CN114334485B - Nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material and preparation method thereof - Google Patents
Nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a nickel oxalate composite fibrous nickel hydroxide super capacitor electrode material and a preparation method thereof, belonging to the technical field of capacitors. The preparation method comprises the following steps: weighing nickel chloride and oxalic acid, dissolving in water at room temperature, and uniformly mixing; putting the mixed solution into a high-temperature reaction kettle, and obtaining nickel oxalate precipitate at 160-200 ℃ and 6 h; washing the precipitate, and drying in a warm oven; weighing nickel oxalate, nickel chloride and urea, placing the nickel oxalate, the nickel chloride and the urea in deionized water at room temperature, and then placing the deionized water in a high-temperature reaction kettle; placing the high-temperature reaction kettle into an oven for heat preservation to obtain a sample; and washing and drying the sample to obtain the supercapacitor electrode material. The invention improves the contact area between the specific surface of the material and the electrolyte and increases the active site.
Description
Technical Field
The invention relates to a nickel oxalate composite fibrous nickel hydroxide super capacitor electrode material and a preparation method thereof, belonging to the technical field of capacitors.
Background
In recent years, with the rapid growth of portable electronic devices and new energy power automobiles, the demand for high-power energy storage devices has increased exponentially. Considering the urgent need for high energy density and high power density energy storage, lithium ion batteries and supercapacitors, which have high energy density and long service life, are widely used in rechargeable energy storage devices, have attracted extensive research interest. However, lithium ion batteries have the disadvantages of higher cost and low power density. Compared with a lithium ion battery, the super capacitor has the characteristics of higher power density, long cycle stability, rapid charge and discharge performance and the like. Although super capacitors are proposed later than batteries, their development speed is rapid. Therefore, in the next generation of power equipment, the super capacitor is used as an independent power supply or a supplementary energy storage unit of the energy collector, and is expected to play an important role in the future self-powered equipment due to the advantages of higher power density and the like.
Among the many transition metal compounds, nickel-based materials are considered as one of the most promising electrode materials due to their rich and inexpensive raw material sources, environmental friendliness, high theoretical capacitance, and the like. In recent years, metallic nickel oxalate has been used as an electroactive material in supercapacitors, mainly because of its reversible electrochemical redox properties. Wan et al synthesized micro-rectangular Ni 0.55 Co 0.45 C 2 O 4 At a current density of 1 Ag -1 Is 562Cg -1 Is a high specific capacity of (a). Gao et al synthesized NiC by solvothermal method 2 O 4 ZIF-67 material, 1 Ag -1 Its specific capacity reaches 1019 Fg -1 . He and the like synthesize NiC 2 O 4 @NiO core-shell layered nanostructured material, which is 1 Ag -1 When reaching 2287.09 Fg -1 High specific capacitance of (2).
Disclosure of Invention
Aiming at the problems, the invention provides a nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material and a preparation method thereof. The invention reduces the structural damage caused by the oxidation-reduction process of charging and discharging by combining nickel oxalate with fibrous nickel hydroxide material, thereby improving the stability and specific capacity of the material. Meanwhile, the nickel oxalate and the fibrous nickel hydroxide material are compounded, so that the contact area between the specific surface of the material and electrolyte is increased, the active site is increased, and the specific capacity is further improved.
The technical scheme of the invention is as follows:
the preparation method of the nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material comprises the following specific steps:
(1) Weighing nickel chloride and oxalic acid according to a molar ratio of 1:3, and placing the nickel chloride and oxalic acid in a beaker containing deionized water at room temperature for dissolution; preferably, the molar mass of nickel chloride and oxalic acid is 1 mmol and 3 mmol respectively;
(2) Placing the beaker in the step (1) into an ultrasonic machine for ultrasonic treatment for 20-30 minutes to uniformly mix the solution; preferably, the beaker in the step (1) is placed in an ultrasonic machine for ultrasonic treatment for 25 minutes;
(3) Placing the mixed solution obtained in the step (2) into a high-temperature reaction kettle, and placing the reaction kettle into a baking oven with the temperature of 160-200 ℃ for constant temperature 6 h to obtain nickel oxalate precipitate; preferably, the mixed solution obtained in the step (2) is placed into a high-temperature reaction kettle, and the reaction kettle is placed into a baking oven at 180 ℃ to be kept at a constant temperature of 6 h so as to obtain nickel oxalate precipitate;
(4) Cross-cleaning the precipitate obtained in the step (3) with deionized water and ethanol, and drying in a 50-80 ℃ oven for 8-16 h; preferably, the mixture is placed in a 60 ℃ oven to be dried for 12 h;
(5) Weighing the following components in percentage by mass: 4:5 nickel oxalate, nickel chloride and urea are placed in a beaker containing deionized water at room temperature; preferably, the mass of the nickel oxalate, the nickel chloride and the urea is respectively 0.03 g, 0.12 g and 0.15 g, and the nickel oxalate, the nickel chloride and the urea are placed in a beaker containing deionized water at room temperature;
(6) Placing the beaker in the step (5) on a magnetic stirrer, stirring for 30-60 min, and then placing the beaker in a high-temperature reaction kettle; placing the beaker in the step (5) on a magnetic stirrer to stir for 60 min;
(7) Placing the high-temperature reaction kettle in the step (6) into an oven at 80-115 ℃ for heat preservation for 10-16 h, and obtaining a sample; preferably, the high-temperature reaction kettle in the step (6) is placed into a 95 ℃ oven for heat preservation of 12 h;
(8) And (3) washing and drying the sample obtained in the step (7) to obtain the supercapacitor electrode material.
