CN110136978B - Reduced graphene/alpha-Fe2O3Super capacitor material and preparation method and application thereof - Google Patents
Reduced graphene/alpha-Fe2O3Super capacitor material and preparation method and application thereof Download PDFInfo
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- 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
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- 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
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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
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- H—ELECTRICITY
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- 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
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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
Reduced graphene/alpha-Fe2O3Supercapacitor material, preparation method and application thereof, and reduced graphene/alpha-Fe2O3The preparation method of the supercapacitor material comprises the following steps: (1) mixing Fe (NO)3)3·9H2O, CTAB, dissolving the urea and graphene oxide dispersion liquid in a methanol solution, and carrying out hydrothermal reaction at 160-200 ℃ for 8-24 h; (2) carrying out suction filtration on the reaction product obtained in the step (1), adding the obtained solid and thiourea into water, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction at 160-200 ℃ for 8-24 h; (3) and (3) carrying out suction filtration, freeze drying and heat treatment on the product obtained in the step (2). The working electrode of the supercapacitor material disclosed by the invention is simple to prepare, the electrochemical working window is-1.05 to-0.3V in an alkaline electrolyte, and the highest specific capacity can reach 1296F/g, so that the supercapacitor material is an ideal negative electrode material; the invention overcomes the defect of lower specific capacity of the cathode material of the super capacitor, is expected to solve the problem of unmatched specific capacities of the anode and the cathode of the super capacitor, and has higher research value.
Description
Technical Field
The invention belongs to the technical field of preparation of supercapacitor materials, and particularly relates to reduced graphene/alpha-Fe2O3A super capacitor material and a preparation method and application thereof.
Background
With the rapid development of economy in China, the living standard and consumption standard of people are continuously improved and enhanced. Meanwhile, automobile exhaust (oxynitride and carbon monoxide), industrial waste gas, solid particles and the like cause serious pollution to air which people rely on to live, the normal life and the body health of people are seriously influenced, and the solution of the environmental problem is not slow. Therefore, the development of low-cost and energy-efficient energy storage devices is an urgent problem to be solved. A super capacitor, also called an electrochemical capacitor, is a novel energy storage device, has the characteristics of higher specific capacity, high energy density, good service life and capability of realizing rapid charge and discharge, and the advantages promote the application of the super capacitor in many fields.
One of the key technologies in current supercapacitors is to obtain an excellent electrode material, which requires good conductivity and sufficient reactive sites to provide high specific capacity. Generally, the cathode material has a high specific capacity, and the traditional cathode material always backs a black pan with a low specific capacity, so that more energy is put into the research of the cathode material by technical workers, and the cathode material is greatly cooled. The low capacity characteristics of the cathode material also make it difficult to match with high capacity cathode materials to obtain high performance supercapacitor devices. Therefore, the significance of effectively preparing the high-performance cathode material is significant. However, the iron oxide is a more traditional cathode material, the resource is rich, and if the effective construction of the iron oxide nano material and the particle size control are realized, a larger specific surface area can be provided to generate more active sites, so that the electrochemical performance of the iron oxide nano material can be improved; in addition, the iron oxide and the reduced graphene are compounded, so that the conductivity of the electrode material can be improved, and the specific capacity of the electrode material can be improved.
Therefore, the reduced graphene and iron oxide composite material with high performance is constructed, and has high research value in the field of super capacitors.
Disclosure of Invention
To solve the above problems, it is an object of the present invention to provide a reduced graphene/α -Fe2O3A super capacitor material and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme thatReduced graphene/alpha-Fe2O3The preparation method of the supercapacitor material comprises the following steps:
(1) 0.404-0.606 g Fe (NO)3)3·9H2Dissolving O, 0.05-0.2 g of CTAB (cetyl trimethyl ammonium bromide), 0.4-0.8 g of urea and 20-40 mL of graphene oxide dispersion in 30-50 mL of methanol solution (the volume ratio of water to methanol is 1: 4-1: 1), and carrying out hydrothermal reaction at 160-200 ℃ for 8-24 h;
(2) carrying out suction filtration on the reaction product obtained in the step (1), adding the obtained solid and 0.3-1.0 g of thiourea into 30-40 mL of water, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction at 160-200 ℃ for 8-24 h;
(3) carrying out suction filtration, freeze drying and heat treatment on the product obtained in the step (2); the heat treatment conditions are as follows: under the protection of inert gas atmosphere, heating to 170-190 ℃ at a heating rate of 1.5-2.5 ℃/min, and keeping at 170-190 ℃ for 30-60 min.
Preferably, the concentration of the graphene oxide dispersion liquid in the step (1) is 1.5-2.5 mg/mL.
