CN111128560A - Preparation method and application of iron oxide/graphene composite nano material - Google Patents
Preparation method and application of iron oxide/graphene composite nano material Download PDFInfo
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- CN111128560A CN111128560A CN201911280665.1A CN201911280665A CN111128560A CN 111128560 A CN111128560 A CN 111128560A CN 201911280665 A CN201911280665 A CN 201911280665A CN 111128560 A CN111128560 A CN 111128560A
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
The invention discloses a preparation method of an iron oxide/graphene composite nano material, which comprises the following steps: (1) adding polyvinylpyrrolidone and potassium ferricyanide into 0.1M hydrochloric acid solution, fully stirring and reacting completely to obtain clear precursor solution; (2) adding graphene oxide into the obtained precursor solution, fully mixing, putting into a reaction kettle, reacting for 24 hours at 80 ℃, filtering to obtain a blue solid, sequentially cleaning for 3 times by using ethanol and redistilled water, and vacuum-drying for 12 hours at 95 ℃ to obtain the ferric ferricyanide/graphene oxide composite material; (3) and putting the prepared ferric ferricyanide/graphene composite material into a muffle furnace, and calcining for 6 hours at 200-600 ℃ to obtain the ferric oxide/graphene composite material. According to the invention, prussian blue type compounds, namely ferric ferricyanide and graphene oxide, are used as precursors, the iron oxide/graphene composite material is prepared through heating and decomposition, and the iron oxide/graphene composite material is self-assembled into a nanocube structure and can adapt to rapid conduction of electrons and ions.
Description
Technical Field
The invention belongs to the technical field of nano functional materials, and particularly relates to a preparation method and application of an iron oxide/graphene composite nano material.
Background
The ferric oxide has the characteristics of wide electrochemical window, various valence state changes and the like, is a more ideal pseudocapacitance material, and the limited conductivity of the ferric oxide influences the exertion of electrochemical performance. Currently, a common improvement method is to compound iron oxide with a carbon material with good conductivity, such as graphene and carbon nanotubes, and obtain an iron oxide/graphene composite material by utilizing a physical or chemical action between the iron oxide and the graphene. The composite material has a unique nano structure, is beneficial to forming more electrode/electrolyte interfaces, and is expected to improve the performance of the super capacitor. Therefore, the synthesis of iron oxide and graphene composite nano-materials has become one of the research hotspots in the field of materials. For example, patent with application number CN201710031844.6 discloses a preparation method of a graphene-iron oxide-graphene composite structure battery negative electrode material; for example, patent with application number CN201611071556.5 discloses a preparation method of an iron oxide/graphene film supercapacitor electrode material; for example, patent with application number CN201611009344.4 discloses a preparation method of a supercapacitor 3D iron oxide/graphene composite electrode material. However, the cubic iron oxide/graphene composite nano material and the synthesis thereof are still blank in the field of nano materials in China.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method and application of an iron oxide/graphene composite nano material.
The technical scheme of the invention is summarized as follows:
a preparation method of an iron oxide/graphene composite nano material comprises the following steps:
(1) preparing a ferric ferricyanide precursor solution: adding polyvinylpyrrolidone and potassium ferricyanide into 0.1M hydrochloric acid solution, fully stirring and reacting completely to obtain clear precursor solution;
(2) synthesizing a ferric ferricyanide/graphene composite material: adding graphene oxide into the obtained precursor solution, fully mixing, putting into a reaction kettle, reacting for 24 hours at 80 ℃, filtering to obtain a blue solid, sequentially cleaning for 3 times by using ethanol and redistilled water, and vacuum-drying for 12 hours at 95 ℃ to obtain the ferric ferricyanide/graphene oxide composite material;
(3) synthesizing an iron oxide/graphene composite material: and putting the prepared ferric ferricyanide/graphene composite material into a muffle furnace, and calcining for 6 hours at 200-600 ℃ to obtain the ferric oxide/graphene composite material.
Preferably, the ratio of the polyvinylpyrrolidone to the potassium ferricyanide to the hydrochloric acid solution to the graphene oxide is 3.8 g: 1 mmol: 50mL of: 0.1 g.
An application of an iron oxide/graphene composite nano material in an electrode material of a super capacitor.
Preferably, the specific capacity of the iron oxide/graphene composite nano material reaches 264F/g.
The invention has the beneficial effects that:
1. according to the invention, the prussian blue type compound ferric ferricyanide and graphene oxide are used as precursors for the first time, and the iron oxide/graphene composite nano material with a cubic structure is self-assembled, so that the iron oxide/graphene composite nano material can adapt to rapid conduction of electrons and ions. Wherein, ferricyanide is cubic structure, and in the thermal decomposition process, oxidation reaction and decomposition reaction are carried out simultaneously, and the maintenance of cubic structure is realized. The graphene oxide provides support for the cubic structure on one hand; on the other hand, the oxygen-containing groups on the surface provide a more sufficient oxidation environment, and at the same time, the graphene oxide reacts with ferric ferricyanide and is reduced to graphene, so that the conductivity is improved.
2. The iron oxide/graphene composite material prepared by the invention has the following advantages: (1) the special cubic structure of the iron oxide can accelerate the conduction of electrons and ions; (2) the graphene improves the conductivity of the iron oxide/graphene composite material, iron oxide particles are dispersed due to the existence of the graphene, more reactive active sites are exposed, and meanwhile, the volume change of the pseudocapacitance material in the circulation process is favorably alleviated.
