CN111261428A - Method for enhancing performance of cobalt nickel sulfide supercapacitor by ammonia plasma - Google Patents
Method for enhancing performance of cobalt nickel sulfide supercapacitor by ammonia plasma Download PDFInfo
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- CN111261428A CN111261428A CN202010123476.XA CN202010123476A CN111261428A CN 111261428 A CN111261428 A CN 111261428A CN 202010123476 A CN202010123476 A CN 202010123476A CN 111261428 A CN111261428 A CN 111261428A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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
Abstract
The invention discloses a method for enhancing the performance of a cobalt nickel sulfide super capacitor by ammonia plasma, which is to treat cobalt nickel sulfide by adopting a plasma chemical vapor deposition (PECVD) system and taking ammonia as a plasma gas source under certain conditions. The electrochemical performance of the sample is evaluated in 1M KOH electrolyte, and the maximum capacity of the cobalt nickel sulfide can reach 3.32F/cm after PECVD treatment2The cycle stability is improved by 14.2% which is about 3 times of that of a sample before PECVD treatment, and the PECVD method can obviously improve the performance of the cobalt nickel sulfide super capacitor.
Description
Technical Field
The invention belongs to the field of super capacitors, and particularly relates to a method for enhancing the electrical property of a cobalt nickel sulfide super capacitor by ammonia plasma.
Background
The super capacitor is an upgrade of a traditional capacitor, the energy density of the super capacitor is larger than that of the traditional capacitor, the power density of the super capacitor is larger than that of a battery, the super capacitor is long in cycle life, safe, environment-friendly, wide in applicable temperature range and the like, and the super capacitor is a novel energy storage device with an application prospect.
The major drawback of supercapacitors is their lower energy density than lithium ion batteries, which hinders their large-scale commercial application. The traditional commercial super capacitor generally uses carbon materials as electrode materials, and the electrode materials store charges by forming an electric double layer between the electrode materials and electrolyte, belong to a physical process and have lower specific capacitance. The pseudocapacitance type electrode material stores charges through highly reversible redox reaction between the active material and the electrolyte, and the pseudocapacitance is about 10-100 times of the electric capacity of an electric double layer under the condition of the same effective area, so that the pseudocapacitance type electrode material has larger energy density.
Cobalt nickel sulfide is a pseudo-capacitor electrode material with great application prospect due to the advantages of high theoretical capacity, multiple redox couples, easy preparation, low cost and the like. However, the conductivity is low, the electron and ion transmission is hindered, the actual capacity is reduced due to low electrochemical reaction activity, and the rate performance and the cycling stability are influenced. The method is compounded with a high-conductivity carbon material to construct an external conductive channel, and is a main measure for optimizing the conductivity of the material at present. When the composite material is compounded with a three-dimensional conductive carbon network, in order to ensure that the active material is fully contacted with the carbon material, the loading capacity of the active material is usually low, which is not beneficial to the energy density of a device; when the carbon layer is coated on the outer surface of the active material, the carbon coating layer is easily damaged by the volume effect in the circulation process, so that the electrical contact between the active material and the carbon material is lost, and the circulation stability of the active material is influenced; at the same time, the introduction of carbon materials also reduces the effective mass of the active material, thereby reducing the energy density of the device.
Disclosure of Invention
The invention aims to solve the problems, starting from the internal electronic structure of cobalt nickel sulfide, treating the cobalt nickel sulfide by ammonia plasma treatment and adopting a plasma chemical vapor deposition method to regulate and control the surface structure of the cobalt nickel sulfide, namely manufacturing surface S vacancies, introducing nitrogen element doping, and optimizing conductivity and ion transmission performance, thereby improving the capacity, rate capability and cycling stability of the electrode, wherein the specific capacitance of the electrode after treatment is about 3 times that of the electrode without treatment, and the cycling stability is improved by at least 14.2%.
