CN109841422B - Co3O4/Co2P coaxial heterostructure material and preparation method and application thereof - Google Patents
Co3O4/Co2P coaxial heterostructure material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to Co3O4/Co2The P coaxial heterostructure material and the preparation method thereof comprise the following steps: 1) sintering the cobalt hydroxide nanowire in a hydrogen phosphide atmosphere to obtain a cobalt phosphide nanowire; 2) subjecting the cobalt phosphide nanowire to rapid annealing treatment to oxidize the surface layer to obtain Co3O4/Co2P coaxial heterostructure micro supercapacitor electrode materials. The invention has the beneficial effects that: for Co3O4/Co2P coaxial heterostructure, outer layer of Co3O4Will provide pseudo-capacitance capacity while the Co of the inner layer2P has high conductivity; meanwhile, because the electrochemical reaction only occurs on the surface or near surface of the material, Co is in the inner layer under higher reaction potential2P cannot directly contact with the adsorption solution ions and does not catalyze water decomposition. Therefore, the coaxial heterostructure keeps higher capacity and cycling stability, also has better electron conductivity, and the multiplying power performance is improved.
Description
Technical Field
The invention belongs to the field of intersection of material preparation and a micro super capacitor, and particularly relates to Co3O4/Co2P coaxial heterostructure material and a preparation method thereof.
Background
With the technological progress and development, the human society has entered the information age, and the modern electronic equipment and technology developed on the basis of the semiconductor technology greatly facilitate the daily life of people, and the appearance and popularization of wearable intelligent electronic equipment and the internet of things further increase the demand of people on the miniaturization and portability of energy storage equipment. In micro energy storage devices, Micro Supercapacitors (MSCs) have attracted extensive attention due to their advantages of high power density, fast charge-discharge time, long cycle life, and the like, and have good application prospects in the fields of microelectronics, medical science, and machinery. However, the energy density of MSCs is low enough to meet the demand of micro-electronic devices, which is the main reason for limiting the development of MSCs.
Disclosure of Invention
The invention provides a Co3O4/Co2P coaxial heterostructure micro supercapacitor electrode material and preparation thereof, the preparation process is simple, and the obtained Co3O4/Co2The P coaxial heterostructure used as the anode material of the micro super capacitor has higher theoretical capacity and keeps good cycle stability and rate capability.
The technical scheme adopted by the invention for solving the technical problems is as follows: co3O4/Co2P coaxial heterostructure material, which is a coaxial heterostructure, the diameter of which is between 70 nanometers and 300 nanometers, the length of which is between 600 nanometers and 2 micrometers, and the inner layer of the nanowire coaxial heterostructure is Co2P, the outer layer being Co3O4Outer layer of Co3O4The oxide layer is 1.2 to 2 nanometers thick.
Said Co3O4/Co2The preparation method of the P coaxial heterostructure material comprises the following steps:
1) sintering the cobalt hydroxide nanowire in a hydrogen phosphide atmosphere to obtain a cobalt phosphide nanowire;
2) subjecting the cobalt phosphide nanowire to rapid annealing treatment to oxidize the surface layer to obtain Co3O4/Co2P coaxial heterostructure micro supercapacitor electrode materials.
According to the scheme, the cobalt hydroxide nanowire is prepared by taking cobalt chloride hexahydrate, ammonium fluoride and urea as raw materials, taking foamed nickel as a substrate and adopting a hydrothermal method.
According to the scheme, the molar ratio of the cobalt chloride hexahydrate to the ammonium fluoride to the urea is 2:1: 4.
According to the scheme, sodium hypophosphite is decomposed at high temperature in the step 1) to be used as a phosphine gas source.
According to the scheme, the sintering in the step 1) is carried out by heating to 300 ℃ at the speed of 2 ℃/min and preserving heat for 3 hours.
According to the scheme, the rapid annealing in the step 2) is to heat up to 250 ℃ in a rapid annealing furnace at the speed of 5 ℃/min and keep the temperature for 3 minutes.
