CN111341567B - 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and preparation method thereof - Google Patents
3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and a preparation method thereof, and belongs to the technical field of capacitors. The super capacitor consists of 3D poplar catkin derived carbon and NiCo-LDH nano sheets, wherein the 3D poplar catkin derived carbon has a rich pore structure when reaching the micron size, and the NiCo-LDH nano sheet rods are reduced in size after being compounded with a 3D poplar catkin derived carbon framework. The 3D poplar catkin derived carbon supported NiCo-LDH nanosheet supercapacitor has good specific capacity, the preparation method is low in cost, and the rate capability of the composite material is excellent.
Description
Technical Field
The invention relates to a 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and a preparation method thereof, and belongs to the technical field of capacitors.
Background
In view of the urgent demand for high energy and high power density power supplies, lithium ion batteries and super capacitors have attracted extensive research interest, and in the field of consumer electronics, even though high energy density lithium ion batteries are currently widely used, there is a serious safety problem. Their development is still limited by the generation of heat and the formation of dendrites. Therefore, supercapacitors with fast charge and discharge, high power density, high cycling stability and high safety are considered to be the most promising candidates for energy storage devices.
Recently, transition metal Layered Double Hydroxides (LDHs) have been considered as one of the most potential electrode materials. The easy regulation of the cations of the lamina and the anion exchangeability still do not change its structure and also give LDHs excellent electrochemical performance. Among various LDHs, NiCo-LDH is widely used as an energy storage electrochemically active material due to its simple synthesis method and abundant reserves. Chen and the like use foamed nickel as a substrate to grow LDH nanosheet array electrodes with different Ni/Co ratios in situ, and when the Ni/Co ratio reaches 3:2, the specific capacity is 3 A.g-12682F g can be achieved under the current density-1The energy density reaches 77.3 Wh/kg-1The power density reaches 623 W.kg-1. Shao et al studied the effect of different core-shell structures on the electrochemical performance of LDH electrodes and discovered hollow spheres in the comparison process of electrochemical performance>Yolk ball>Core-shell structure>And (3) nanoparticles. 80.3%). Liu and the like use ZnO as a template to synthesize a NiCo @ NiCo-LDH core-shell structure by an electrodeposition method. The structure is 5 A.g-1Can still maintain 2200F g under the current density-1High specific capacity of (2). Then, at 20A g-1Can still maintain 80 percent of capacity retention rate under high current density and shows good rate performance. Li and the like prepare the Ni nanowire @ NiCo-LDH composite electrode by introducing the Ni nanowire, wherein the introduction of the Ni nanowire increases reaction active sites and reduces an electron transmission path, so that the specific capacity of the electrode is remarkably improved.
Disclosure of Invention
The invention provides a 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and a preparation method thereof. The super capacitor is composed of a 3D porous carbon frame and NiCo-LDH nanosheets, and the substrate of the super capacitor is the 3D porous carbon frame prepared by taking natural poplar wadding as a carbon source. According to the invention, the volume effect caused by the redox reaction in the charging and discharging process is inhibited through the composition of the NiCo-LDH nanosheet and the 3D poplar porous carbon framework, so that the stability and specific capacity of the material are improved. The 3D poplar derived carbon has rich pore structures, and the pore structures can be used as pore channels for ion transmission and can also inhibit the aggregation of active particles of NiCo-LDH nano sheets in the oxidation-reduction reaction, so that the specific capacity and the cycling stability of the composite material are finally improved.
The technical scheme of the invention is as follows:
a preparation method of a 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor comprises the following specific steps:
(1) repeatedly cleaning and drying the natural poplar catkin fibers by using a mixed solution of ethanol and water; preferably, the volume ratio of ethanol to water is 1: 3;
(2) soaking the poplar fiber obtained in the step (1) in NaOH solution at room temperature for 24 hours; preferably, the concentration of the NaOH solution is 0.5 to 5 mol.L-1More preferably 1 mol. L-1。
(3) Repeatedly cleaning and drying the poplar catkin fibers soaked in the step (2) by using deionized water;
(4) soaking the dried poplar fiber in the step (3) in cobalt nitrate (Co (NO) at 50-70 DEG C3)2·6H2O) in solution; preferably, the poplar fiber after drying in the step (3) is soaked in 0.05 mol.L at the temperature of 60 DEG C-1Cobalt nitrate (Co (NO)3)2·6H2O) for 24h in solution.