The technical scheme of the invention comprises the following steps:
(1) cleaning of the foamed nickel substrate: ultrasonically cleaning and drying the foamed nickel by using tap water, acetone, dilute hydrochloric acid and distilled water in sequence;
(2) preparing a cobalt-nickel precursor: dissolving a certain amount of cobalt nitrate, nickel nitrate and urea in deionized water, stirring until the cobalt nitrate, the nickel nitrate and the urea are fully dissolved, pouring the mixture into a reaction kettle, adding foamed nickel, sealing, performing hydrothermal reaction for a period of time, sequentially washing the mixture by using the deionized water and absolute ethyl alcohol, and naturally drying the mixture to obtain a cobalt-nickel precursor;
(3) preparing cobalt nickel sulfide: adding a sodium sulfide solution into a cobalt-nickel precursor, sealing, carrying out hydrothermal reaction for a period of time, sequentially washing with deionized water and absolute ethyl alcohol, and naturally drying to obtain cobalt-nickel sulfide;
(4) and (3) regulating the pressure and temperature in the cavity of the prepared cobalt nickel sulfide plasma chemical vapor deposition system, applying ammonia plasma, and performing vapor deposition to obtain the cobalt nickel sulfide supercapacitor.
The molar ratio of the cobalt nitrate to the nickel nitrate to the urea is 1:1-2:3.5-6, and the urea can be replaced by ammonium fluoride.
The hydrothermal reaction temperature in the step (2) is 100-.
The concentration of the sodium sulfide solution is 0.05-0.3 mol/L, and the cobalt-nickel precursor is a film sample and is directly put into the sodium sulfide solution.
The hydrothermal reaction temperature in the step (3) is 100-.
The pressure in the cavity of the plasma chemical vapor deposition system in the step (3) is adjusted to 10-4-10-3Pa, the temperature in the cavity is adjusted to be 150 ℃ and 350 DEG C. The flow of the introduced ammonia gas is 10-30sccm, the time is 5-30min, the temperature is 150-.
Compared with the cobalt nickel sulfide which is not treated, the cobalt nickel sulfide prepared by the preparation method of the invention has obviously improved capacity and cycle stability, because: after PECVD treatment, more sulfur vacancies are generated on the surface of the cobalt nickel sulfide, and more nitrogen elements are doped, so that the conductivity of the cobalt nickel sulfide is higher, and finally, the electrochemical reaction activity, the rate capability and the cycling stability are obviously improved.
Drawings
FIG. 1 is a graph showing the charge and discharge curves of cobalt nickel sulfide electrodes before and after PECVD treatment in examples 1 and 2.
FIG. 2 is a graph showing specific capacitance curves of cobalt nickel sulfide electrodes at different current densities before and after PECVD treatment in examples 1 and 2.
FIG. 3 is a graph showing the cycle stability of cobalt nickel sulfide electrodes before and after PECVD treatment in examples 1 and 2 (current density of 20 mA/cm)2)。
FIG. 4 is an EIS curve of cobalt nickel sulfide electrodes before and after PECVD treatment in examples 1 and 2.
FIG. 5 is a graph showing the charge and discharge curves of cobalt nickel sulfide electrodes before and after the PECVD treatment in examples 3 and 4.
FIG. 6 is a graph of specific capacitance of cobalt nickel sulfide electrodes at different current densities before and after PECVD treatment in examples 3 and 4.
FIG. 7 is an EIS curve of cobalt nickel sulfide electrodes before and after PECVD treatment in examples 3 and 4.
The specific implementation mode is as follows:
in order to further understand the summary and features of the present invention, several examples of the present invention are given below, and it should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
The experimental procedures in the following examples are conventional unless otherwise specified.
Example 1
(1) Cleaning of the foamed nickel substrate: and ultrasonically cleaning the foamed nickel by using tap water, acetone, dilute hydrochloric acid and distilled water in sequence and drying.
(2) Preparing a cobalt-nickel precursor: weighing 2mmol of nickel chloride, 4mmol of cobalt nitrate and 12mmol of urea, dissolving in 35mL of deionized water, magnetically stirring until the nickel chloride, the cobalt nitrate and the urea are completely dissolved, and transferring the solution to a polytetrafluoroethylene lining. And putting the foamed nickel into the lining, covering the lining and the stainless steel outer sleeve, putting the lining and the stainless steel outer sleeve into an oven, and reacting for 7 hours at the temperature of 120 ℃. After the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, sequentially washing the foamed nickel by deionized water and absolute ethyl alcohol, and drying at the temperature of 60 ℃.
(3) Preparing cobalt nickel sulfide: preparing a sodium sulfide solution with the concentration of 0.2mol/L, pouring the sodium sulfide solution into a lining of a reaction kettle, putting the sample obtained in the step (2) into the reaction kettle, sealing, heating for 6 hours at the temperature of 120 ℃, washing with deionized water and absolute ethyl alcohol in sequence, and naturally drying.