The method also comprises the super capacitor electrode material obtained by the preparation method and the super capacitor prepared by the super capacitor electrode material.
Compared with the prior art, the invention has the following advantages:
1. compared with the electrode material of the supercapacitor made of pure nickel oxalate or fibrous nickel hydroxide, the invention overcomes the defect of reduced multiplying power performance of the supercapacitor under high current density.
2. The invention improves the specific surface area of the material, increases active sites, reduces resistance, promotes electron transmission and improves the specific capacity of the material by compounding nickel oxalate and fibrous nickel hydroxide material.
3. The super capacitor is prepared by using the nickel oxalate and nickel hydroxide composite material which is low in cost and environment-friendly, is beneficial to reducing consumption, and accords with the concept of green and environment protection.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is an XRD pattern of an electrode material; a, B, C is respectively a nickel oxalate electrode material, a nickel hydroxide electrode material and the nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material obtained in the embodiment 1 of the invention;
FIG. 2 is a scanning electron microscope image of an electrode material, wherein a represents a nickel hydroxide electrode material, b represents a nickel oxalate electrode material, c and d represent nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode materials obtained in example 1 with different magnifications;
FIG. 3 is a transmission electron microscopic view of an electrode material, wherein a represents a nickel hydroxide electrode material, b represents a nickel oxalate electrode material, and c represents a nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material obtained in example 1;
fig. 4 is a graph showing the electrochemical test performance of a nickel oxalate electrode material, a nickel hydroxide electrode material, the nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material obtained in example 1, and GCD and CV test charts of nickel oxalate nickel hydroxide, wherein A, B, C is the nickel oxalate electrode material, the nickel hydroxide electrode material, and the nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material obtained in example 1, respectively.
Fig. 5 is a graph showing CV and GCD tests of the electrode material of the nickel oxalate composite fiber-shaped nickel hydroxide supercapacitor obtained in example 1, a is a CV test, and b is a GCD test.
Detailed Description
The invention will be further described with reference to specific embodiments, and advantages and features of the invention will become apparent from the description. The embodiments are merely exemplary and do not limit the scope of the invention in any way. It will be understood by those skilled in the art that various changes and substitutions of details and forms of the technical solution of the present invention may be made without departing from the spirit and scope of the present invention, but these changes and substitutions fall within the scope of the present invention.
The reagents used in the present invention are all commercially available.
Example 1: nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material and preparation method thereof
The preparation method comprises the following specific steps:
(1) Weighing 1 mmol of nickel chloride and 3 mmol of oxalic acid, and placing the mixture in a beaker containing 35 ml deionized water at room temperature for dissolution;
(2) Placing the beaker in the step (1) into an ultrasonic machine for ultrasonic treatment for 25 minutes to uniformly mix the solution;
(3) Placing the mixed solution obtained in the step (2) into a 50 ml high-temperature reaction kettle, and placing the reaction kettle into a 180 ℃ oven for constant temperature 6 h to obtain nickel oxalate precipitate;
(4) Cross-cleaning the precipitate obtained in the step (3) with deionized water and ethanol for 6 times, and drying in a constant-temperature oven at 60 ℃ for 15 h;
(5) Weighing a 0.03. 0.03 g nickel oxalate sample, 0.12. 0.12 g nickel chloride and 0.15. 0.15 g urea, and placing the nickel oxalate sample and the nickel chloride and the 0.15.3534 urea in a beaker containing 35 ml deionized water at room temperature;
(6) Placing the beaker in the step (5) on a magnetic stirrer, stirring for 60 min, and then placing the beaker in a high-temperature reaction kettle of 50 ml;
(7) And (3) placing the high-temperature reaction kettle in the step (6) into a baking oven at 95 ℃ for 12h, and obtaining a sample.
