CN113394030B - Nickel-based electrode material and preparation method and application thereof - Google Patents
Nickel-based electrode material and preparation method and application thereof Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 85
- 239000007772 electrode material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 21
- 230000004913 activation Effects 0.000 claims abstract description 20
- 238000002791 soaking Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- 239000006260 foam Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000003990 capacitor Substances 0.000 claims description 8
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical group [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 229940075397 calomel Drugs 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910000474 mercury oxide Inorganic materials 0.000 claims description 2
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000011230 binding agent Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000001994 activation Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000011149 active material Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000011800 void material Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000000224 chemical solution deposition Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical class [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000003313 weakening effect Effects 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
- H01G11/84—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
-
- 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
-
- 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
-
- 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)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The invention discloses a nickel-based electrode material and a preparation method and application thereof. The nickel-based electrode material is obtained by performing electrochemical activation through cyclic voltammetry and then soaking and activating in water. The preparation method of the invention maintains the three-dimensional structure of the foamed nickel electrode material, avoids the limitation of using a binder and a coating process, thereby improving the utilization rate of active substances, increasing the number of reactive active sites, reducing contact resistance, being beneficial to the transmission of electrons and further improving the charge storage performance of the electrode. In addition, the preparation method is simple, simple in operation and lower in cost, can greatly improve the capacitance performance of the nickel electrode, reduces energy loss, protects the environment and is more suitable for industrial production.
Description
Technical Field
The invention belongs to the field of electrode materials, and particularly relates to a nickel-based electrode material as well as a preparation method and application thereof.
Background
Due to the development of society and science and technology, the demand of human beings on clean and efficient energy is increasing, and the continuous exploration of novel energy storage equipment by scientific researchers at home and abroad is driven. The super capacitor is used as a novel clean energy storage device, has the unique advantages of high charging speed, high power density, long service life, wide working temperature range and the like, is nontoxic and pollution-free in the production process of the raw materials, has high safety, and is an ideal green power supply.
Nickel oxides and hydroxides are favored for their high void fraction, high specific capacitance, low cost, and the like, making them promising for application in supercapacitors. The foam nickel net has good performances in corrosion resistance, electric conduction and the like; the composite material has a three-dimensional reticular structure, high void ratio, large specific surface area, uniform quality and certain advantages in the structure; and the nickel-based capacitor material has higher theoretical specific capacitance, better thermal stability and lower price, so the nickel-based capacitor material is an ideal electrode substrate material. The nickel hydroxide with the lamellar structure has larger interlayer spacing and higher theoretical specific capacitance, and becomes a hot gate electrode material of a super capacitor.
However, most of the reported methods are carried out under severe conditions of high temperature and high pressure, strong acid and strong alkali, etc., for example, Yuan et al use Chemical Bath Deposition (CBD) method to put foamed nickel in 40ml of NiSO with 1mol/L 4 30ml of 0.25mol/L K 2 S 2 O 8 10mL of ammonia water (25% -28% NH) 3 ) And 20mL of deionized water, stirring the mixed solution at 300rpm for 1 hour at 20 ℃, taking out, washing and drying. Therefore, the method which is milder and has less damage to instruments and equipment is more suitable for the requirement of industrial production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a nickel-based electrode material, which specifically adopts the following technical scheme:
a preparation method of a nickel-based electrode material comprises the following steps:
step one, electrochemical activation: taking foamed nickel as a working electrode, platinum as an auxiliary electrode, and an Ag/AgCl electrode, a mercury oxide electrode or a calomel electrode as a reference electrode, and performing cyclic voltammetry scanning for 25-200 circles in 1mol/L inorganic salt solution under a voltage window of 0-1.5V, wherein the scanning speed is 5 mV/s; the inorganic salt is magnesium sulfate, aluminum sulfate, sodium sulfate, magnesium nitrate or ferric sulfate;
step two, soaking and activating: and then soaking the scanned foamed nickel in water at 60 ℃ for 5-70h to obtain the nickel-based electrode material.
The method takes the foamed nickel as a substrate and a nickel source at the same time, and grows the nickel hydroxide thin layer on the nickel substrate in situ in a mode of electrochemical activation and water soaking activation in sequence. The electrochemical test result shows that the prepared electrode material has better capacitance performance, the method adopted by the invention breaks through the limitation of other harsh conditions such as high temperature, strong acid and strong alkali and the like in the past, and a new way is developed for preparing high-performance electrode materials.
