CN109243850B - Ni-Co oxide nanocrystalline and controllable synthesis method and application thereof - Google Patents
Ni-Co oxide nanocrystalline and controllable synthesis method and application thereof Download PDFInfo
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- CN109243850B CN109243850B CN201811310079.2A CN201811310079A CN109243850B CN 109243850 B CN109243850 B CN 109243850B CN 201811310079 A CN201811310079 A CN 201811310079A CN 109243850 B CN109243850 B CN 109243850B
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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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
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to the field of material chemistry, in particular to Ni-Co oxide nanocrystals and a controllable synthesis method and application thereof. The Ni-Co oxide nanocrystalline with a solid sphere structure is controllably synthesized by changing the synthesis conditions such as the amount of the solvent, the calcination temperature and the like and the process. The preparation process is simple, the process control is strong, the synthesis time is short, and the method has good industrial application prospect. Meanwhile, the Ni-Co oxide nanocrystalline prepared by the method has excellent performance of a solid asymmetric flexible supercapacitor, can be bent, can be rapidly charged and discharged, has high-efficiency electric energy storage performance, and has important guiding significance for the technical development of renewable energy sources.
Description
Technical Field
The invention relates to the field of material chemistry, in particular to the field of synthesis and application of nanocrystals, and more particularly relates to a Ni-Co oxide nanocrystal and a controllable synthesis method and application thereof.
Background
Ni-Co oxide refers to an oxide having NiCo2O4A compound oxide of the formula. Since the composite compound has excellent conductivity and electrochemical activity, the research on the Ni — Co oxide has been a hot problem in the field of material chemistry, particularly in the research field of supercapacitors in recent years.
For example, NiCo having a spinel structure as disclosed in the prior art has been disclosed2O4Black nano-powder. NiCo disclosed by T.Y.Wei et al2O4Gel, NiCo, published by H.L.Wang et al2O4A nanowire. And NiCo disclosed by G.Q.Zhang et al2O4Nanoneedles, and the like.
Different NiCo2O4The structure may provide different electrical properties, that is, the electrical properties of the nanocrystals have a large dependence on the nanocrystal structure and size. Therefore, controlling the formation of nanocrystalline structures through a careful, controllable synthesis method is an important means and method for obtaining nanocrystals with different electrical properties and the like. In other words, different nanocrystal structures may exhibit different electrical properties, and therefore, for a new electrical application, it is crucial to find a nanocrystal structure that satisfies the requirements and a controllable synthesis method for obtaining the nanocrystal structure.
With the popularization of portable electronic devices and the vigorous development of electric automobiles, people have higher and higher requirements on the performance of energy storage materials, but the development of the energy storage materials is lagged. On one hand, the energy density of the energy storage material is insufficient, so that the service time of the electric appliance is too short, the charging is frequent, serious inconvenience is brought to daily use, and the use of the electric automobile is also greatly limited. On the other hand, the power of the energy storage material is insufficient, so that the charging time of the energy storage material is too long.
In recent years, with the rise of wearable portable electronic devices, the problems of insufficient energy density and insufficient power of energy storage materials are more prominent. Meanwhile, due to the introduction of "wearable", a new requirement is put on the energy storage device, namely, the energy storage device is required to have flexibility.
Literature research shows that the transition metal is widely applied to energy storage materials due to good reversibility and high reaction speed in the oxidation and reduction processes. For example, Yaning et al found Fe2O3The mixture of nanoclusters and rGO has good properties as the negative electrode of a flexible supercapacitor, and has high energy density and power density. Can show that the graphene composite material has better current activity, which is mainly related to graphiteThe graphene serves as a framework structure to be a good carrier, and meanwhile, the graphene has excellent conductivity.
Therefore, the energy storage material manufactured by using the transition metal has the potential of preparing a flexible super capacitor. Therefore, the research and development of an efficient synthesis method of the transition metal nanocrystalline with a special structure is a hot spot of the current research, and particularly, the method has important significance and great challenges for an electrode material which can be used for an all-solid-state asymmetric flexible supercapacitor.
Disclosure of Invention
The invention aims to solve the technical problem of disclosing an electrode material which can be used for an all-solid-state asymmetric flexible supercapacitor, thereby meeting the requirements of wearable portable electronic equipment on an energy storage device and providing a basis for the development of the wearable portable electronic equipment.
In order to solve the technical problems, the invention discloses Ni-Co oxide nanocrystals which are solid nanosphere-shaped structures.
Furthermore, the invention also discloses that the Ni-Co oxide nanocrystal is a solid nano spherical structure with the diameter of 3-5 nm.