Preferably, the heat treatment conditions are: in N2Under the protection of atmosphere, the temperature is raised to 180 ℃ at the heating rate of 2 ℃/min, and the temperature is kept at 180 ℃ for 30 min.
The reduced graphene/alpha-Fe2O3The super capacitor material is applied to a super capacitor after being activated under the potential of-1.3V to-0.3V.
The invention has the following beneficial effects: the invention provides reduced graphene/alpha-Fe2O3The raw materials used in the preparation method of the supercapacitor material are easy to obtain, are all industrial products, and have low price, simple preparation method and small pollution; the whole process has good safety and controllability, high yield of target products, good quality and low total cost, and is suitable for industrial production. In the prepared electrode material, alpha-Fe2O3The particle diameter of the anode material is between 20 and 100 nm, the electrochemical window of the electrode material is between-1.05 and-0.3V, the specific capacity is up to 1296F/g, and the defects of low capacity and high capacity of the conventional anode material are well overcomeIn two aspects, firstly, a reaction carrier with a large area is provided by adopting three-dimensional graphene, and the problem that ethylene glycol is required to be added as a suspension solution to prepare small nano iron oxide particles in the prior art is avoided; adopts water and methanol as mixed solvent, and utilizes urea to hydrolyze in water to generate hydroxyl ions (OH)-) And further with iron ions (Fe)3+) Hydrothermally generating iron hydroxide nanoparticles; the urea is firstly decomposed into ammonia gas, hydrogen bonds can be formed between the ammonia gas and water and methanol, the speed of further hydrolyzing the ammonia gas into hydroxide ions is inhibited, so that the iron ions and the hydroxide ions can be uniformly combined to obtain smaller nano particles, if strong base such as NaOH is added into an iron ion solution, iron hydroxide particles are easily and directly generated, and the nano iron hydroxide particles with smaller sizes are difficult to control. Second, addition of thiourea, H produced by thiourea2S is further hydrolyzed to obtain S2-The ion can react with ferric hydroxide to obtain Fe2S3(because of its smaller Ksp value), Fe2S3Unstable, the final stable product being alpha-Fe2O3In the process, the surface of the iron oxide particle after vulcanization has more reactive active sites than the surface of the ferric hydroxide nanoparticle which is not vulcanized, and the rapid shuttling of electrolyte ions is facilitated, so that the electrochemical performance is better; meanwhile, thiourea is added, so that the problem that the compound of the reduced graphene and the iron oxide can be obtained only by high-temperature treatment of the compound of the reduced graphene and the iron hydroxide obtained in the step (1) can be solved, and the composite material has a high specific surface area. Thirdly, the electrode material is activated under the potential of-1.3V to-0.3V, so that the reduced graphene/alpha-Fe is greatly improved2O3Specific capacity of the supercapacitor material. The method provides possibility for the industrial production of high-performance super capacitor devices, is an excellent super capacitor cathode material, and has high application value.
Drawings
FIG. 1 shows reduced graphene/α -Fe prepared in example 1 of the present invention2O3XRD patterns of supercapacitor materials;
FIG. 2 shows reduced graphene/α -Fe prepared in example 1 of the present invention2O3XPS plot of supercapacitor material;
FIG. 3 shows reduced graphene/α -Fe prepared in example 1 of the present invention2O3SEM images of supercapacitor materials;
FIG. 4 shows reduced graphene/α -Fe prepared in example 1 of the present invention2O3A TEM image of the supercapacitor material;
FIG. 5 shows reduced graphene/α -Fe in example 1 of the present invention2O3A CV plot of the supercapacitor electrode material;
FIG. 6 shows reduced graphene/α -Fe in example 1 of the present invention2O3A constant current charge-discharge curve graph of the electrode material of the super capacitor under different current densities;
FIG. 7 shows reduced graphene/α -Fe in example 1 of the present invention2O3An electrochemical impedance plot of the supercapacitor electrode material;
FIG. 8 is a CV diagram and a constant current charging and discharging curve diagram of a reduced graphene/α -Fe2O3 supercapacitor electrode material prepared in example 4 of the present invention;
fig. 9 is a CV graph and a constant current charging and discharging curve of the electrode material obtained when thiourea is not added to the reduced graphene/α -Fe2O3 supercapacitor electrode material prepared in example 5 of the present invention.
Detailed Description
In order to make the objects and advantages of the present invention more apparent, the present invention is further described below with reference to examples. Furthermore, various changes and modifications may be made by those skilled in the art after reading the teachings herein, and such equivalents are intended to fall within the scope of the appended claims.