(8) And (3) using the sample obtained in the step (7). And (3) after the ethanol and the water are subjected to cross cleaning for 6 times, drying in a baking oven at 40 ℃ for 12h, and obtaining the finished electrode material of the supercapacitor.
Example 2: nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material and preparation method thereof
(1) Weighing 0.5 mmol of nickel chloride and 1.5 mmol of oxalic acid, and placing the mixture in a beaker containing 35 ml deionized water at room temperature for dissolution;
(2) Placing the beaker in the step (1) into an ultrasonic machine for ultrasonic treatment for 20 min, so that the solution is uniformly mixed;
(3) Placing the mixed solution obtained in the step (2) into a 50 ml high-temperature reaction kettle, and placing the reaction kettle into a 170 ℃ oven for 6 h constant temperature to obtain nickel oxalate precipitate;
(4) Cross-cleaning the precipitate obtained in the step (3) with deionized water and ethanol for 6 times, and drying in a constant temperature oven at 55 ℃ for 15 h;
(5) Weighing a 0.03. 0.03 g nickel oxalate sample, 0.12. 0.12 g nickel chloride and 0.15. 0.15 g urea, and placing the nickel oxalate sample and the nickel chloride and the 0.15.3534 urea in a beaker containing 35 ml deionized water at room temperature;
(6) Placing the beaker in the step (5) on a magnetic stirrer for stirring, and placing the beaker into a high-temperature reaction kettle of 50 ml after 50 min;
(7) And (3) placing the high-temperature reaction kettle in the step (6) into an oven at 85 ℃ for heat preservation of 12 and h, and obtaining a sample.
(8) And (3) using the sample obtained in the step (7). And (3) after the ethanol and the water are subjected to cross cleaning for 6 times, drying in a baking oven at 40 ℃ for 12h, and obtaining the finished electrode material of the supercapacitor.
Example 3: nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material and preparation method thereof
The preparation method comprises the following specific steps:
(1) Weighing 1.2 mmol of nickel chloride and 3.6 mmol of oxalic acid, and placing the mixture in a beaker containing 35 ml deionized water at room temperature for dissolution;
(2) Placing the beaker in the step (1) into an ultrasonic machine for ultrasonic treatment for 30 minutes to uniformly mix the solution;
(3) Placing the mixed solution obtained in the step (2) into a 50 ml high-temperature reaction kettle, and placing the reaction kettle into a 200 ℃ oven for constant temperature 6 h to obtain nickel oxalate precipitate;
(4) Cross-cleaning the precipitate obtained in the step (3) with deionized water and ethanol for 6 times, and drying in a constant temperature oven at 70 ℃ for 15 h;
(5) Weighing a 0.04 g nickel oxalate sample, 0.16 g nickel chloride and 0.20 g urea, and placing the nickel oxalate sample and the nickel chloride and the 0.20 g urea in a beaker containing 35 ml deionized water at room temperature;
(6) Placing the beaker in the step (5) on a magnetic stirrer, stirring for 45 min, and then placing the beaker in a high-temperature reaction kettle of 50 ml;
(7) Putting the high-temperature reaction kettle in the step (6) into a baking oven at 110 ℃ for heat preservation of 10 h to obtain a sample;
(8) And (3) using the sample obtained in the step (7). The finished electrode material of the super capacitor can be obtained after the ethanol and water are washed for 6 times in a cross way and then are put into a 40 ℃ oven for drying 12h
Experimental example 1
The electrode material of the nickel oxalate composite fibrous nickel hydroxide supercapacitor obtained in the embodiment 1 of the present invention is used for performance detection, the XRD pattern is shown in fig. 1, and A, B, C in the figure is the nickel oxalate electrode material, the nickel hydroxide electrode material, and the nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material obtained in the embodiment 1, respectively. The scanning electron microscope is shown in fig. 2, wherein a represents nickel hydroxide electrode material, b represents nickel oxalate electrode material, c and d represent nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode materials obtained in example 1 with different magnifications. The transmission electron microscope is shown in fig. 3, wherein a represents nickel hydroxide electrode material, b represents nickel oxalate electrode material, and c represents nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material obtained in example 1. The electrochemical test comparison graphs of the nickel oxalate electrode material, the nickel hydroxide electrode material and the nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material obtained in the embodiment 1 are shown in fig. 4, wherein a, b, c, d is a performance comparison graph of three materials, a is a CV comparison graph of three materials, b is a multiplying power performance comparison graph of three materials, c is a GCD comparison graph of three materials under specific current density, and c is a comparison graph of transfer resistances of three materials, A, B, C is nickel oxalate, nickel hydroxide, nickel oxalate and nickel hydroxide composite materials respectively, and the CV area of the nickel oxalate and nickel hydroxide composite materials can be found to be larger, the impedance is smaller, and the electrochemical performance is better through comparison. The CV and GCD test patterns of the electrode material of the nickel oxalate composite fibrous nickel hydroxide supercapacitor obtained in example 1 are shown in fig. 5, wherein a and b are respectively CV and GCD test patterns.