Drawings
FIG. 1 is a flow chart of a method for preparing an iron oxide/graphene composite nanomaterial of the present invention;
FIG. 2 is an X-ray diffraction characterization of the FeHCF/GO composite made in example 1;
FIG. 3 is a scanning electron micrograph of a FeHCF/GO composite made in example 1;
FIG. 4 shows Fe prepared in example 12O3Scanning electron microscope images of the/G composite material;
FIG. 5 shows Fe prepared in example 22O3And an electrochemical characterization diagram of the/G composite material electrode.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
Example 1 preparation of iron oxide/graphene composite nanomaterial
(1) Preparing a ferric ferricyanide precursor solution: adding 3.8g of polyvinylpyrrolidone and 1mmol of potassium ferricyanide into 50mL of 0.1M hydrochloric acid solution, and fully stirring until the reaction is complete to obtain a clear precursor solution;
(2) synthesizing a ferric ferricyanide/graphene composite material: adding 0.1g of graphene oxide into the obtained precursor solution, fully mixing, putting into a reaction kettle, reacting for 24 hours at 80 ℃, filtering to obtain a blue solid, sequentially cleaning for 3 times by using ethanol and redistilled water, and carrying out vacuum drying for 12 hours at 95 ℃ to obtain a FeHCF/GO composite material;
(3) synthesizing an iron oxide/graphene composite material: putting the prepared ferric ferricyanide/graphene composite material into a muffle furnace, and calcining for 6h at 500 ℃ to obtain Fe2O3a/G composite material.
Example 2 electrochemical testing of the iron oxide/graphene composite material prepared in example 1
(1) Preparing an electrode: the electrode material to be tested was Fe2O3Composite material/G Fe prepared in example 12O3the/G composite material is an active material, acetylene black is a conductive agent, and polyvinylidene fluoride is a bonding agent according to a mass ratio of 80: 10: 10, taking N-methyl pyrrolidone as a solvent, and grinding the mixture into uniform slurry in a mortar;
dropping the slurry on carbon paper, controlling the electrode area to be 2.0cm multiplied by 1.0cm, the mass of the active electrode material to be about 1mg, and drying at 80 ℃ to obtain Fe2O3a/G composite electrode;
(2) electrochemical testing: electrochemical performance testing in a three-electrode system
The electrolyte is alkaline electrolyte (1M KOH), and the working electrode is prepared Fe2O3The counter electrode is a platinum sheet, and the reference electrode is Hg/HgO;
testing of Fe by cyclic voltammetry2O3The energy storage mechanism and the specific capacity of the/G composite material electrode. As shown in FIG. 5Fe2O3Shown in the electrochemical characterization chart of the electrode of the/G composite material, Fe2O3the/G composite material electrode has obvious oxidation peaks and reduction peaks in a test interval, and shows that the energy is stored by using the oxidation-reduction reaction on the surface of the material.
And (3) calculating the specific capacity of the electrode material based on the cyclic voltammetry curve, wherein the calculation formula is as follows:
Vaand VcRespectively represent a maximum voltage and a minimum voltage; Δ V (V) is the potential window (from V) of the testaTo Vc) (ii) a m (g) is the mass of the electrode material; v (mV s)-1) Is the sweep rate in cyclic voltammetry tests.
According to the calculation formula, the prepared Fe is obtained2O3the/G composite material electrode has a specific capacity of 264F/G.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (4)
1. The preparation method of the iron oxide/graphene composite nano material is characterized by comprising the following steps:
(1) preparing a ferric ferricyanide precursor solution: adding polyvinylpyrrolidone and potassium ferricyanide into 0.1M hydrochloric acid solution, fully stirring and reacting completely to obtain clear precursor solution;
(2) synthesizing a ferric ferricyanide/graphene composite material: adding graphene oxide into the obtained precursor solution, fully mixing, putting into a reaction kettle, reacting for 24 hours at 80 ℃, filtering to obtain a blue solid, sequentially cleaning for 3 times by using ethanol and redistilled water, and vacuum-drying for 12 hours at 95 ℃ to obtain the ferric ferricyanide/graphene oxide composite material;
(3) synthesizing an iron oxide/graphene composite material: and putting the prepared ferric ferricyanide/graphene composite material into a muffle furnace, and calcining for 6 hours at 200-600 ℃ to obtain the ferric oxide/graphene composite material.
2. The method for preparing the iron oxide/graphene composite nanomaterial according to claim 1, wherein the ratio of polyvinylpyrrolidone to potassium ferricyanide to hydrochloric acid solution to graphene oxide is 3.8 g: 1 mmol: 50mL of: 0.1 g.
3. The use of the iron oxide/graphene composite nanomaterial as defined in any one of claims 1 to 2 in an electrode material of a supercapacitor.
4. The use according to claim 3, wherein the specific capacity of the iron oxide/graphene composite nanomaterial is 264F/g.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113295739A (en) * | 2021-04-19 | 2021-08-24 | 济南大学 | Based on hollow Fe2O3The dual-mode electrochemical aptamer sensor and the method for determining acetamiprid |
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Application publication date: 20200508 |