Said Co3O4/Co2The P coaxial heterostructure material is applied as a micro super capacitor electrode anode material.
With Co3O4/Co2P coaxial heterostructure as anode material and Fe2O3The nano-wire structure is made of a negative electrode material, and a microelectrode is prepared by adopting a nano-indentation technology and assembled into the asymmetric micro supercapacitor.
Invention incorporating Co3O4And Co2Different characteristics and synthesis preparation methods of P creatively provide design and synthesis of Co3O4/Co2A P-coaxial heterostructure. To have Co of coaxial heterostructure3O4/Co2When P is applied to MSCs with high load, surface layer Co3O4The electrochemical reaction can provide very high capacitance, and Co2P provides a rapid electron transport channel to meet the requirement of longitudinal electron conduction of the device, so that the specific energy density of the MSCs can be effectively improved in the aspect of material structure, the electron conduction network of the MSCs is prevented from being optimized through a complex micromachining process, the energy density and the rate capability of the MSCs are effectively improved, and an effective, simple and feasible new way is provided for further development of the MSCs.
The invention has the beneficial effects that: for Co3O4/Co2P coaxial heterostructure, outer layer of Co3O4Will provide pseudo-capacitance capacity while the Co of the inner layer2P has high conductivity; meanwhile, because the electrochemical reaction only occurs on the surface or near surface of the material, Co is in the inner layer under higher reaction potential2P cannot directly contact with the adsorption solution ions and does not catalyze water decomposition. Therefore, the coaxial heterostructure keeps higher capacity and cycling stability, also has better electron conductivity, and the multiplying power performance is improved.
Drawings
FIG. 1 shows Co in an embodiment of the present invention3O4/Co2A preparation flow chart of the electrode material of the P coaxial heterostructure micro supercapacitor;
FIG. 2 is an SEM image of example 1 of the invention, wherein FIG. 2a is an SEM image of cobalt phosphide nanowires in example 1 of the invention; FIG. 2b shows Co in example 1 of the present invention3O4/Co2SEM image of P coaxial heterostructure; FIG. 2c is an SEM image of the iron trioxide nanowires in examples 1, 2 and 3 of the present invention;
FIG. 3 shows Co in example 1 of the present invention3O4/Co2An energy spectrum of the electrode material of the P coaxial heterostructure micro supercapacitor;
FIG. 4 is a cyclic voltammogram (FIG. a) of cobalt phosphide nanowires prepared in example 1 of the present invention at a sweep rate of 5mV/s with Co3O4/Co2Cyclic voltammogram of the P-axial heterostructure at sweep rate of 5mV/s (FIG. b);
FIG. 5 is a graph of rate capability of cobaltosic oxide nanowires prepared in example 1 of the present invention (FIG. a) and Co3O4/Co2Graph of the rate performance of the P-axial heterostructure (graph b).
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
co3O4/Co2The preparation process of the P coaxial heterostructure micro supercapacitor electrode material, as shown in figure 1, comprises the following steps:
1) preparing the cobalt hydroxide nanowire by a hydrothermal method:
1a) cleaning foamed nickel: firstly, shearing foamed nickel, sequentially performing ultrasonic treatment on the foamed nickel for 15 minutes by using hydrochloric acid, deionized water, acetone and ethanol, drying the foamed nickel in an oven at the temperature of 60 ℃ for 12 hours, taking out the dried foamed nickel, and weighing the mass of the dried foamed nickel;
1b) adding 2mmol of cobalt chloride hexahydrate, 1mmol of ammonium fluoride and 4mmol of urea into 70mL of deionized water, and stirring for 15 minutes to dissolve the cobalt chloride hexahydrate, the ammonium fluoride and the urea uniformly;
1c) adding the solution into a polytetrafluoroethylene reaction kettle, adding the weighed foam nickel after cleaning, carrying out hydrothermal treatment at 120 ℃ for 8-12 hours, cooling, carrying out centrifugal washing by using deionized water and ethanol, and drying in an oven to obtain the foam nickel loaded with the cobalt hydroxide nanowires;
2) taking sodium hypophosphite pyrolysis as a phosphine source, placing the cobalt hydroxide nanowires and sodium hypophosphite into two porcelain boats according to the mass ratio of 1:10, placing the porcelain boats together into a tubular furnace, heating to 300 ℃ at the speed of 2 ℃/min, and preserving heat for 3 hours to obtain the cobalt phosphide nanowires.
