Method for preparing composite electrode material of super capacitor

A supercapacitor and composite electrode technology, applied in capacitors, electrolytic capacitors, circuits, etc., can solve the problems of low rate and unsatisfactory cycle life, and achieve the effects of low equipment use requirements, good cycle stability and simple operation process.

Inactive Publication Date: 2013-01-30
DONGHUA UNIV
3 Cites 24 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0004] Although the spherical flower-shaped cobalt oxide and the sandwich-structured spherical nickel hydroxide exhibit high specific capacitance when used as supercap...
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Method used

(3) cycle 2000 times under the scan rate of 50mV s-1, Ni(OH)2/CoO/rGO composite electrode material's spe...
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Abstract

The invention relates to a method for preparing a composite electrode material of a super capacitor. The method comprises the following steps of: (1) ultrasonically dispersing graphite, sodium nitrate and concentrated sulfuric acid into an ice bath, adding potassium hypermanganate, magnetically stirring, adding deionized water, magnetically stirring to make a mixture uniform, re-adding the deionized water, stirring at constant temperature, reacting in a water bath, cooling, adding hydrogen peroxide, centrifugally washing, freezing and drying in vacuum, and thus obtaining graphite oxide; (2) dispersing the graphite oxide, nickel salt and cobalt salt into a solvent, and performing solvothermal reaction to synthesize a Ni(OH)2/CoO/rGO composite material; and (3) uniformly mixing a Ni(OH)2/CoO reduction graphene oxide composite material, carbon black and polyvinylidene fluoride, stirring at room temperature, uniformly coating on the surface of nickel foam, drying in vacuum, and thus obtaining the composite electrode material of the super capacitor. The method is easy to operate and low in equipment using requirement. Raw materials are easily obtained, low in toxicity and low in cost. A novel method is provided for preparation of a nanosheet composite electrode material.

Application Domain

Electrolytic capacitors

Technology Topic

ChemistryHydrogen peroxide +24

Image

  • Method for preparing composite electrode material of super capacitor
  • Method for preparing composite electrode material of super capacitor
  • Method for preparing composite electrode material of super capacitor

Examples

  • Experimental program(3)

Example Embodiment

[0030] Example 1
[0031] (1) Preparation of graphite oxide
[0032] Add 1.5g graphite and 1.5g NaNO into a 500ml beaker 3 , 70ml of H 2 SO 4 (98%), ultrasonic for 15 minutes, then transfer to an ice bath, then slowly add 9g of KMnO to the reaction flask 4 , Magnetic stirring for 2 hours, the solution turns from black to brown, then add 100ml of deionized water, after magnetic stirring, add 200ml of water, the solution changes from brown to yellowish brown, then transfer to a water bath at 90°C Stir at a constant temperature for 1 hour, the solution turns yellow. When it is cooled to about 40°C, add 5ml of hydrogen peroxide (30%), and then centrifuge several times with deionized water and ethanol. The resulting sample is vacuum freeze-dried for 24 hours to obtain oxidation graphite.
[0033] (2) Preparation of Ni(OH) 2 /CoO/rGO composite electrode material
[0034] Take 12 mg of the prepared graphite oxide and disperse it with 24 ml of ethylene glycol ultrasonically, while dispersing 156 mg of nickel acetate tetrahydrate and 156 mg of cobalt acetate tetrahydrate in 90 ml of ethylene glycol. Subsequently, the above two dispersions were transferred to the inner lining of the reactor, stirred at room temperature for 2 hours, and then subjected to solvothermal reaction, reacted at 160°C for 6 hours to obtain Ni(OH) 2 /CoO/rGO composite material.
[0035] (3) Preparation of electrode materials
[0036] First, wash the foamed nickel with hydrochloric acid, deionized water and ethanol respectively, and dry it under vacuum for use. The prepared Ni(OH) 2 The /CoO/rGO composite material is uniformly mixed with carbon black and polyvinylidene tetrafluoroethylene, and the mass ratio of the three is 85:10:5. Stir at room temperature for 24 hours to make a viscous liquid, then evenly coat it on the surface of the foamed nickel, and finally dry the prepared electrode in a vacuum at 120°C for 4 hours to make an electrode material.
[0037] by image 3 with Figure 4 The following conclusions can be drawn:
[0038] (1) When the current density is 1A·g -1 The composite electrode material exhibits a high specific capacitance (1530F·g -1 ), or when the scan rate is 1mV·s -1 At the same time, the composite electrode material also exhibits a high specific capacitance (1514F·g -1 );
[0039] (2) When the current density increases to 10A·g -1 When, Ni(OH) 2 /CoO/rGO composite electrode material still has high specific capacitance (895F·g -1 );
[0040] (3) At 50mV·s -1 Cycle 2000 times at the scan rate, Ni(OH) 2 The specific capacitance retention rate of the /CoO/rGO composite electrode material is 83%, indicating that the electrode material has good cycle performance.

