolving sodium hydroxide and selenium powder in water, fully stirring, performing ultrasonic treatment, and performing hydrothermal reaction at 160-200 ℃ to obtain Na2SeO3A solution;
step 4, mixing Ni (OH)2-Co(OH)2/NF soaking in Na2SeO3In the solution, carrying out hydrothermal selenization at 160-200 ℃, washing with water and absolute ethyl alcohol, and drying to obtain CoSe2A NiSe electrode material.
Preferably, in the step 1, the concentration of cobalt nitrate in the mixed solution of cobalt nitrate and nickel nitrate is 0.18-0.22 mol L-1The concentration of the nickel nitrate is 0.18-0.22 mol L-1。
Preferably, in the step 3, the hydrothermal reaction time is 8-16 h.
Preferably, in the step 4, the hydrothermal selenization time is 6-10 h.
Compared with the prior art, the invention has the following advantages:
(1) ni (OH) is deposited on the foam nickel by means of electrodeposition2-Co(OH)2The nano sheet is simple and convenient in method, and precursors of Ni and Co are attached to the foamed nickel more compactly, so that the stability of the electrode is facilitated;
(2) preparation of Binder-free CoSe with multiple Components by hydroxide selenization Using hydrothermal method2The NiSe selenide can greatly improve the electrochemical performance, the original hydroxide is etched in the selenizing process to form more active sites, the specific surface area of the material is effectively increased, the diffusion of electrolyte ions in the electrode is promoted, and the electron transmission is accelerated;
(3) CoSe of the invention2NiSe self-supportingThe support electrode material has ultrahigh multiplying power performance of 15mA cm-2The specific capacitance of the capacitor reaches 17.4F cm-2And when the current density is increased up to 125mA cm-2The specific capacitance is still as high as 11.6F cm-2The specific capacitance retention was 67%.
Drawings
FIG. 1 is a nickel foam based CoSe2A preparation flow chart of a NiSe self-supporting high-rate performance electrode.
FIG. 2 is a direct electrodeposition of Ni (OH) on the nickel foam prepared in comparative example 12-Co(OH)2Nanosheets without selenized Ni (OH)2-Co(OH)2Electrode (a) and electrodeposited Ni (OH) first prepared in example 12-Co(OH)2Then carrying out selenization to obtain CoSe2Scanning electron micrograph of/NiSe electrode (b).
FIG. 3 shows Ni (OH) produced in comparative example 12-Co(OH)2Electrode, CoSe obtained in example 12NiSe electrode, CoSe obtained in example 22NiSe electrode and CoSe obtained in example 32NiSe electrode material at 15mA cm-2Charge and discharge curves at current density.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
Example 1
Step 3, dissolving sodium hydroxide (2.9g) and selenium powder (0.23g) in 30mL deionized water, fully stirring, performing ultrasonic treatment, and performing hydrothermal treatment at 180 ℃ for 8h to prepare the selenium-enriched zinc oxideTo obtain Na2SeO3Cooling the solution to room temperature;
step 4, mixing the Ni (OH) prepared in the step 22-Co(OH)2NF soaking in step 3 to obtain Na2SeO3The solution is subjected to hydrothermal reaction at 180 ℃ for 8h for selenylation, washed by water and absolute ethyl alcohol and dried to obtain CoSe2A NiSe electrode material.
The scanning electron micrograph of the product obtained in example 1 is shown in FIG. 2(b), and CoSe2the/NiSe covers the surface of the nickel foam, so the surface looks rough, presenting etched petals and lamellae. Prepared CoSe2NiSe electrode at 15mA cm-2The charge-discharge curve under the current density is shown as curve d in figure 3, and the specific capacitance is as high as 17.4F cm-2Compared with the final product prepared in the comparative example 1, the specific capacitance is greatly improved, and the electrochemical performance is good.
Comparative example 1
In step 1, cobalt nitrate hexahydrate (2.326g) and nickel nitrate hexahydrate (1.164g) were dissolved in 40mL of deionized water and sufficiently stirred to prepare a clear and transparent electrodeposition solution.
The scanning electron micrograph of the product obtained in comparative example 1 is shown in FIG. 2(a), petal-shaped and nanosheet-shaped Ni (OH)2-Co(OH)2The surface of the foamed nickel is covered densely and uniformly without crowding. Prepared Ni (OH)2-Co(OH)2Electrodes at 15mA cm-2The charge-discharge curve under current density is shown as curve a in FIG. 3, and the specific capacitance reaches 7.7F cm-2Compared with the final product prepared in example 1, the specific capacitance is small, and the electrochemical performance is poor.
