CN104409222A - Preparation method for ternary composites of graphene/manganese dioxide nanosheet /polyaniline nanorod - Google Patents
Preparation method for ternary composites of graphene/manganese dioxide nanosheet /polyaniline nanorod Download PDFInfo
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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
- H01G11/48—Conductive polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a preparation method for ternary composites of graphene /manganese dioxide nanosheet/polyaniline nanorod. The preparation method includes: drawing graphene oxide suspension liquid into graphene oxide papers using vacuum suction filter, and obtaining the graphene oxide papers under the reducing action of hydroiodic acid; obtaining manganese dioxide nanosheets on the graphene paper surface by a constant voltage deposition method; embedding the polyaniline nanorods between the manganese dioxide nanosheets by an in situ polymerization method to improve the electrical conductivity of the composite materials. The preparation method is simple and is easy to operate, and the material cost is low; in addition, the material has high specific capacitance and excellent electrochemical stability and excellent rate capability. Moreover, the final product is the self-support flexible material, and the graphene paper can act as a current collector and electrode material, and can also be assembled into the flexible components, and has the very good application prospect.
Description
Technical field
The invention belongs to new energy materials field, relate to a kind of preparation method of electrode material for super capacitor, be specifically related to a kind of preparation of Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material.
Background technology
Along with socioeconomic development, people more and more pay close attention to for green energy resource and biological environment.Ultracapacitor is as a kind of novel energy storage device, there is the features such as high power density, long circulation life and wide serviceability temperature scope, in its various quick high-power start system at electric power, green energy resource, aerospace field, unattended operation and Mobile energy system, backup power system etc., have extremely important using value.The particularly rise of environmental-protecting type electric automobile and electronic product, high-power and flexible super capacitor shows unprecedented application prospect.Therefore, ultracapacitor is fallen over each other research and production by increasing country and enterprise.Electrode material is the key factor affecting ultracapacitor performance.The electrode material of ultracapacitor mainly contains: the material with carbon element, transition metal oxide, conducting polymer etc. of high-specific surface area.
Material with carbon element utilizes the interfacial electric double layer formed between electrode and electrolyte to realize energy storage, this energy storage is carried out electrochemical polarization to realize by electrolyte solution, do not produce electrochemical reaction, therefore there is good cyclical stability and higher specific power density, and Graphene has unique two-dimensional sheet structure, there is the conductivity being better than other material with carbon elements, therefore can as the electrode material of ultracapacitor, but limit its application in practice due to low specific energy density.Manganese oxide resource is extensive, cheap, friendly to environment, has multiple oxidation state, stores electric charge, therefore have higher ratio capacitance, but its lower conductivity limits its practical application by valence transition.And conducting polymer utilizes redox reaction, doping state and going state of adulterating converts stored energy mutually, therefore not only all there is highdensity electric charge in interface but also in whole volume in conducting polymer, there is high specific energy density, but because it makes cyclical stability very poor in the redox reaction of energy storage process, this also counteracts that its application in practice.Therefore how the advantages of this three classes material to be got up, prepare high specific capacitance, excellent electrochemical stability and the composite material of outstanding multiplying power property, become study hotspot in recent years.
Can be known by analysis above, by three kinds of material couples to prepare the composite material of superior performance, so not only can utilize the electric double layer capacitance of carbon but also the Faraday pseudo-capacitance of manganese dioxide and polyaniline can have been utilized, the collaborative chemical property playing three, thus significantly improve the specific capacity of ultracapacitor, cyclical stability and high rate performance.
Summary of the invention
The object of the invention is the preparation method proposing a kind of Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material, to overcome the above-mentioned defect existing for prior art.