(5) Washing the poplar wadding fiber treated by the cobalt nitrate in the step (4) with deionized water, and drying;
(6) soaking the dried poplar fiber in the step (5) in a KOH solution at the temperature of 60-100 ℃ for activation; preferably, the poplar fiber after being dried in the step (5) is soaked in 1 mol.L at the temperature of 80 DEG C-1Activating in KOH solution for 48 hours.
(7) Placing the activated poplar fiber in the step (6) into a tube furnace at 4.5-5.5 ℃ for min-1The temperature is raised to 300 ℃ at the temperature raising rate and is kept for 1 hour, and then the temperature is continuously raised to 4.5-5.5 ℃ for min-1Heating to 800 ℃ at a heating rate and keeping the temperature for 1h to obtain a black sample; preferably, the poplar fiber after KOH activation in the step (6) is put into a tube furnace at the temperature of 5 ℃ per minute-1The temperature is raised to 300 ℃ at the temperature raising rate and is kept for 1h, and then the temperature is continuously raised to 5 ℃ for min-1The temperature is raised to 800 ℃ at the temperature raising rate and is kept for 1 hour.
(8) Will be described in detail(7) Placing the obtained black sample in HCl solution, stirring, removing redundant Co simple substance, and obtaining poplar catkin derived carbon; preferably, the concentration of the HCl solution is 1 to 3 mol.L-1(ii) a More preferably, the concentration of the HCl solution is 2 mol. L-1。
(9) Mixing the poplar catkin derived carbon obtained in the step (8) with nickel nitrate (Ni (NO)3)2·6H2O), cobalt nitrate (Co (NO)3)2·6H2Adding O), hexamethylenetetramine (hexamethylenetetramine) and water into a reaction kettle, and stirring for 1 h; preferably, the mass molar ratio g/mmol of the poplar fiber-derived carbon to the nickel nitrate is 3: 10, wherein the molar ratio of the nickel nitrate to the cobalt nitrate to the hexamethylenetetramine is 1:2: 6; the mass volume ratio g/L of the poplar derived carbon to the water is 30: 4. More preferably, the poplar seed derived carbon is 0.3g, nickel nitrate: cobalt nitrate: hexamethylenetetramine is 1mmol, 2mmol and 6mmol, respectively, water is 40mL, and the volume of water is 4/5 of the volume of the reaction kettle.
(10) And (4) keeping the solution obtained in the step (9) at the constant temperature of 90-100 ℃ for 10-20h, centrifugally washing and drying to obtain the finished product of the super capacitor. Preferably, the solution obtained in step (9) is kept at a constant temperature of 95 ℃ for 15 h.
The invention also comprises the super capacitor obtained by the preparation method.
Compared with the prior art, the invention has the following advantages:
1. compared with a pure NiCo-LDH super capacitor, the super capacitor overcomes the defect of reduction of multiplying power performance in the charge-discharge process under high current density.
2. Compared with the traditional carbon-based material, the 3D poplar catkin derived carbon in the super capacitor has the characteristics of good specific surface area, rich pore structure and environmental friendliness.
3. According to the super capacitor disclosed by the invention, the specific surface area of the material is improved by introducing the 3D poplar catkin derived carbon framework, the contact area of the material and the electrolyte is further increased, the reaction sites are increased, the electron transfer is promoted, and the specific capacity of the material is improved.
Drawings
FIG. 1 is an XRD pattern of example 1 of the present invention; wherein A, B represents NiCo-LDH and NiCo-LDH/C, respectively.
FIG. 2 is a scanning transmission electron micrograph of Populus bombycis-derived carbon SEM according to example 1 of the present invention; b represents poplar catkin derived carbon TEM; c represents NiCo-LDH SEM; d represents NiCo-LDH TEM.
FIG. 3 is a graph comparing the performance of NiCo-LDH and NiCo-LDH/C obtained in example 1 of the present invention, wherein A, B represents NiCo-LDH and NiCo-LDH/C, respectively.