(4) PECVD treatment: putting the sample obtained in the step (3) into a cavity of a PECVD system, fixing the sample on a sample table, and reducing the vacuum degree of the PECVD system to 10-4Pa, when the temperature is increased to 250 ℃, applying ammonia plasma, wherein the flow of ammonia is 15sccm, the ventilation duration is 15min, the pressure is 60Pa, and the power is 250W. (5) The electrode is used as a working electrode, a platinum electrode is used as a counter electrode, a mercury oxide electrode is used as a reference electrode, a three-electrode testing system is formed, 1M KOH is used as electrolyte, and a CHI760E electrochemical testing system is adopted. Electrochemical test results show that the charging and discharging time of the electrode after PECVD treatment is obviously longer than that of the sample before treatment (shown in figure 1), and according to a capacity calculation formula:
the current density is 6mA/cm2When the specific capacitance is larger than the maximum specific capacitance, the specific capacitance is 3.23F/cm2Even if the current density is increased to 50mA/cm2The specific capacitance is still as high as 2.38F/cm2(FIG. 2); in contrast, the current density of the electrode before PECVD treatment was 10mA/cm2When the specific capacitance is 1.3F/cm2When the current density is 50mA/cm2When the capacity is reduced to 0.83F/cm2. FIG. 3 shows the current density of the cobalt nickel sulfide electrode at 20mA/cm before and after PECVD treatment2Under the conditions of (1) obtaining a stable cycleQualitatively, it can be seen that the cycling stability of the electrode is improved by 14.2% after the PECVD treatment. FIG. 4 is a comparison of Electrochemical Impedance (EIS) graph, and the enlarged EIS graph and the equivalent circuit graph are inserted, and it can be analyzed that the internal resistance (Rs) of the electrode after PECVD treatment is reduced from 1.41 to 1.38 Ω, and the ion diffusion resistance is also obviously reduced (i.e. the slope of the straight line of the EIS curve is obviously increased).
Example 2
The same as example 1 except that PECVD was not performed, was performed as compared with example 1. The test results are shown in FIGS. 1-4.
Example 3
(1) Cleaning of the foamed nickel substrate: and ultrasonically cleaning the foamed nickel by using tap water, acetone, dilute hydrochloric acid and distilled water in sequence and drying.
(2) Preparing a cobalt-nickel precursor: 1mmol of nickel nitrate, 1mmol of cobalt nitrate and 3.5mmol of ammonium fluoride are weighed, dissolved in 35mL of deionized water, and the solution is transferred to a polytetrafluoroethylene lining after being magnetically stirred until the solution is completely dissolved. And putting the foamed nickel into the lining, covering the lining and the stainless steel outer sleeve, putting the lining and the stainless steel outer sleeve into an oven, and reacting for 8 hours at the temperature of 120 ℃. After the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, sequentially washing the foamed nickel by deionized water and absolute ethyl alcohol, and drying at the temperature of 60 ℃.
(3) Preparing cobalt nickel sulfide: preparing a sodium sulfide solution with the concentration of 0.1mol/L, pouring the sodium sulfide solution into a lining of a reaction kettle, putting the sample obtained in the step (2) into the reaction kettle, sealing, heating for 6 hours at the temperature of 120 ℃, washing with deionized water and absolute ethyl alcohol in sequence, and naturally drying.
(4) PECVD treatment: putting the sample obtained in the step (3) into a cavity of a PECVD system, fixing the sample on a sample table, and reducing the vacuum degree of the PECVD system to 10-4Pa, when the temperature is increased to 300 ℃, applying ammonia plasma, wherein the flow of ammonia is 15sccm, the ventilation duration is 10min, the pressure is 60Pa, and the power is 250W.