3) And (3) putting the cobaltous hydroxide nanowire into a tube furnace, taking argon as protective atmosphere, heating to 350 ℃ at the speed of 2 ℃/min, and preserving heat for 2 hours to obtain the cobaltosic oxide nanowire.
4) Putting the cobalt phosphide nanowire into a rapid annealing furnace, heating to 250 ℃ at the speed of 5 ℃/min, and preserving the temperature for 3 minutes to oxidize the cobalt phosphide on the surface, thereby obtaining Co3O4/Co2A P-coaxial heterostructure.
5) A three-electrode test system is constructed by taking a 1mol/L potassium hydroxide aqueous solution as an electrolyte and using a mercury-mercury oxide reference electrode to test electrochemical properties, including cyclic voltammetry, constant current charge and discharge and the like. And weighing the mass to obtain the loading capacity of the active material on the foamed nickel, and calculating the mass specific capacity of the material.
6) With Co3O4/Co2P coaxial heterostructure as anode material and Fe2O3The nano-wire structure is made of a negative electrode material, and a microelectrode is prepared by adopting a nano-indentation technology and assembled into the asymmetric micro supercapacitor.
Co obtained in this example3O4/Co2P coaxial heterostructure micro super capacitor electrode material with Co as inner layer2P, the outer layer being Co3O4. By adopting the synthesis scheme, the diameter of the cobalt phosphide nanowire structure is about 100 nanometers (as shown in figure 2 a), the length of the cobalt phosphide nanowire structure is 800 nanometers (as shown in figure 2 a), and the nanowires are uniformly grown on the foamed nickel substrate. Co3O4/Co2The outer layer of the P coaxial heterostructure is Co3O4An oxide layer (shown in fig. 3) having a thickness of 1.2 to 2 nm. Co obtained by sintering in argon3O4Morphology of nanowires substantially associated with hydrogenThe cobalt oxide nanowires were uniform. Co due to the crystal transformation during sintering3O4The nano-wire is actually formed by connecting a plurality of tiny nano-rods with each other and arranging the nano-wires into a nano-wire shape. Co obtained by sintering in hydrogen phosphide atmosphere2Co finally obtained after P surface oxidation3O4/Co2The P coaxial heterostructure, which has the same morphology as the cobalt phosphide nanowire, uniformly grows on the foamed nickel substrate (as shown in fig. 2 b). Synthetic Fe2O3The nanowires are about 70 nm in diameter and about 500 nm in length and are uniformly grown on the foamed nickel substrate (as shown in fig. 2 c).
Co obtained in this example3O4/Co2The P coaxial heterostructure micro supercapacitor electrode material is tested in 1mol/L potassium hydroxide aqueous solution, and Co is added under the current density of 1A/g3O4The specific capacity of nanowire mass is 767F/g, Co2The specific mass capacity of the P nanowire is 446F/g (shown in figure 4 a), and the Co is3O4/Co2The P-axial heterostructure has a specific mass capacity of 590F/g (as shown in fig. 4 b). At a current density of 20A/g, Co3O4The specific mass capacity of the nanowire is that the specific mass capacity can still be maintained at 390F/g, and the capacity is attenuated 49.15% (as shown in figure 5 a); co3O4/Co2The P coaxial heterostructure has the specific mass capacity up to 468F/g and the capacity attenuation of only 20.68 percent (as shown in figure 5 b). Co3O4/Co2The P coaxial heterostructure serving as the super capacitor has excellent rate performance and chemical stability. In the construction of the energy production-storage-function integrated device, due to its high energy density, the LED or the like can be lit up when the solar cell is disconnected after being used in conjunction with the solar cell.