FIG. 4 is a graph of NiCo-LDH CV and GCD and a graph of NiCo-LDH/C CV and GCD for example 1 of the present invention.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1: 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and preparation method thereof
The method comprises the following specific steps:
(1) repeatedly cleaning and drying the natural poplar catkin fibers by using a mixed solution of ethanol and water; wherein the volume ratio of the ethanol to the water is 1: 3;
(2) soaking the poplar fiber obtained in the step (1) in 1 mol.L at room temperature-1NaOH solution for 24 hours;
(3) repeatedly cleaning and drying the poplar catkin fibers soaked in the step (2) by using deionized water;
(4) soaking the poplar fiber dried in the step (3) in 0.05 mol.L at the temperature of 60 DEG C-1Cobalt nitrate (Co (NO)3)2·6H2O) solution for 24 hours;
(5) washing the poplar wadding fiber treated by the cobalt nitrate in the step (4) with deionized water, and drying;
(6) soaking the dried poplar fiber in 1 mol.L at the temperature of 80 DEG C-1Activating in KOH solution for 48 hours;
(7) placing the poplar catkin fiber activated by KOH in the step (6) into a tubular furnace at the temperature of 5 ℃ for min-1The temperature is raised to 300 ℃ at the temperature raising rate and is kept for 1h, and then the temperature is continuously raised to 5 ℃ for min-1Heating to 800 ℃ at a heating rate and keeping the temperature for 1h to obtain a black sample;
(8) placing the black sample obtained in the step (7) in 2 mol. L-1Stirring in HCl solution to remove redundant Co simple substance and obtain poplar catkin derived carbon;
(9) mixing the poplar catkin derived carbon obtained in the step (8) with nickel nitrate (Ni (NO)3)2·6H2O), cobalt nitrate (Co (NO)3)2·6H2O), hexamethylenetetramine (hexamethylenetetramine) and 40mL of water were added to a 50mL reaction vessel and stirred for 1 hour, wherein the carbon derived from poplar fibers was 0.3g, and the molar ratio of nickel nitrate: cobalt nitrate: 1mmol, 2mmol and 6mmol of hexamethylenetetramine respectively;
(10) and (4) keeping the temperature of the solution obtained in the step (9) constant at 95 ℃ for 15h, centrifugally washing and drying to obtain a finished product of the super capacitor.
Embodiment 2A 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and a preparation method thereof
The method comprises the following specific steps:
(1) repeatedly cleaning and drying the natural poplar catkin fibers by using a mixed solution of ethanol and water; wherein the volume ratio of the ethanol to the water is 1: 3;
(2) soaking the poplar fiber obtained in the step (1) in NaOH solution at room temperature for 24 hours; wherein the concentration of the NaOH solution is 3 mol.L-1；
(3) Repeatedly cleaning and drying the poplar catkin fibers soaked in the step (2) by using deionized water;
(4) soaking the poplar fiber dried in the step (3) in 0.08 mol.L at the temperature of 55 DEG C-1Cobalt nitrate (Co (NO)3)2·6H2O) neutralizing in the solution for 30 hours;
(5) washing the poplar wadding fiber treated by the cobalt nitrate in the step (4) with deionized water, and drying;
(6) soaking the dried poplar fiber in 1.5 mol.L at 65 DEG C-1In KOH solution ofActivating for 40 h;
(7) placing the activated poplar fiber in the step (6) into a tube furnace at 4.5 ℃ for min-1The temperature is raised to 300 ℃ at the temperature raising rate and is kept for 1 hour, and then the temperature is continuously raised to 4.5 ℃ for min-1Heating to 800 ℃ at a heating rate and keeping the temperature for 1h to obtain a black sample;
(8) placing the black sample obtained in the step (7) in 1.5 mol. L-1Stirring in HCl solution to remove redundant Co simple substance and obtain poplar catkin derived carbon;
(9) mixing the poplar catkin derived carbon obtained in the step (8) with nickel nitrate (Ni (NO)3)2·6H2O), cobalt nitrate (Co (NO)3)2·6H2Adding O), hexamethylenetetramine (hexamethylenetetramine) and water into a reaction kettle, and stirring for 1 h; wherein the poplar catkin derived carbon is 0.6g, the content of nickel nitrate: cobalt nitrate: hexamethylenetetramine is 2mmol, 4mmol and 12mmol respectively, water is 80mL, and the volume of water is 4/5 of the volume of the reaction kettle.