Design of the present invention is such:
Preparation has high-energy-density density and good circulation stability, and the electrode material of outstanding high rate performance is the key of ultracapacitor commercial applications.If the synergy of material with carbon element, transition metal oxide and conducting polymer can be given full play to, so the energy density of capacitor, cyclical stability and high rate performance will be significantly improved.The people such as Dai utilize the Graphene of hydro-thermal one-step synthesis method and the compound of manganese dioxide nanowire, at 0.2A g
-1under condition under can reach 176F g
-1wherein graphene base body improves the electric conductivity of composite material, and manganese dioxide nanowire serves the effect at interval between graphene layer, thus improve specific area and the porosity of material, and its fake capacitance part too increases the ratio capacitance of material simultaneously, thus improve the chemical property of material.The people such as Gui obtains graphene/polyaniline self-supporting flexible composite by the method for micro-emulsion polymerization and self assembly in addition, and this material ratio capacitance is at 0.5A g
-1condition under can reach 448F g
-1simultaneously due to the synergy of Graphene and polyaniline, the cyclical stability of compound is significantly improved, after carrying out 5000 charge and discharge cycles, still can keep the ratio capacitance of 81%, show it is a developing direction of electrode material for super capacitor by the conducting polymers such as polyaniline and Graphene compound.
But up to the present, research about Graphene-manganese dioxide-polyaniline ternary system is still less, Graphene-polyaniline-manganese dioxide the ternary complex that had the researchers such as Han by two step synthesis recently, first one deck polyaniline is deposited by the method for in situ chemical oxidative polymerization at graphenic surface, enhance the capacitive property of Graphene, then obtain trielement composite material at polyaniline surface self-organization one deck manganese dioxide, its ratio capacitance can reach 512F g
-1, and after 5000 circulations, its specific capacity still can keep 97%.But the preparation and application report tied up in flexible electrode material about Graphene-manganese dioxide-polyaniline ternary complex is less.The present invention utilizes two step experimental methods at graphene paper superficial growth manganese dioxide nano-plates and polyaniline nano-line exactly, forms ternary nano composite material, and it can be used as ultracapacitor self-supporting flexible electrode material.The ratio capacitance of this material is obtained at 1A g by electrochemical property test
-1636F g can be reached under condition
-1, after charge and discharge process repetitive cycling 5000 times, ratio capacitance still can keep more than 90%, at 50A g
-1still have the ratio capacitance conservation rate of 50% under current density, there is good high rate performance.
The present invention is achieved by the following technical solutions:
A preparation method for Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material, comprises the steps:
(1) Hummer method (the reference W.Lv. first by improving, et.al, ACS Nano, 2009,3,3730) prepare graphene oxide, be configured to suspension 50 ~ 100ml that concentration is the graphene oxide of 0.5 ~ 1mg/ml after drying, utilize the method for vacuum filtration to obtain graphene oxide paper by sand core funnel;
(2) it is in the hydroiodic acid of 40 ~ 45% that graphene oxide paper step (1) obtained immerses mass fraction, reduction 3 ~ 6h at 70 ~ 90 DEG C, and after cleaning with deionized water and ethanol, vacuumize 2 ~ 4h obtains graphene paper.
(3) compound concentration is the four water acetic acid manganese solutions of 0.1 ~ 0.5M, then prepares the metabisulfite solution of 0.1 ~ 0.5M, and both are to stir after the mixing of the volume ratio of 1:1; Graphene paper leaching step (2) prepared in this solution, under the condition of 0.5 ~ 1V constant voltage, deposit 200 ~ 900s (controlling thickness and the quality of the manganese dioxide nano-plates layer of graphenic surface deposition) with Autolab electrochemical workstation by three-electrode system and obtain manganese dioxide nano-plates, clean by washed with de-ionized water, vacuumize 5 ~ 10h; Described three-electrode system is that Ag/AgCl is as reference electrode, and graphene paper is as work electrode using platinized platinum as to electrode;
(4) aniline monomer (wanting decompression distillation before use) measuring 1.0 ~ 1.5ml is poured in the deionized water of 60 ~ 80ml, and adds 1.5 ~ 2.3g camphorsulfonic acid simultaneously, stirs 1 ~ 3min rapidly; The ammonium persulfate taking 3.0 ~ 3.5g is dissolved in the deionized water of 30 ~ 40ml, stir 1 ~ 2min, dissolve completely, two kinds of solution are with aniline solution: ammonium perchlorate's liquor capacity mixes rapidly than the volume ratio for 2:1, after stirring 1 ~ 2min, immerse the product that step (3) obtains, leave standstill 2 ~ 5h, namely obtain described Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material.