Example 2:
co3O4/Co2The preparation process of the P coaxial heterostructure micro supercapacitor electrode material comprises the following steps:
1) preparing the cobalt hydroxide nanowire by a hydrothermal method:
1a) cleaning foamed nickel: firstly, shearing foamed nickel, sequentially performing ultrasonic treatment on the foamed nickel for 15 minutes by using hydrochloric acid, deionized water, acetone and ethanol, drying the foamed nickel in an oven at the temperature of 60 ℃ for 12 hours, taking out the dried foamed nickel, and weighing the mass of the dried foamed nickel;
1b) respectively adding 5mmol of cobalt chloride hexahydrate, 2.5mmol of ammonium fluoride and 10mmol of urea into 70mL of deionized water, and stirring for 20 minutes to uniformly dissolve the cobalt chloride hexahydrate, the ammonium fluoride and the urea;
1c) adding the solution into a polytetrafluoroethylene reaction kettle, adding the weighed foam nickel after cleaning, carrying out hydrothermal treatment at 120 ℃ for 8-12 hours, cooling, carrying out centrifugal washing by using deionized water and ethanol, and drying in an oven to obtain the foam nickel loaded with the cobalt hydroxide nanowires;
2) taking sodium hypophosphite pyrolysis as a phosphine source, placing the cobalt hydroxide nanowires and sodium hypophosphite into two porcelain boats according to the mass ratio of 1:10, placing the porcelain boats together into a tubular furnace, heating to 300 ℃ at the speed of 2 ℃/min, and preserving heat for 3 hours to obtain the cobalt phosphide nanowires.
3) And (3) putting the cobaltous hydroxide nanowire into a tube furnace, taking argon as protective atmosphere, heating to 350 ℃ at the speed of 2 ℃/min, and preserving heat for 2 hours to obtain the cobaltosic oxide nanowire.
4) Putting the cobalt phosphide nanowire into a rapid annealing furnace, heating to 250 ℃ at the speed of 5 ℃/min, and preserving the temperature for 3 minutes to oxidize the cobalt phosphide on the surface, thereby obtaining Co3O4/Co2A P-coaxial heterostructure.
5) A three-electrode test system is constructed by taking a 1mol/L potassium hydroxide aqueous solution as an electrolyte and using a mercury-mercury oxide reference electrode to test electrochemical properties, including cyclic voltammetry, constant current charge and discharge and the like. And weighing the mass to obtain the loading capacity of the active material on the foamed nickel, and calculating the mass specific capacity of the material.
6) With Co3O4/Co2P coaxial heterostructure as anode material and Fe2O3The nano-wire structure is made of a negative electrode material, and a microelectrode is prepared by adopting a nano-indentation technology and assembled into the asymmetric micro supercapacitor.
Co obtained in this example3O4/Co2P coaxial heterostructure micro supercapacitor electrode material tested in 1mol/L potassium hydroxide aqueous solutionAt a current density of 1A/g, Co3O4The specific capacity of the nanowire reaches 700F/g, Co2The specific mass capacity of the P nanowire is 440F/g, and the P nanowire is Co3O4/Co2The specific mass capacity of the P coaxial heterostructure is 557F/g. At a current density of 20A/g, Co3O4/Co2The specific capacity of the P coaxial heterostructure reaches 432F/g, and the capacity attenuation is only 22.44%. Co3O4/Co2The P coaxial heterostructure serving as the super capacitor has excellent rate performance and chemical stability. In the construction of the energy production-storage-function integrated device, due to its high energy density, the LED or the like can be lit up when the solar cell is disconnected after being used in conjunction with the solar cell.