(10) And (4) keeping the temperature of the solution obtained in the step (9) constant for 20 hours at the temperature of 90 ℃, and centrifugally washing and drying to obtain a finished product of the super capacitor.
Embodiment 3A 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and a preparation method thereof
The method comprises the following specific steps:
(1) repeatedly cleaning and drying the natural poplar catkin fibers by using a mixed solution of ethanol and water; wherein the volume ratio of the ethanol to the water is 1: 3;
(2) soaking the poplar fiber obtained in the step (1) in NaOH solution at room temperature for 24 hours; wherein the concentration of the NaOH solution is 3 mol.L-1；
(3) Repeatedly cleaning and drying the poplar catkin fibers soaked in the step (2) by using deionized water;
(4) soaking the poplar fiber dried in the step (3) in 0.1 mol.L at the temperature of 70 DEG C-1Cobalt nitrate (Co (NO)3)2·6H2O) for 18h in solution.
(5) Washing the poplar wadding fiber treated by the cobalt nitrate in the step (4) with deionized water, and drying;
(6) drying the step (5)Soaking the post poplar fiber in 1 mol.L at 90 DEG C-1Activating in KOH solution for 48 hours.
(7) Placing the activated poplar fiber in the step (6) into a tube furnace at 5.5 ℃ for min-1The temperature is raised to 300 ℃ at the temperature raising rate and is kept for 1 hour, and then the temperature is continuously raised to 5.5 ℃ for min-1Heating to 800 ℃ at a heating rate and keeping the temperature for 1h to obtain a black sample;
(8) placing the black sample obtained in the step (7) in an HCl solution, stirring, removing redundant Co simple substance, and obtaining poplar catkin derived carbon; wherein the concentration of the HCl solution is 3 mol.L-1；
(9) Mixing the poplar catkin derived carbon obtained in the step (8) with nickel nitrate (Ni (NO)3)2·6H2O), cobalt nitrate (Co (NO)3)2·6H2Adding O), hexamethylenetetramine (hexamethylenetetramine) and water into a reaction kettle, and stirring for 1 h; wherein the poplar catkin derived carbon is 0.3g, the content of nickel nitrate: cobalt nitrate: hexamethylenetetramine is 1mmol, 2mmol and 6mmol, respectively, water is 40mL, and the volume of water is 4/5 of the volume of the reaction kettle.
(10) And (4) keeping the temperature of the solution obtained in the step (9) constant at 98 ℃ for 12h, centrifugally washing and drying to obtain a finished product of the super capacitor.
Experimental example 1
The 3D poplar-derived carbon-supported NiCo-LDH nanosheet supercapacitor obtained in example 1 of the invention is used for performance detection, and an XRD (X-ray diffraction) spectrum is shown in figure 1, wherein A, B respectively represents NiCo-LDH and NiCo-LDH/C (3D poplar-derived carbon-supported NiCo-LDH nanosheet supercapacitor). The scanning transmission electron micrograph is shown in FIG. 2. A comparison of the NiCo-LDH and NiCo-LDH/C performance is shown in FIG. 3, where A, B represents NiCo-LDH and NiCo-LDH/C, respectively. The CV and GCD plots are shown in FIG. 4, where a is the CV plot for NiCo-LDH, b is the GCD plot for NiCo-LDH, C is the CV plot for NiCo-LDH/C, and d is the GCD plot for NiCo-LDH/C.
Experimental example 2
The specific capacity of the super capacitor is detected, and the detection result is as follows:
at 4 A.g-1The specific capacity of the super capacitor reaches 358 mAh.g under the current density-1(ii) a At 10 A.g-1The specific capacity retention rate of the super capacitor reaches 73.2% under the current density.