The thickness of the graphene paper that step (1) obtains is 6 ~ 15 μm, the accumulation that its graphene layer is orderly, and conductivity is 80 ~ 100S/cm.
In step (1) process, the thickness of graphene paper is controlled by the concentration (0.5 ~ 1mg/ml) of suspension and volume (50 ~ 100ml).
In step (4) process, the mol ratio of ammonium persulfate and aniline is 1:0.5 ~ 2.
In Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material that step (4) prepares, the thickness of graphene paper is 10 ~ 20 μm, manganese dioxide nano-plates thickness is 50 ~ 100nm, and polyaniline nano-rod length is 60 ~ 100nm.
Described Graphene/manganese dioxide/polyaniline trielement composite material can be used as the electrode material of ultracapacitor, in 1M sodium sulphate electrolyte, have height ratio capacity, energy density, power density and electrochemical stability and high rate performance.
Positive beneficial effect of the present invention: utilize the method for vacuum filtration that graphene oxide suspension suction filtration is obtained graphene oxide paper, graphene paper is obtained under the reduction of hydroiodic acid, then the method deposited by constant voltage on graphene paper surface obtains one deck manganese dioxide nano-plates, finally between manganese dioxide nano-plates, embed by the method for in-situ chemical polymerization the conductivity that polyaniline nano-rod improves composite material, finally obtain the composite material of Graphene/manganese dioxide nano-plates/polyaniline nano-rod.The composite material utilizing this serial of methods to prepare can play the synergy of Graphene, transition metal oxide and conducting polymer, makes it have excellent chemical property, comprises high specific capacitance, excellent electrochemical stability and multiplying power property.By the morphosis regulating the sedimentation time of manganese dioxide and the polymerization time of aniline can control composite material, thus affect its chemical property.Preparation method is simple; Lower cost for material; This material has the advantage of high specific capacitance, excellent electrochemical stability and outstanding multiplying power property in addition; And final resulting materials is self-supporting flexible material, graphene paper not only serves as collector but also as electrode material, can assemble and obtain flexible device, has good application prospect
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of embodiment 1 product;
Fig. 2 is the electromicroscopic photograph of embodiment 2 product;
Fig. 3 is that two kinds of compounds prepared by example 2,3 carry out the infrared spectrum that infrared detection obtains;
Fig. 5 be example 1,2 prepare two kinds of compounds and graphene paper with the metabisulfite solution of 1M for electrolyte is at 5mV s
-1cyclic voltammetry curve under condition;
Fig. 4 be example 1,2 prepare two kinds of compounds and graphene paper with the metabisulfite solution of 1M at 1A.g
-1current density under charging and discharging curve.
Embodiment by reference to the accompanying drawings, is further described invention.
Embodiment 1
The four water acetic acid manganese solutions of the 0.1M of preparation and the metabisulfite solution of 0.1M are mixed with the volume ratio of 1:1, then self-control graphene paper is immersed in mixed solution, under the constant-pressure conditions of 0.8V, electro-deposition 300s is carried out with Autolab electrochemical operation, then clean by washed with de-ionized water, vacuumize 6h.
Embodiment 2
Measuring 1.2ml aniline monomer (wanting decompression distillation before use) moves in 75ml deionized water, stir 1min, weigh the deionized water that 3.4g ammonium persulfate solid adds 37.5ml, stir 1min, then above-mentioned two kinds of solution are mixed, stir 1min, the Graphene of preparation in embodiment 1/manganese dioxide binary composite is immersed in mixed liquor, polyase 13 h under static conditions.