Example 3:
co3O4/Co2The preparation process of the P coaxial heterostructure micro supercapacitor electrode material comprises the following steps:
1) preparing the cobalt hydroxide nanowire by a hydrothermal method:
1a) cleaning foamed nickel: firstly, shearing foamed nickel, sequentially performing ultrasonic treatment on the foamed nickel for 15 minutes by using hydrochloric acid, deionized water, acetone and ethanol, drying the foamed nickel in an oven at the temperature of 60 ℃ for 12 hours, taking out the dried foamed nickel, and weighing the mass of the dried foamed nickel.
1b) 10mmol of cobalt chloride hexahydrate, 5mmol of ammonium fluoride and 20mmol of urea are respectively added into 70mL of deionized water, and stirred for 30 minutes to be uniformly dissolved.
1c) Adding the solution into a polytetrafluoroethylene reaction kettle, adding the weighed foam nickel after cleaning, carrying out hydrothermal treatment at 120 ℃ for 8-12 hours, cooling, carrying out centrifugal washing by using deionized water and ethanol, and drying in an oven to obtain the foam nickel loaded with the cobalt hydroxide nanowires.
2) Taking sodium hypophosphite pyrolysis as a phosphine source, placing the cobalt hydroxide nanowires and sodium hypophosphite into two porcelain boats according to the mass ratio of 1:10, placing the porcelain boats together into a tubular furnace, heating to 300 ℃ at the speed of 2 ℃/min, and preserving heat for 3 hours to obtain the cobalt phosphide nanowires.
3) And (3) putting the cobaltous hydroxide nanowire into a tube furnace, taking argon as protective atmosphere, heating to 350 ℃ at the speed of 2 ℃/min, and preserving heat for 2 hours to obtain the cobaltosic oxide nanowire.
4) Putting the cobalt phosphide nanowire into a rapid annealing furnace, heating to 250 ℃ at the speed of 5 ℃/min, and preserving the temperature for 3 minutes to oxidize the cobalt phosphide on the surface, thereby obtaining Co3O4/Co2A P-coaxial heterostructure.
5) A three-electrode test system is constructed by taking a 1mol/L potassium hydroxide aqueous solution as an electrolyte and using a mercury-mercury oxide reference electrode to test electrochemical properties, including cyclic voltammetry, constant current charge and discharge and the like. And weighing the mass to obtain the loading capacity of the active material on the foamed nickel, and calculating the mass specific capacity of the material.
6) With Co3O4/Co2P coaxial heterostructure as anode material and Fe2O3The nano-wire structure is made of a negative electrode material, and a microelectrode is prepared by adopting a nano-indentation technology and assembled into the asymmetric micro supercapacitor.
Co obtained in this example3O4/Co2The P coaxial heterostructure micro supercapacitor electrode material is tested in 1mol/L potassium hydroxide aqueous solution, and Co is added under the current density of 1A/g3O4The specific capacity of nanowire mass is up to 680F/g, Co2The specific mass capacity of the P nanowire is 423F/g, Co3O4/Co2The specific mass capacity of the P coaxial heterostructure is 543F/g. At a current density of 20A/g, Co3O4/Co2The specific capacity of the P coaxial heterostructure reaches 416F/g, and the capacity attenuation is only 23.38%. Co3O4/Co2The P coaxial heterostructure serving as the super capacitor has excellent rate performance and chemical stability. In the construction of the energy production-storage-function integrated device, due to its high energy density, the LED or the like can be lit up when the solar cell is disconnected after being used in conjunction with the solar cell.
Claims (1)
1.Co3O4/Co2Application of P coaxial heterostructure material as electrode anode material of micro super capacitor, and Co3O4/Co2P coaxial heterostructureThe material is a coaxial heterostructure, the diameter is between 70 nanometers and 300 nanometers, the length is between 600 nanometers and 2 micrometers, and the inner layer of the coaxial heterostructure of the nanowire is Co2P, the outer layer being Co3O4Outer layer of Co3O4The oxide layer is 1.2 to 2 nanometers thick.
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