Example Embodiment

[0041] Example 2
[0042] (1) Preparation of graphite oxide
[0043] Add 1.5g graphite and 1.5g NaNO into a 500ml beaker 3 , 70ml of H 2 SO 4 (98%), ultrasonic for 15 minutes, then transfer to an ice bath, and then slowly add 6g KMnO to the reaction flask 4 , Magnetically stirred for 1 hour, the solution changed from black to brown, then add 100ml of deionized water, after magnetic stirring, add 200ml of water, the solution changed from brown to yellow-brown, then transferred to the water bath at 80 °C Stir at a constant temperature for 2 hours, the solution turns yellow. When it is cooled to about 10°C, add 5ml of hydrogen peroxide (30%), then centrifuge several times with deionized water and ethanol, and freeze-dry the obtained sample for 24 hours in vacuum to obtain oxidation graphite.
[0044] (2) Preparation of Ni(OH) 2 /CoO/rGO composite electrode material
[0045] Take 12 mg of the prepared graphite oxide and ultrasonically disperse it with 24 ml of ethylene glycol, while dispersing 156 mg of nickel acetate tetrahydrate and 312 mg of cobalt acetate tetrahydrate in 90 ml of ethylene glycol. Subsequently, the above two dispersions were transferred to the inner lining of the reactor, stirred at room temperature for 4 hours, and then subjected to solvothermal reaction, reacted at 120°C for 8 hours to obtain Ni(OH) 2 /CoO/rGO composite material.
[0046] (3) Preparation of electrode materials
[0047] First wash the foamed nickel with hydrochloric acid, deionized water and ethanol, and dry it in vacuum for use. The prepared Ni(OH) 2 The /CoO/rGO composite material is uniformly mixed with carbon black and polyvinylidene tetrafluoroethylene, and the mass ratio of the three is 85:10:5. Stir at room temperature for 12 hours to make a viscous liquid, and then evenly coat it on the surface of the foamed nickel, and finally dry the prepared electrode in a vacuum at 100°C for 4 hours to make an electrode material.

Example Embodiment

[0048] Example 3
[0049] (1) Preparation of graphite oxide
[0050] Add 1.5g graphite and 1.5g NaNO into a 500ml beaker 3 , 70ml of H 2 SO 4 (98%), ultrasonic for 15 minutes, then transfer to an ice bath, then slowly add 18g KMnO to the reaction flask 4 , Magnetic stirring for 3 hours, the solution turns from black to brown, then add 100ml of deionized water, after magnetic stirring, add 200ml of water, the solution changes from brown to yellowish brown, then transfer to a water bath at 100°C Stir at a constant temperature for 0.5 hours, the solution turns yellow. When it is cooled to about 20°C, add 5ml of hydrogen peroxide (30%), and then centrifuge several times with deionized water and ethanol. The resulting sample is vacuum freeze-dried for 12 hours to obtain oxidation graphite.
[0051] (2) Preparation of Ni(OH) 2 /CoO/rGO composite electrode material
[0052] Take 12 mg of the prepared graphite oxide and ultrasonically disperse it with 24 ml of ethylene glycol. At the same time, 156 mg of nickel acetate tetrahydrate and 468 mg of cobalt acetate tetrahydrate are dispersed in 90 ml of ethylene glycol. Subsequently, the above two dispersions were transferred to the inner lining of the reactor, stirred at room temperature for 1 hour, and then subjected to solvothermal reaction, reacted at 180°C for 2 hours to obtain Ni(OH) 2 /CoO/rGO composite material.
[0053] (3) Preparation of electrode materials
[0054] First wash the foamed nickel with hydrochloric acid, deionized water and ethanol, and dry it in vacuum for use. The prepared Ni(OH) 2 The /CoO/rGO composite material is uniformly mixed with carbon black and polyvinylidene tetrafluoroethylene, and the mass ratio of the three is 85:10:5. Stir at room temperature for 24 hours to make a viscous liquid, then evenly coat it on the surface of the foamed nickel, and finally dry the prepared electrode in a vacuum at 120°C for 3 hours to make an electrode material.
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PUM

PropertyMeasurementUnit
Specific capacitance1530.0F/g
Specific capacitance1514.0F/g
Specific capacitance895.0F/g
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

  • Low price
  • The operation process is simple

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High specific capacitanceGood cycle stabilityRoom temperaturePotassiumWater bathsNickel saltSulfuric acidCapacitor
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