In some preferred embodiments, before step one, a pretreatment step is further included, specifically comprising: and (4) ultrasonically cleaning the foamed nickel by using water and absolute ethyl alcohol in sequence, and drying.
In some preferred embodiments, the nickel foam has a size of: the length is 1cm, the width is 1cm, and the thickness is 0.3 mm.
In some preferred embodiments, the drying conditions are: the drying temperature is 60 ℃, and the drying time is 2 h.
In some preferred embodiments, the window voltage is 0-1.2V.
In some preferred embodiments, the number of cycles of the cyclic voltammetry scan is 100 cycles.
In some preferred embodiments, the nickel foam after scanning is soaked in water at 60 ℃ for 50 h.
The invention also provides a nickel-based electrode material prepared by the preparation method, and the nickel-based electrode material can be applied to batteries and/or capacitors.
The beneficial effects of the invention are as follows:
(1) the foam nickel net has a three-dimensional net structure, high void ratio, large specific surface and uniform quality, and has certain advantages in the structure; and the nickel-based capacitor material has high theoretical specific capacitance, good thermal stability and low price, thereby belonging to an ideal electrode substrate material.
(2) The preparation method of the invention maintains the three-dimensional structure of the foamed nickel electrode material, avoids the limitation of using a binder and a coating process, thereby improving the utilization rate of active substances, increasing the number of reactive active sites, reducing contact resistance, being beneficial to the transmission of electrons and further improving the charge storage performance of the electrode.
(3) The preparation method is simple, simple in operation and lower in cost, can greatly improve the capacitance performance of the nickel electrode, reduces the energy loss, protects the environment, and is more suitable for industrial production.
Drawings
FIG. 1 is an SEM image of the electrode surface after different treatment methods;
FIG. 2 is a graph showing the results of electrochemical performance of electrodes treated by different treatment methods;
FIG. 3 is a graph showing the electrochemical performance results of the electrode after two-step activation treatment under different voltage window conditions;
FIG. 4 is a diagram showing the results of electrochemical performance of the electrode after two-step activation treatment under different numbers of scanning cycles;
FIG. 5 is a graph showing the results of the electrochemical performance of the electrode after two-step activation under different soaking time conditions.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments and the accompanying drawings to fully understand the objects, aspects and effects of the present invention.
Example 1:
a foamed nickel electrode is prepared by the following steps:
(1) pretreatment of foamed nickel: shearing porous foamed nickel with the thickness of 1cm x 0.3mm, sequentially carrying out ultrasonic cleaning by using deionized water and absolute ethyl alcohol, removing oil stains and dust on the surface of the nickel net and in grids, and drying for 2 hours at 60 ℃ for later use;
(2) two-step activation: a three-electrode system (an auxiliary electrode is a platinum sheet electrode, pretreated foamed nickel is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode) is adopted, in 1mol/L magnesium sulfate solution, Cyclic Voltammetry (CV) scanning is carried out for 100 circles under the window voltage of 0-1.2V, the scanning speed is 5mV/s, the electrochemical activation of the first step is completed, then a nickel net is soaked in deionized water at the temperature of 60 ℃ for 50 hours, the soaking activation of the second step is carried out, and finally the foamed nickel electrode (nickel-based electrode) is obtained.
Comparative example 1:
a nickel foam electrode was prepared without electrochemical activation, and the remainder was identical to example 1, i.e., only the immersion activation process was performed.
Comparative example 2:
a nickel foam electrode was prepared without a soaking activation process, and the rest was identical to example 1, i.e., only an electrochemical activation process was performed.
Effect verification experiment:
(1) the SEM images of the nickel foam electrodes obtained in example 1 (abbreviated as N12), comparative example 1 (abbreviated as N2), and comparative example 2 (abbreviated as N1), and the nickel foam without any activation process (only pre-treatment) (hereinafter referred to as control or N0) are shown in fig. 1, wherein fig. 1(a) is the SEM image of the nickel foam surface of the control, and it can be seen that the nickel foam surface is smoother and has no impurities and defects; fig. 1(b) is an SEM image of the surface of the nickel foam electrode of comparative example 1, and it can be seen that a small amount of thin film structure appears on the surface of the resulting nickel foam electrode; fig. 1(c) is an SEM image of the surface of the nickel foam electrode of comparative example 2, and it can be seen that the surface of the resulting nickel foam electrode becomes rough and a large number of fine pores are generated; fig. 1(d) is an SEM image of the surface of the foamed nickel electrode of example 1, and it can be seen that a large number of nanosheets grown on the surface of the foamed nickel electrode stand on the surface of the nickel substrate, and present in a honeycomb shape, and this structure is more favorable for increasing the specific surface area of the active material, and in addition, as the active material directly grows on the foamed nickel current collector, the loss caused by the binder is reduced, thereby improving the utilization rate of the active material and contributing to improving the electrochemical performance of the electrode material.