Example 2
In step 1, cobalt nitrate hexahydrate (2.326g) and nickel nitrate hexahydrate (1.164g) were dissolved in 40mL of deionized water and sufficiently stirred to prepare a clear and transparent electrodeposition solution.
Step 3, dissolving sodium hydroxide (2.9g) and selenium powder (0.23g) in 30mL deionized water, fully stirring, performing ultrasonic treatment, and performing hydrothermal treatment at 180 ℃ for 8 hours to prepare Na2SeO3Cooled to room temperature.
Step 4, mixing the Ni (OH) prepared in the step 22-Co(OH)2NF soaking in step 3 to obtain Na2SeO3In the solution, the solution is subjected to hydrothermal reaction at 180 ℃ for 6h for selenylation, washed by water and absolute ethyl alcohol and dried to obtain CoSe2NiSe electrode material
Example 2 the product obtained was at 15mA cm-2The charge-discharge curve under the current density is shown as curve b in FIG. 3, and the specific capacitance reaches 13.9F cm-2Compared with the final product prepared in example 1, the specific capacitance is slightly reduced, and the electrochemical performance is general.
Example 3
In step 1, cobalt nitrate hexahydrate (2.326g) and nickel nitrate hexahydrate (1.164g) were dissolved in 40mL of deionized water and sufficiently stirred to prepare a clear and transparent electrodeposition solution.
Step 3, dissolving sodium hydroxide (2.9g) and selenium powder (0.23g) in 30mLFully stirring in ionized water, performing ultrasonic treatment, and performing hydrothermal treatment at 180 ℃ for 8 hours to obtain Na2SeO3Cooled to room temperature.
Step 4, mixing the Ni (OH) prepared in the step 22-Co(OH)2/NF soaking step 3 to obtain Na2SeO3The solution is processed by hydrothermal for 10h selenization at 180 ℃, washed by water and absolute ethyl alcohol and dried to obtain CoSe2A NiSe electrode material.
Example 3 the product obtained was at 15mA cm-2The charge-discharge curve under the current density is shown as curve c in figure 3, and the specific capacitance reaches 14.8F cm-2Compared with the final product prepared in example 1, the specific capacitance is smaller, and the electrochemical performance is general.
Claims (4)
1. The preparation method of the self-supporting high-rate performance electrode based on the foamed nickel is characterized by comprising the following specific steps of:
step 1, dissolving cobalt nitrate hexahydrate and nickel nitrate hexahydrate in water, and fully stirring to prepare an electrodeposition solution;
step 2, taking AgCl/Ag as a reference electrode, a platinum sheet electrode as a counter electrode, foamed nickel as a working electrode, taking the mixed solution of cobalt nitrate and nickel nitrate obtained in the step 1 as an electrodeposition solution, carrying out constant potential electrodeposition with the voltage of-0.8-1.2V and the constant potential deposition time of 600-1200 s, after the electrodeposition is finished, cleaning with water and ethanol, and drying to obtain Ni (OH)2-Co(OH)2/NF；
Step 3, dissolving sodium hydroxide and selenium powder in water, fully stirring, performing ultrasonic treatment, and performing hydrothermal reaction at 160-200 ℃ to obtain Na2SeO3A solution;
step 4, mixing Ni (OH)2-Co(OH)2/NF soaking in Na2SeO3In the solution, hydrothermally selenizing at 180 ℃ for 8h, washing with water and absolute ethyl alcohol, and drying to obtain CoSe2A NiSe electrode material.
2. The method according to claim 1, wherein in step 1, the cobalt nitrate and the nitrate are mixedIn the mixed solution of the nickel acid, the concentration of the cobalt nitrate is 0.18-0.22 mol L-1The concentration of the nickel nitrate is 0.18-0.22 mol L-1。
3. The preparation method according to claim 1, wherein in the step 3, the hydrothermal reaction time is 8-16 h.
4. The self-supporting high rate performance electrode based on foamed nickel prepared by the preparation method according to any one of claims 1 to 3.
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| WO2008102351A2 (en) * | 2007-02-20 | 2008-08-28 | Yissum Research Development Company Of The Hebrew University Of Jerusalem, Ltd. | Hybrid metal-semiconductor nanoparticles and methods for photo-inducing charge separation and applications thereof |
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