Example 1
Reduced graphene/alpha-Fe2O3The preparation method of the supercapacitor material comprises the following steps:
(1) 0.404 g Fe (NO)3)3·9H2O, 0.1 g CTAB, 0.6 g urea and 30mL of graphene oxide dispersion (2 mg/mL) were dissolved in 40Reacting in mL methanol solution (volume ratio of water to methanol is 3: 4) at 180 deg.C in 100 mL reaction kettle for 12 h;
(2) carrying out suction filtration on the reaction product obtained in the step (1), adding the obtained solid and 0.6 g of thiourea into 35mL of water, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction at 180 ℃ for 12 h;
(3) carrying out suction filtration, freeze drying and heat treatment on the product obtained in the step (2); the heat treatment conditions are as follows: in N2Under the protection of atmosphere, heating to 180 ℃ at the heating rate of 2 ℃/min, and keeping at 180 ℃ for 30min to obtain reduced graphene and alpha-Fe2O3Black powder of nano-particle composite material.
The powder phase structure of the powder can be seen from an XRD (fig. 1), and diffraction peaks corresponding to the powder are respectively 24.138 degrees, 33.152 degrees, 35.611 degrees, 40.854 degrees, 43.518 degrees, 49.479 degrees, 54.089 degrees, 57.589 degrees, 62.449 degrees, 63.989 degrees, 69.599 degrees, 71.935 degrees, 75.428 degrees, 77.727 degrees, 80.709 degrees, 84.913 degrees and 88.539 degrees which are known by a map and well equal to alpha-Fe2O3(PDF:33-0664) and the peak position at about 24.138 degrees is overlapped with the peak of the reduced graphene, which shows that the reduced graphene is combined with alpha-Fe2O3The complex of (1). Fig. 2 is an XPS diagram of the composite, from which it can be observed that the composite contains three elements of C, O and Fe, and it is known that the XPS peak of the Fe element is a trivalent Fe atom, and fig. 3 is an SEM diagram of the composite, from which it can be seen that the composite has many pore structures, which are beneficial for the rapid shuttling of electrolyte ions and provide more reactive sites. FIG. 4 is a TEM image of the composite material, from which it can be more clearly observed that the reduced graphene with the corrugated structure and the alpha-Fe2O3Are well combined together and are alpha-Fe2O3Most of the particles are irregular particles, only a few of the particles have a regular rhombohedral structure, and the alpha-Fe2O3The particle size is between about 30-80 nm. Reducing graphene with alpha-Fe2O3The nano-particle composition not only can improve the conductivity of the composite material, but also can improve the small-sized alpha-Fe2O3The nanoparticles can provide a higher specific surface area, so thatThe composite material has higher specific capacity.
Using the obtained reduced graphene and alpha-Fe2O3Uniformly mixing the nanoparticle composite material, the conductive carbon black and Polytetrafluoroethylene (PTFE) according to a mass ratio of 80: 15: 5, preparing a uniform film, drying the film in a drying oven at 120 ℃ for 12 hours, and pressing a certain amount of the film on nickel foam under the pressure of 10MPa to prepare the working electrode. The electrode material was then electrochemically tested in 2M KOH electrolyte, with a platinum sheet as the counter electrode and HgO/HgO as the reference electrode, under the test system CHI 660E.
As shown in FIG. 5a, when the electrode material has a scanning rate of 20 mV/s and the electrochemical window of the CV curve of the first circle is-1.05 to-0.3V, the CV area is smaller; when the electrochemical window of the second circle of CV curve is-1.15 to-0.3V, the CV area is obviously increased; when the electrochemical window of the third CV curve is-1.3 to-0.3V, the CV area becomes larger; when the electrochemical window of the CV curve in the fourth circle is changed to-1.05 to-0.3V again, the CV area is much larger than that in the first circle, which shows that the specific capacity of the electrode material is greatly improved after the electrode material is activated under the potential of-1.3 to-0.3V. FIG. 5b shows that at scan rates of 5-25 mV/s for the electrode material, different CV curves with a distinct pair of redox peaks and increasing area of the CV curve with increasing scan rate can be obtained at electrochemical windows of-1.05 to-0.3V. FIG. 6 shows the constant current charging and discharging curves of the electrode material at 2, 4, 6, 8 and 10A/g, and the specific capacities at these current densities are 1296F/g, 1214F/g, 1181F/g, 1156F/g and 1128F/g, respectively, which shows that the electrode material has higher specific capacity. Fig. 7 shows an impedance diagram of the electrode material, which can be seen to have a lower resistance.