(2) Electrochemical performance tests are carried out on the foamed nickel of example 1, comparative examples 1-2 and a control group, and the results are shown in figure 2:
fig. 2(a) is a graph comparing CV curves of the nickel foam after different treatment modes at a sweep rate of 5mV/s, and it can be seen that the CV curve area of the nickel foam of comparative example 1 is improved compared with that of a control group, but the CV scan area of the nickel foam of example 1 is larger compared with that of the other three groups, which illustrates that the effect of two-step activation in example 1 is better.
Fig. 2(b) is a CV curve graph of the nickel foam after different treatment modes at scanning rates of 5, 10, 20, 50 and 100mV/s, and it can be seen that each curve shows a corresponding redox peak, the material, surface nickel foam, can perform highly reversible redox reaction, when the scanning rate is increased, the position of the redox peak is respectively shifted to two sides due to different diffusion rates of electrons and ions when the redox reaction occurs, while the nickel foam prepared in example 1 shows the largest CV curve area, which indicates that the specific capacitance of the nickel foam after two-step activation is larger.
FIG. 2(c) shows the foamed nickel at 2mA/cm after different treatment modes 2 The charging and discharging curve under the current density can be visually seen from the figure, the charging and discharging time is greatly increased by the two-step activation, and the charge storage performance is greatly improved.
Fig. 2(d) is a graph of the area specific capacitance of the nickel foam after different treatment modes and the corresponding current density, and it can be seen that the area specific capacitance of the nickel foam after two steps of activation is higher than that of the comparative examples 1-2 and the control group at any current density, which shows that the nickel foam after two steps of activation has better area specific capacitance and better rate performance.
(3) After changing the voltage window in example 1, the electrochemical performance of the foamed nickel after two-step activation was tested, and the results are shown in fig. 3:
fig. 3(a) is a CV curve graph of the nickel foam electrode obtained in the voltage windows of 0-0.5, 0-0.8, 0-1.0, 0-1.2, and 0-1.5V, and it can be seen that the integrated area of the CV curve increases with the increase of the voltage window, and the integrated area of the CV curve is the largest in the voltage window of 0-1.2V.
FIG. 3(b) shows that the current density of the foamed nickel electrode obtained at different voltage windows is 2mA/cm 2 When the voltage window is 0-0.5, 0-0.8, 0-1.0, 0-1.2 and 0-1.5V, the area specific capacitance is 301, 670, 765, 997 and 530mF/cm in sequence 2 The optimum voltage window is shown to be 0-1.2V, with results consistent with CV results.
Fig. 3(c) is a point line graph of the area specific capacitance of the nickel foam electrode obtained in different voltage windows under different current densities, and it can be known from the graph that the area specific capacitance shows a descending trend along with the increase of the current density, and the descending trend is rapid and then gentle.
In the above test, when the voltage window is continuously increased to 0-1.5V, the capacitance and rate capability of the electrode are reduced, and it may be that the hydrogen oxide layer on the surface of the electrode is too thick, and the active material therein is difficult to be fully utilized, thereby weakening the mass-charge transfer capability of the surface of the electrode and reducing the electrochemical performance thereof.
(4) The number of scanning cycles in example 1 was changed, and the electrochemical performance of the foamed nickel after two-step activation was measured, and the results are shown in fig. 4:
the CV curve of the nickel foam electrode obtained at 5mV/s sweep rate for different sweep times of fig. 4(a) shows that the CV curve area of the obtained electrode increases with the increase of the sweep times, and the CV curve area of the obtained electrode is the largest when the sweep times are 100, which indicates that the capacitance performance is the best.
FIG. 4(b) shows the current density of the foamed nickel electrode obtained at different scanning turns of the electrode at 2mA/cm 2 The area specific capacitance of the time-lapse charge-discharge curve is respectively 701, 997, 1059 and 1022mF/cm when the number of scanning turns is 25, 50, 100 and 200 turns by calculation 2 The result was consistent with the CV curve.
Fig. 4(c) is a graph comparing the electrode capacitance of the nickel foam electrode obtained at different scanning turns under different current densities, and it can be seen visually that the optimal scanning turn is 100 turns, and furthermore, as the current density increases, the area specific capacitance gradually decreases, which is influenced by the internal resistance of the electrode.