Meanwhile, the invention also discloses a controllable synthesis method of the Ni-Co oxide nanocrystal, which comprises the following steps:
s1: mixing Ni (CH)3COO)2·4H2O、Co(CH3COO)2·4H2Adding O into a mixed solution of Oleic Acid (OA), dodecylamine and Octadecene (ODE);
s2: gradually heating to 180 ℃;
s3: keeping the temperature at 180 ℃ for reaction to obtain a precursor containing Ni-Co oxide nanocrystals;
s4: dispersing, settling and centrifuging;
s5: gradually heating to 350 ℃;
s6: and calcining at 350 ℃ to obtain the Ni-Co oxide nanocrystal.
Meanwhile, Ni (CH) is further disclosed in the present invention3COO)2·4H2O、Co(CH3COO)2·4H2O, Oleic Acid (OA), dodecylamine and Octadecene (ODE) are added in the ratio of Ni (CH)3COO)2·4H2When O is 3.62mmol, Co (CH)3COO)2·4H2The amount of O added was 1.81mmol, the amount of ODE added was 10mL, the amount of dodecylamine added was 5mL, and the amount of OA added was 5 mL.
Preferably, the temperature rising rate in the step S2 is 3-4 ℃ min-1。
Further preferably, the reaction is carried out in step S3 for 18 hours while maintaining the temperature at 180 ℃.
In a preferred embodiment, the step S4 uses an absolute ethanol-n-heptane mixed solution for dispersion and sedimentation. Further preferably, the mixing volume ratio of the absolute ethyl alcohol to the n-heptane is 1: 1.
Further preferably, the step S4 further includes washing after the dispersion sedimentation and the centrifugation.
In a preferred technical scheme, the washing adopts an absolute ethyl alcohol-n-heptane mixed solution. Further preferably, the mixing volume ratio of the absolute ethyl alcohol to the n-heptane is 1: 1.
As another preferable technical means, the temperature rise rate in the step S5 is 10 ℃ min-1。
And as a preferable technical means, the calcination is performed for 1 hour under the condition of keeping the temperature at 350 ℃ in the step S6.
Finally, the invention also discloses application of the Ni-Co oxide nanocrystalline in a solid asymmetric flexible supercapacitor electrode material.
The Ni-Co oxide nanocrystalline prepared by the invention has excellent performance of a solid asymmetric flexible super capacitor, can be bent, can be rapidly charged and discharged, and has high-efficiency electric energy storage performance. Through detection, the performance of the flexible super capacitor is superior to that of the current commercial asymmetric flexible super capacitor, and the flexible super capacitor has important guiding significance for the technical development of renewable energy sources.
Meanwhile, the Ni-Co oxide nanocrystalline with a solid sphere structure is controllably synthesized by a controllable synthesis method through changing the synthesis conditions such as the amount of a solvent, the calcination temperature and the like and a process. The preparation process is simple, the process control is strong, the synthesis time is short, the standard of industrial production is met, and the method has good industrial application prospect.
Drawings
FIG. 1 is a TEM image of Ni-Co oxide nanocrystals synthesized in the present invention.
FIG. 2 is a chart of Cyclic Voltammetry (CV) of Ni-Co oxide nanocrystals synthesized in accordance with the present invention.
FIG. 3 is a constant current charge and discharge (GCD) diagram of Ni-Co oxide nanocrystals synthesized by the present invention.
FIG. 4 is a cyclic voltammogram of a Ni-Co oxide nanocrystal synthesized in accordance with the present invention when unbent; the photograph is shown in the unbent state.
FIG. 5 is a cyclic voltammogram of the Ni-Co oxide nanocrystals synthesized in accordance with the present invention after being bent; the picture therein is a representation of the state of the bend detection.
Detailed Description
In order that the invention may be better understood, we now provide further explanation of the invention with reference to specific examples.
Example 1
0.9008g of Ni (CH) were weighed at room temperature (25. + -. 5 ℃ C.)3COO)2·4H2O and 0.4509g of Co (CH)3COO)2·4H2O was poured into a Teflon liner containing 10mL of Octadecene (ODE), 5mL of dodecylamine, and 5mL of Oleic Acid (OA), magnetically stirred for 15min and placed in a stainless steel reaction kettle, and the kettle lid was tightened. Placing in an oven, adjusting the temperature to 180 deg.C, and heating at 3-4 deg.C/min-1After the temperature reached 180 ℃, the reaction was continued for 18 hours. After the reaction is finished, cooling to room temperature, opening the reaction kettle, adding a proper amount of absolute ethyl alcohol-n-heptane (the volume ratio is 1:1) for dispersion, and centrifugally separating solids. Washing the solid with n-heptane-anhydrous ethanol (volume ratio 1:1), vacuum drying in a vacuum drying oven overnight, placing in a muffle furnace, adjusting temperature to 350 deg.C, and heating at 10 deg.C/min-1，And when the temperature reaches 350 ℃, continuously calcining for 1 hour to obtain the Ni-Co oxide nanocrystalline.