Claims (13)
1. A3D poplar catkin derived carbon supported NiCo-LDH nanosheet supercapacitor material is characterized in that the supercapacitor material is composed of a 3D porous carbon frame and NiCo-LDH nanosheets;
the preparation method of the supercapacitor material comprises the following specific steps:
(1) repeatedly cleaning and drying the natural poplar catkin fibers by using a mixed solution of ethanol and water;
(2) soaking the poplar fiber obtained in the step (1) in NaOH solution at room temperature for 24 hours;
(3) repeatedly cleaning and drying the poplar catkin fibers soaked in the step (2) by using deionized water;
(4) soaking the poplar fiber dried in the step (3) in a cobalt nitrate solution at the temperature of 50-70 ℃;
(5) washing the poplar wadding fiber treated by the cobalt nitrate in the step (4) with deionized water, and drying;
(6) soaking the dried poplar fiber in the step (5) in a KOH solution at the temperature of 60-100 ℃ for activation;
(7) placing the activated poplar fiber in the step (6) into a tube furnace at the temperature of 4.5-5.5 ℃ for min-1The temperature is raised to 300 ℃ at the heating rate and is kept for 1h, and then the temperature is continuously raised to 4.5-5.5 ℃ for min-1Heating to 800 ℃ at a heating rate and keeping the temperature for 1h to obtain a black sample;
(8) placing the black sample obtained in the step (7) in an HCl solution, stirring, removing redundant Co simple substance, and obtaining poplar catkin derived carbon;
(9) adding the poplar catkin derived carbon obtained in the step (8), nickel nitrate, cobalt nitrate, hexamethylenetetramine and water into a reaction kettle and stirring for 1 h;
(10) and (4) keeping the solution obtained in the step (9) at the constant temperature of 90-100 ℃ for 10-20h, centrifugally washing and drying to obtain the finished product of the supercapacitor material.
2. The 3D poplar catkin-derived carbon-supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein the substrate of the supercapacitor material is a 3D porous carbon framework prepared with natural poplar catkin as a carbon source.
3. The 3D poplar derived carbon supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein the volume ratio of ethanol to water in step (1) is 1: 3.
4. The 3D poplar derived carbon supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein the NaOH solution in step (2) is at a concentration of 0.5-5 mol-L-1。
5. The 3D poplar derived carbon supported NiCo-LDH nanosheet supercapacitor material of claim 4, wherein the concentration of NaOH solution in step (2) is 1 mol.L-1。
6. The 3D poplar derived carbon-supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein in step (4), the dried poplar fibers from step (3) are soaked in 0.05 mol.L at 60 ℃-1For 24 hours in cobalt nitrate solution.
7. The 3D poplar derived carbon-supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein in step (6), the dried poplar fibers from step (5) are soaked in 1 mol.L at 80 ℃-1Activating in KOH solution for 48 hours.
8. The 3D poplar derived carbon supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein in step (7) the KOH-activated poplar fibers of step (6) were placed in a tube furnace at 5 ℃ for min-1The temperature is raised to 300 ℃ at the temperature raising rate and is kept for 1 hour, and then the heating is continuedAt 5 ℃ for min-1The temperature is raised to 800 ℃ at the temperature raising rate and is kept for 1 hour.
9. The 3D poplar derived carbon supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein the concentration of HCl solution in step (8) is 1-3mol-1。
10. The 3D poplar derived carbon supported NiCo-LDH nanosheet supercapacitor material of claim 9, wherein the concentration of HCl solution in step (8) is 2mol-1。
11. The 3D poplar catkin-derived carbon-supported NiCo-LDH nanosheet supercapacitor material of claim 1, wherein the mass molar ratio g/mmol of poplar catkin-derived carbon to nickel nitrate in step (9) is 3: 10, wherein the molar ratio of the nickel nitrate to the cobalt nitrate to the hexamethylenetetramine is 1:2: 6; the mass volume ratio g/L of the poplar derived carbon to the water is 30: 4.
12. The 3D poplar catkin-derived carbon-supported NiCo-LDH nanosheet supercapacitor material of claim 11, wherein the poplar catkin-derived carbon is 0.3g, nickel nitrate: cobalt nitrate: hexamethylenetetramine is 1mmol, 2mmol and 6mmol, respectively, water is 40mL, and the volume of water is 4/5 of the volume of the reaction kettle.
13. The 3D poplar derived carbon-supported NiCo-LDH nanosheet supercapacitor material according to claim 1, wherein the solution obtained in step (9) is thermostatted at 95 ℃ for 15h in step (10).
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