Experimental example 2
The specific capacity of the supercapacitor prepared by the supercapacitor electrode material obtained by the invention is detected, and the detection result is as follows:
at 1A g -1 The capacity of the super capacitor of the invention reaches 668C g under the current density -1 At 5A g -1 The specific capacity retention rate of the super capacitor material can reach 65.4 percent under the current density.
Claims (10)
1. The preparation method of the nickel oxalate composite fibrous nickel hydroxide supercapacitor electrode material is characterized by comprising the following specific steps of:
(1) According to 1: weighing nickel chloride and oxalic acid according to the molar ratio of 3-9, and placing the nickel chloride and oxalic acid in a beaker containing deionized water at room temperature for dissolution;
(2) Placing the beaker in the step (1) into an ultrasonic machine for ultrasonic treatment for 20-30 minutes to uniformly mix the solution;
(3) Placing the mixed solution obtained in the step (2) into a high-temperature reaction kettle, and placing the reaction kettle into a baking oven with the temperature of 160-200 ℃ for constant temperature 6 h to obtain nickel oxalate precipitate;
(4) Cross-cleaning the precipitate obtained in the step (3) with deionized water and ethanol, and drying in a 50-80 ℃ oven for 8-16 h;
(5) Weighing the following components in percentage by mass: 3-5:5 nickel oxalate, nickel chloride and urea are placed in a beaker containing deionized water at room temperature;
(6) Placing the beaker in the step (5) on a magnetic stirrer, stirring for 30-60 min, and then placing the beaker in a high-temperature reaction kettle;
(7) Placing the high-temperature reaction kettle in the step (6) into an oven at 80-115 ℃ for heat preservation for 10-16 h, and obtaining a sample;
(8) Washing and drying the sample obtained in the step (7) to obtain the supercapacitor electrode material
And (5) material.
2. The method according to claim 1, wherein the molar ratio of nickel chloride to oxalic acid in step (1) is 1:6.
3. The method of claim 1, wherein in step (2) the following steps are performed
The beaker in the step (1) is placed in an ultrasonic machine for ultrasonic treatment for 25 minutes.
4. The method of claim 1, wherein in step (3) the following steps are performed
And (3) placing the mixed solution obtained in the step (2) into a high-temperature reaction kettle, and placing the reaction kettle into a baking oven at 180 ℃ for constant temperature 6 h to obtain nickel oxalate precipitate.
5. The method according to claim 1, wherein the step (4) is performed centrally
12, h were dried in an oven at 60 ℃.
6. The method according to claim 1, wherein the step (5) is called
The mass ratio is 1:4:5 nickel oxalate, nickel chloride and urea are placed in a beaker containing deionized water at room temperature.
7. The method of claim 1, wherein in step (6)
The beaker in the step (5) is placed on a magnetic stirrer to be stirred for 60 min.
8. The method of claim 1, wherein in step (7)
And (3) placing the high-temperature reaction kettle in the step (6) into a 95 ℃ oven for heat preservation of 12 h.
9. The supercapacitor electrode material obtained by the method of any one of claims 1 to 8.
10. A supercapacitor made using the supercapacitor electrode material of claim 9.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110080054A (en) * | 2010-01-04 | 2011-07-12 | 인하대학교 산학협력단 | Method for manufacturing metal oxalate nano structures for supercapacitors |
| CN103646788A (en) * | 2013-12-19 | 2014-03-19 | 山东大学 | Nickel oxalate based asymmetrical supercapacitor and preparation method thereof |
| CN107954483A (en) * | 2017-12-28 | 2018-04-24 | 济南大学 | A kind of class alpha-phase nickel hydroxide ultrathin nanometer piece and preparation method thereof |
| CN110395774A (en) * | 2019-07-19 | 2019-11-01 | 五邑大学 | A kind of preparation method and application of cobalt acid nickel porous material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110080054A (en) * | 2010-01-04 | 2011-07-12 | 인하대학교 산학협력단 | Method for manufacturing metal oxalate nano structures for supercapacitors |
| CN103646788A (en) * | 2013-12-19 | 2014-03-19 | 山东大学 | Nickel oxalate based asymmetrical supercapacitor and preparation method thereof |
| CN107954483A (en) * | 2017-12-28 | 2018-04-24 | 济南大学 | A kind of class alpha-phase nickel hydroxide ultrathin nanometer piece and preparation method thereof |
| CN110395774A (en) * | 2019-07-19 | 2019-11-01 | 五邑大学 | A kind of preparation method and application of cobalt acid nickel porous material |
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