Example 2
Reduced graphene/alpha-Fe2O3The preparation method of the supercapacitor material comprises the following steps:
(1) 0.606g Fe (NO)3)3·9H2O, 0.2g CTAB, 0.8g urea and 20 mL of graphene oxide dispersion (concentration 1.5 mg/mL) were dissolved in 30mL of methanolCarrying out hydrothermal reaction for 8 h at 200 ℃ in a liquid (the volume ratio of water to methanol is 3: 4);
(2) carrying out suction filtration on the reaction product obtained in the step (1), adding the obtained solid and 0.3 g of thiourea into 30mL of water, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction for 8 h at 200 ℃;
(3) carrying out suction filtration, freeze drying and heat treatment on the product obtained in the step (2); the heat treatment conditions are as follows: in N2Under the protection of atmosphere, heating to 190 ℃ at the heating rate of 1.5 ℃/min, and keeping at 190 ℃ for 30min to obtain reduced graphene and alpha-Fe2O3Black powder of nano-particle composite material.
Example 3
Reduced graphene/alpha-Fe2O3The preparation method of the supercapacitor material comprises the following steps:
(1) 0.505 g of Fe (NO)3)3·9H2Dissolving O, 0.05 g CTAB, 0.4 g urea and 40mL of graphene oxide dispersion (the concentration is 2.5 mg/mL) in 50 mL of methanol solution (the volume ratio of water to methanol is 3: 4), and carrying out hydrothermal reaction at 160 ℃ for 24 h;
(2) carrying out suction filtration on the reaction product obtained in the step (1), adding the obtained solid and 1.0 g of thiourea into 40mL of water, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction at 160 ℃ for 24 h;
(3) carrying out suction filtration, freeze drying and heat treatment on the product obtained in the step (2); the heat treatment conditions are as follows: in N2Under the protection of atmosphere, heating to 170 ℃ at the heating rate of 2.5 ℃/min, and keeping at 170 ℃ for 60min to obtain reduced graphene and alpha-Fe2O3Black powder of nano-particle composite material.
Example 4
Fe (NO) was added to the mixture of example 13)39H2O mass was adjusted to 0.2g, with all other steps and synthesis parameters unchanged, to prepare working electrodes. As shown in FIG. 8, when the amount of the added ferric nitrate was small, the specific capacity of the prepared electrode material was 440F/g at a current density of 2A/g. The specific capacity is significantly reduced compared to example 1, saidThe reason why the specific capacity of the composite material is high is mainly caused by alpha-Fe2O3Is contributed.
Example 5
On the basis of example 1, thiourea was removed and the other steps and synthesis parameters were unchanged. As shown in FIG. 9, the results of constant current charge and discharge tests on the electrode material obtained by hydrothermal reaction without adding thiourea show that the constant current charge and discharge curves of the electrode material at 2, 4, 6, 8 and 10A/g have specific capacities of 1098F/g, 800F/g, 660F/g, 568F/g and 500F/g at the current densities. The comparison shows that the electrode material obtained by adding thiourea for hydrothermal reaction has better performance.
Claims (5)
1. Reduced graphene/alpha-Fe2O3The preparation method of the supercapacitor material is characterized by comprising the following steps of:
(1) 0.404-0.606 g Fe (NO)3)3·9H2Dissolving O, 0.05-0.2 g of CTAB, 0.4-0.8 g of urea and 20-40 mL of graphene oxide dispersion liquid in 30-50 mL of methanol solution, and carrying out hydrothermal reaction at 160-200 ℃ for 8-24 h, wherein the volume ratio of water to methanol in the methanol solution is 1: 4-1: 1;
(2) carrying out suction filtration on the reaction product obtained in the step (1), adding the obtained solid and 0.3-1.0 g of thiourea into 30-40 mL of water, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction at 160-200 ℃ for 8-24 h;
(3) carrying out suction filtration, freeze drying and heat treatment on the product obtained in the step (2); the heat treatment conditions are as follows: under the protection of inert gas atmosphere, heating to 170-190 ℃ at a heating rate of 1.5-2.5 ℃/min, and keeping at 170-190 ℃ for 30-60 min.
2. Reduced graphene/α -Fe as in claim 12O3The preparation method of the supercapacitor material is characterized by comprising the following steps: the concentration of the graphene oxide dispersion liquid in the step (1) is 1.5-2.5 mg/mL.
3. Reduced graphene/α -Fe as in claim 12O3The preparation method of the supercapacitor material is characterized by comprising the following steps: the heat treatment conditions are as follows: in N2Under the protection of atmosphere, the temperature is raised to 180 ℃ at the heating rate of 2 ℃/min, and the temperature is kept at 180 ℃ for 30 min.
4. Reduced graphene/alpha-Fe prepared by the method of any one of claims 1 to 32O3A supercapacitor material.
5. The reduced graphene/α -Fe of claim 42O3The super capacitor material is applied to a super capacitor after being activated under the potential of-1.3V to-0.3V.
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