Embodiment 3
As the control group of embodiment 2, measuring 1.2ml aniline monomer (wanting decompression distillation before use) moves in 75ml deionized water, stir 1min, weigh the deionized water that 3.4g ammonium persulfate solid adds 37.5ml, stir 1min, then above-mentioned two kinds of solution are mixed, stir 1min, simple graphene paper is immersed in mixed liquor, polyase 13 h under same static conditions.
Embodiment 4
Graphene/manganese dioxide nano-plates/polyaniline nano-rod the ternary complex of field emission microscope (HITACHI S4800) to preparation in above-described embodiment 2 is used to carry out morphology characterization respectively, result is as Fig. 1 and Fig. 2, then utilize the sample of FTIS to example 2 and example 3 to carry out infrared detection, result is as Fig. 3.
Embodiment 5
Graphene prepared by embodiment 1/manganese dioxide nano-plates composite material, Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material prepared by embodiment 2, and graphene paper is under three-electrode system, with Ag/AgCl electrode for reference electrode, be to electrode with platinum electrode, do electrolyte with 1M metabisulfite solution, Autolab electrochemical workstation carries out cyclic voltammetry, test voltage interval is-0.1 ~ 0.9V, compares at 5mV s
-1the cyclic voltammetry curve of lower embodiment 1,2 and graphene paper, as Fig. 4; Continue to preparation embodiment 1,2 and graphene paper on Autolab work station at 1A g
-1test its charge-discharge performance under current density, result is as Fig. 5.Can calculate the ratio capacitance value of embodiment 1,2 electrode material under different current densities of preparation according to charging and discharging curve, result is as table 1.
The specific capacity of C-active material in formula, F g
-1
The current value of I-constant, A
T-discharge time, s
The quality of active material on m-electrode slice, g
Δ V-discharge voltage is interval, V
Specific capacity (the F g of the embodiment 1,2 utilizing this formula to be calculated by Fig. 4 under different current density
-1) as shown in table 1.
Table 1
Claims (5)
1. a preparation method for Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material, is characterized in that, comprise the steps:
(1) the Hummer legal system first passing through to improve, for graphene oxide, is configured to suspension 50 ~ 100ml that concentration is the graphene oxide of 0.5 ~ 1mg/ml, utilizes the method for vacuum filtration to obtain graphene oxide paper by sand core funnel after drying;
(2) it is in the hydroiodic acid of 40% ~ 45% that graphene oxide paper step (1) obtained immerses mass fraction, reduction 3 ~ 6h at 70 ~ 90 DEG C, and after cleaning with deionized water and ethanol, vacuumize 2 ~ 4h obtains graphene paper;
(3) compound concentration is the four water acetic acid manganese solutions of 0.1 ~ 0.5M, then prepares the metabisulfite solution of 0.1 ~ 0.5M, and both are to stir after the mixing of the volume ratio of 1:1; The graphene paper obtained in step (2) is soaked in this solution, under the condition of 0.5 ~ 1V constant voltage, deposit 200 ~ 900s with Autolab electrochemical workstation by three-electrode system and obtain manganese dioxide nano-plates, clean by washed with de-ionized water, vacuumize 5 ~ 10h; Described three-electrode system is that Ag/AgCl is as reference electrode, and graphene paper is as work electrode using platinized platinum as to electrode;
(4) aniline monomer measuring 1.0 ~ 1.5ml is poured in the deionized water of 60 ~ 80ml, and adds 1.5 ~ 2.3g camphorsulfonic acid simultaneously, stirs 1 ~ 3min rapidly; The ammonium persulfate taking 3.0 ~ 3.5g is dissolved in the deionized water of 30 ~ 40ml, stir 0.5 ~ 2min, dissolve completely, aniline solution and ammonium persulfate solution are mixed rapidly with the volume ratio of 2:1, after stirring 0.5 ~ 2min, immerse the product that step (3) obtains, leave standstill 2 ~ 5h, namely obtain described Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material.