Example 2
The Ni-Co oxide nanocrystal product obtained in example 1 was examined by a Transmission Electron Microscope (TEM), and the result is shown in fig. 1, from which fig. 1 it can be seen that the Ni-Co oxide nanocrystal has a solid sphere nanocrystal structure and a diameter of 3-5 nm.
Example 3
The electrochemical properties of the Ni-Co oxide nanocrystal sample (hereinafter referred to as sample) obtained in example 1 were tested in a two-electrode system by cyclic voltammetry and constant current charge-discharge methods, and the specific procedure was as follows:
the electrochemical experiments were carried out on an electrochemical workstation model CHI660d, using a two-electrode test system, the corresponding positive electrode being a sample-modified nickel foam electrode as obtained herein. The negative electrode is a foam nickel electrode modified by active carbon. All potentials herein are relative to RHE. The electrolyte was a 3M KOH solution. All electrochemical tests were performed at 25 ℃. At each experiment, all electrodes were tested in 3M KOH solution.
The preparation method of the sample modified foam nickel comprises the following steps:
before each test, the foamed nickel is cut into the size of 1cm multiplied by 5cm, ultrasonically cleaned for 15min by deionized water, ultrasonically cleaned for 15min by ethanol, and dried for 2h at 50 ℃ for standby.
40mg of Ni-Co oxide nanocrystals and 7.5mg of acetylene black were ground in a mortar for 15 min. Then adding a proper amount of isopropanol, and continuing to grind for 15 min. Finally, 1-2 drops of Polytetrafluoroethylene (PTFE) emulsion are added and are dropped on the surface of the foam nickel to be used before after being stirred slightly. After drying at 50 ℃ for 2h, the electrochemical test was waited for.
40mg of activated carbon and 7.5mg of acetylene black were ground in a mortar for 15 min. Then adding a proper amount of isopropanol, and continuing to grind for 15 min. Finally, 1-2 drops of Polytetrafluoroethylene (PTFE) emulsion are added and are dropped on the surface of the foam nickel to be used before after being stirred slightly. After drying at 50 ℃ for 2h, the electrochemical test was waited for.
And (3) carrying out cyclic voltammetry and constant current charge and discharge tests on the modified sample foamed nickel in the two-electrode system. The detection results are shown in FIGS. 2 and 3. Test knotThe results show that the Ni-Co oxide nanocrystals showed excellent supercapacitor performance, and the current densities of the Ni-Co oxide nanocrystals were 5mA cm/cm, respectively, as calculated from FIG. 3-2、10mA cm-2、15mA cm-2、20mA cm-2And 25mA cm-2When the specific capacitance is 330.8mF cm-2、300.6mF cm-2、278.5mF cm-2、251.3mF cm-2And 212.0mF cm-2。
Example 4
Testing the flexibility of a Ni-Co oxide nanocrystalline device (hereinafter referred to as a device) by assembling an all-solid flexible asymmetric capacitor device and comparing cyclic voltammograms before and after bending; the specific process is as follows:
the electrochemical experiments were carried out on an electrochemical workstation model CHI660d, using a two-electrode test system, the corresponding positive electrode being a sample-modified nickel foam electrode as obtained herein. The negative electrode is a foam nickel electrode modified by active carbon. All potentials herein are relative to RHE. The electrolyte was a 3M KOH solution. All electrochemical tests were performed at 25 ℃. At each experiment, all electrodes were tested in 3M KOH solution.
The preparation method of the sample modified foam nickel comprises the following steps:
before each test, the foamed nickel is cut into the size of 1cm multiplied by 5cm, ultrasonically cleaned for 15min by deionized water, ultrasonically cleaned for 15min by ethanol, and dried for 2h at 50 ℃ for standby.
40mg of Ni-Co oxide nanocrystals and 7.5mg of acetylene black were ground in a mortar for 15 min. Then adding a proper amount of isopropanol, and continuing to grind for 15 min. Finally, 1-2 drops of Polytetrafluoroethylene (PTFE) emulsion are added and are dropped on the surface of the foam nickel to be used before after being stirred slightly. And drying at 50 ℃ for 2h, and waiting for the assembly of the all-solid-state flexible asymmetric capacitor.