(5) The electrode is used as a working electrode, a platinum electrode is used as a counter electrode, a mercury oxide electrode is used as a reference electrode, a three-electrode testing system is formed, 1M KOH is used as electrolyte, and a CHI760E electrochemical testing system is adopted. The electrochemical test results show that after PECVD treatmentThe discharge time of the electrode was significantly longer than the sample before treatment (fig. 5), indicating a significant increase in the capacity of the electrode. According to a capacity calculation formula:
the current density is 5mA/cm2When the specific capacitance is 1.23F/cm2The current density was increased to 50mA/cm2The specific capacitance is still as high as 1F/cm2(FIG. 6); in contrast, the current density of the electrode before PECVD treatment was 5mA/cm2Although the capacitance is 1.13F/cm2However, when the current density is 30mA/cm2When the volume is reduced to 0.75F/cm2The rate performance is clearly worse than the treated samples. FIG. 7 is a comparison of Electrochemical Impedance (EIS) graph, and the enlarged EIS graph and the equivalent circuit graph are inserted, and it can be analyzed that the internal resistance (Rs) of the electrode after PECVD treatment is reduced from 2.46 to 1.96 omega, and the ion diffusion resistance is also obviously reduced (i.e. the slope of the straight line of the EIS curve is obviously increased).
Example 4
Compared with example 3, the same effects as in example 3 were obtained except that no PECVD was performed, as shown in FIGS. 5, 6 and 7.
Claims (7)
1. A method for enhancing the performance of a cobalt nickel sulfide supercapacitor by ammonia plasma is characterized by comprising the following steps:
(1) cleaning of the foamed nickel substrate: ultrasonically cleaning and drying the foamed nickel by using tap water, acetone, dilute hydrochloric acid and distilled water in sequence;
(2) preparing a cobalt-nickel precursor: dissolving a certain amount of cobalt nitrate, nickel nitrate and urea in deionized water, stirring until the cobalt nitrate, the nickel nitrate and the urea are fully dissolved, pouring the mixture into a reaction kettle, adding foamed nickel, sealing, performing hydrothermal reaction for a period of time, sequentially washing the mixture by using the deionized water and absolute ethyl alcohol, and naturally drying the mixture to obtain a cobalt-nickel precursor;
(3) preparing cobalt nickel sulfide: putting the cobalt-nickel precursor into a sodium sulfide solution, sealing, carrying out hydrothermal reaction for a period of time, sequentially washing the cobalt-nickel precursor with deionized water and absolute ethyl alcohol, and naturally drying the cobalt-nickel precursor to obtain cobalt-nickel sulfide;
(4) and (3) regulating the pressure and temperature in the cavity of the prepared cobalt nickel sulfide plasma chemical vapor deposition system, applying ammonia plasma, and performing vapor deposition to obtain the cobalt nickel sulfide supercapacitor electrode.
2. The method for enhancing the performance of the cobalt nickel sulfide supercapacitor by ammonia gas plasma according to claim 1, wherein the molar ratio of the cobalt nitrate to the nickel nitrate to the urea in the step (2) is in the range of 1:1-2:3.5-6, and the urea can be replaced by ammonium fluoride.
3. The method for enhancing the performance of the cobalt nickel sulfide supercapacitor by using the ammonia gas plasma as claimed in claim 2, wherein the hydrothermal reaction temperature in the step (2) is 100 ℃ and 140 ℃, and the hydrothermal reaction time is 5-10 h.
4. The method for enhancing the performance of the cobalt nickel sulfide supercapacitor by ammonia gas plasma according to claim 3, wherein the concentration of the sodium sulfide solution is 0.05-0.3 mol/L.
5. The method for enhancing the performance of the cobalt nickel sulfide supercapacitor by using the ammonia gas plasma as claimed in claim 4, wherein the hydrothermal reaction temperature in the step (3) is 100 ℃ and 140 ℃, and the hydrothermal reaction time is 5-10 h.
6. The method for enhancing the performance of a cobalt nickel sulfide supercapacitor by ammonia plasma according to claim 5, wherein the pressure in the cavity of the plasma chemical vapor deposition system is adjusted to 10-4-10-3Pa, regulating the temperature in the cavity to be 150-350 ℃.
7. The method as claimed in claim 6, wherein the flow rate of the introduced ammonia gas is 10-30sccm, the time is 5-30min, the temperature is 150-350 ℃, the sputtering power is 100-400W, and the sputtering pressure is 40-80 Pa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113174584A (en) * | 2021-01-16 | 2021-07-27 | 黄辉 | Porous nitride electrode and preparation method and application thereof |
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| CN113174584A (en) * | 2021-01-16 | 2021-07-27 | 黄辉 | Porous nitride electrode and preparation method and application thereof |
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