2. preparation method according to claim 1, is characterized in that, the thickness of the graphene paper that step (1) obtains is 6 ~ 15 μm, and its graphene layer is piled up in an orderly manner, and conductivity is 80 ~ 100S/cm.
3. preparation method according to claim 1, is characterized in that, the mol ratio of described ammonium persulfate and aniline is 1:0.5 ~ 2.
4. preparation method according to claim 1, it is characterized in that, in described Graphene/manganese dioxide nano-plates/polyaniline nano-rod trielement composite material, the thickness of graphene paper is 10 ~ 20 μm, manganese dioxide nano-plates thickness is 50 ~ 100nm, and polyaniline nano-rod length is 60 ~ 100nm.
5. preparation method according to claim 1, is characterized in that, described Graphene/manganese dioxide nano-plates/polyaniline nano-rod ternary complex is applied to ultracapacitor as electrode material.
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Cited By (14)
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|---|---|---|---|---|
| CN105070514A (en) * | 2015-07-06 | 2015-11-18 | 常州大学 | Preparing polyaniline/graphene/manganese dioxide composite material through interface method and applying polyaniline/graphene/manganese dioxide composite material to super capacitor |
| CN105405671A (en) * | 2015-11-27 | 2016-03-16 | 南京师范大学 | Oxidized graphene/pure graphene/polyaniline ternary conductive composite material and preparation method thereof |
| CN106024427A (en) * | 2016-07-29 | 2016-10-12 | 上海交通大学 | Polyaniline nanotube modified ultrathin graphene membrane electrode and preparation method thereof |
| CN106128802A (en) * | 2016-07-04 | 2016-11-16 | 上海电力学院 | A kind of preparation method of the electrode material for ultracapacitor |
| CN106298286A (en) * | 2016-10-15 | 2017-01-04 | 成都育芽科技有限公司 | The preparation method of Graphene/manganese dioxide/polyaniline nano-rod array and application |
| CN106449131A (en) * | 2016-12-09 | 2017-02-22 | 天津大学 | Graphene-covered flower-like nickel hydroxide composite electrode material and preparation method thereof |
| CN106449148A (en) * | 2016-11-22 | 2017-02-22 | 中国地质大学（北京） | Method for preparing tubular manganese dioxide / poly-aniline / graphene composite material |
| CN106653393A (en) * | 2016-12-26 | 2017-05-10 | 合肥工业大学 | Graphite oxide/polyaniline/hollow tubular manganese dioxide composite material and synthesis method thereof |
| CN107253716A (en) * | 2017-06-14 | 2017-10-17 | 青岛大学 | A kind of preparation method of graphene paper |
| CN108845007A (en) * | 2018-04-25 | 2018-11-20 | 上海第二工业大学 | A kind of platinum/graphen paper nanometer combined electrode material and preparation method thereof for detecting hydrogen peroxide |
| CN110350152A (en) * | 2018-04-02 | 2019-10-18 | 中国科学院化学研究所 | Graphite alkene/manganese dioxide nano-plates array material and its preparation method and application |
| CN110797214A (en) * | 2019-09-16 | 2020-02-14 | 中车青岛四方机车车辆股份有限公司 | Co-assembly preparation of MnO2Method for preparing/graphene composite material and application thereof |
| CN111416096A (en) * | 2020-03-24 | 2020-07-14 | 中南大学 | Graphene oxide/polyaniline/manganese dioxide composite electrode, preparation method thereof and application thereof in seawater battery |
| CN113786846A (en) * | 2021-09-30 | 2021-12-14 | 上海电力大学 | Tungsten disulfide/manganese dioxide micromotor and preparation and application thereof |
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