40mg of activated carbon and 7.5mg of acetylene black were ground in a mortar for 15 min. Then adding a proper amount of isopropanol, and continuing to grind for 15 min. Finally, 1-2 drops of Polytetrafluoroethylene (PTFE) emulsion are added and are dropped on the surface of the foam nickel to be used before after being stirred slightly. And drying at 50 ℃ for 2h, and waiting for the assembly of the all-solid-state flexible asymmetric capacitor.
The assembly method of the all-solid-state flexible asymmetric capacitor device comprises the following steps:
two 1cm multiplied by 4cm polyvinyl chloride (PVC) sheets are taken, 3-5 drops of a mixed solution of 3M KOH and polyethylene glycol are slowly dropped on one of the two sheets, and the whole PVC sheet is paved. And placing the foam nickel modified with the sample and the foam nickel modified with the activated carbon at two ends of the PVC sheet, and weighing about 1cm to ensure that the foam nickel is immersed in the mixed solution of 3M KOH and polyethylene glycol. Then another PVC sheet is carefully covered to be completely overlapped, and the whole device is wrapped by the preservative film to prevent liquid leakage. After drying at 50 ℃ for 12h, the electrochemical test is waited for.
And (3) carrying out cyclic voltammetry test on the all-solid-state flexible asymmetric capacitor device in the two-electrode system, and then bending the all-solid-state flexible asymmetric capacitor device to carry out cyclic voltammetry test, wherein the detection result is shown in the figure 4 and the figure 5. The test result shows that the cyclic voltammogram (figure 4) when the device is not bent is not obviously different from the cyclic voltammogram (figure 5) after the device is bent, which indicates that the capacitance performance of the device is not obviously changed before and after the device is bent, and the flexibility performance is good.
What has been described above is a specific embodiment of the present invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.
Claims (12)
- A controllable synthesis method of Ni-Co oxide nanocrystals is characterized in that the Ni-Co oxide nanocrystals are solid nanosphere-shaped structures with the diameter of 3-5nm, and the controllable synthesis method specifically comprises the following steps:s1: mixing Ni (CH)3COO)2∙4H2O、Co(CH3COO)2∙4H2Adding O into a mixed solution of Oleic Acid (OA), dodecylamine and Octadecene (ODE);s2: gradually heating to 180 ℃;s3: keeping the temperature at 180 ℃ for reaction to obtain a precursor containing Ni-Co oxide nanocrystals;s4: dispersing, settling and centrifuging;s5: gradually heating to 350 ℃;s6: and calcining at 350 ℃ to obtain the Ni-Co oxide nanocrystal.
- 2. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 1, wherein: ni (CH)3COO)2∙4H2O、Co(CH3COO)2∙4H2O, Oleic Acid (OA), dodecylamine and Octadecene (ODE) are added in the ratio of Ni (CH)3COO)2∙4H2When O is 3.62mmol, Co (CH)3COO)2∙4H2The amount of O added was 1.81mmol, the amount of ODE added was 10mL, the amount of dodecylamine added was 5mL, and the amount of OA added was 5 mL.
- 3. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 1, wherein: in the step S2, the heating rate is 3-4 ℃ min-1。
- 4. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 1, wherein: in step S4, an absolute ethanol-n-heptane mixed solution is used for dispersion and sedimentation.
- 5. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 4, wherein: the mixing volume ratio of the absolute ethyl alcohol to the n-heptane is 1: 1.
- 6. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 1, wherein: step S4 includes washing after dispersion sedimentation and centrifugation.
- 7. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 6, wherein: the washing adopts an absolute ethyl alcohol-n-heptane mixed solution.
- 8. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 7, wherein: the volume ratio of the absolute ethyl alcohol to the n-heptane is 1: 1.
- 9. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 1, wherein: in the step S5, the temperature rise rate is 10 ℃ min-1。
- 10. The controllable synthesis method of Ni-Co oxide nanocrystals according to claim 1, wherein: the reaction time in step S6 was 1 hour.
- 11. The Ni-Co oxide nanocrystal prepared by the controlled synthesis method of the Ni-Co oxide nanocrystal according to any one of claims 1 to 10, characterized in that: the Ni-Co oxide nanocrystal is a solid nanosphere structure with the diameter of 3-5 nm.
- 12. Use of the Ni-Co oxide nanocrystals according to claim 11 in solid-state asymmetric flexible supercapacitor electrode materials.
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