Fig. 4(d) Nyquist plots of the foamed nickel electrodes obtained at different scanning turns (the inset/small plot is an enlarged view of the high frequency region), it can be seen from the figure that the Nyquist curve at the low frequency region is approximately a straight line, and the slope of the straight line is the largest when the scanning turns are 100 turns, which indicates that the diffusion resistance of the electrode is small at this time, and the electrode has better capacitance performance.
(5) The soaking time in example 1 was changed, and the electrochemical performance of the foamed nickel after two-step activation was measured, and the results are shown in fig. 5:
fig. 5(a) is a CV curve graph of the nickel foam electrode obtained at different soaking times (5, 10, 30, 50, and 70h, respectively) at a sweeping speed of 5mV/s, and it can be seen from the graph that the CV curves corresponding to 5 electrodes show more obvious and symmetrical redox peaks, which indicates that the reversibility of the electrode and the electrode reaction thereof under the conditions is enhanced.
FIG. 5(b) foamed nickel electrodes obtained at different soaking times at 2mA/cm 2 The charge and discharge curves at current density are compared, and it can be seen from the graph that these curves are not completely symmetrical, just conforming to the characteristics of the faraday capacitor, and in contrast, the discharge time of the electrode soaked for 50h is the longest, indicating that it has better rate performance.
Fig. 5(c) is a graph comparing the capacitance of the nickel foam electrode obtained at different current densities for different soaking times, and it can be seen that the area specific capacitance gradually decreases under the condition of increasing current density.
Fig. 5(d) is a Nyquist point diagram (an inset graph/a small graph is an enlarged graph of a high frequency region) of the electrode of the foamed nickel electrode obtained at different soaking times, and it is found through observation that a Nyquist curve corresponding to the prepared electrode is almost intersected with a horizontal axis at one point, which shows that the internal resistance of the electrodes has small difference, and it can be seen from the low frequency region that the slope of a straight line of the electrode obtained by soaking for 50 hours is the largest and the ion diffusion rate is the fastest.
In summary, soaking for 50h is the best time.
The above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above embodiment, and the present invention shall fall within the protection scope of the present invention as long as the technical effects of the present invention are achieved by the same means. The invention is capable of other modifications and variations in its technical solution and/or its implementation, within the scope of protection of the invention.
Claims (9)
1. The preparation method of the nickel-based electrode material is characterized by comprising the following steps of:
step one, electrochemical activation: taking foamed nickel as a working electrode, platinum as an auxiliary electrode, and an Ag/AgCl electrode, a mercury oxide electrode or a calomel electrode as a reference electrode, and performing cyclic voltammetry scanning for 25-200 circles in 1mol/L inorganic salt solution under a voltage window of 0-1.5V, wherein the scanning speed is 5 mV/s; the inorganic salt is magnesium sulfate, aluminum sulfate, sodium sulfate, magnesium nitrate or ferric sulfate;
step two, soaking and activating: and then soaking the scanned foamed nickel in water at 60 ℃ for 5-70h to obtain the nickel-based electrode material.
2. The preparation method according to claim 1, further comprising a pretreatment step before the first step, wherein the pretreatment step comprises the following specific steps: and (4) ultrasonically cleaning the foamed nickel by using water and absolute ethyl alcohol in sequence, and drying.
3. The method of claim 2, wherein the nickel foam has a size of: the length is 1cm, the width is 1cm, and the thickness is 0.3 mm.
4. The method of claim 2, wherein the drying conditions are: the drying temperature is 60 ℃, and the drying time is 2 h.
5. The method of claim 1, wherein the voltage window is 0-1.2V.
6. The method of claim 1, wherein the number of cyclic voltammetry scans is 100.
7. The method of claim 1, wherein the scanned nickel foam is soaked in water at 60 ℃ for 50 hours.
8. A nickel-based electrode material, characterized by being produced by the production method according to any one of claims 1 to 7.
9. Use of the nickel-based electrode material according to claim 8 in batteries and/or capacitors.
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| CN202110715975.2A CN113394030B (en) | 2021-06-26 | 2021-06-26 | Nickel-based electrode material and preparation method and application thereof |
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| CN202110715975.2A CN113394030B (en) | 2021-06-26 | 2021-06-26 | Nickel-based electrode material and preparation method and application thereof |
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| CN113394030A CN113394030A (en) | 2021-09-14 |
| CN113394030B true CN113394030B (en) | 2022-09-09 |
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