CN105977053A - Graphene/manganese dioxide composite material mixed-type electrode material with enhanced specific capacity and preparation method thereof - Google Patents
Graphene/manganese dioxide composite material mixed-type electrode material with enhanced specific capacity and preparation method thereof Download PDFInfo
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- CN105977053A CN105977053A CN201610213891.8A CN201610213891A CN105977053A CN 105977053 A CN105977053 A CN 105977053A CN 201610213891 A CN201610213891 A CN 201610213891A CN 105977053 A CN105977053 A CN 105977053A
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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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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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- 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
- H01G11/46—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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- 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 graphene/manganese dioxide composite material mixed-type electrode material with enhanced specific capacity, which is characterized by being prepared from the following raw materials in parts by weight: 60-63 parts of loofah, 37-40 parts of scaphium scaphigerum, an appropriate amount of distilled water, 39.5-40 parts of zinc chloride, 8-8.5 parts of lithium chloride, 14-16 parts of powdery graphite oxide, 18-20 parts of liquid nitrogen, 2-3 parts of nanometer titanium dioxide, 30-33 parts of potassium permanganate, 15-17 parts of absolute ethyl alcohol and 9-10 parts of polytetrafluoroethylene emulsion. Manganese dioxide is loaded on a home-made graphene sheet layer through a certain step and then combined with plant-based porous carbon, and the specific capacity and the conductivity of the material are improved under a synergistic effect. A supercapacitor manufactured by the electrode material has excellent energy density and power density.
Description
Technical field
The present invention relates to electrode material technical field, particularly relate to a kind of graphene/manganese dioxide composite material mixed type electrode material strengthening specific capacity and preparation method thereof.
Background technology
The transition of fossil energy is relied on and consumes and causes serious environmental problem and energy crisis by the mankind, and for realizing the development and utilization of the energy of sustainable development, new forms of energy and the research of novel energy device cause extensive concern.Ultracapacitor is class novel energy-storing device between traditional capacitor and battery, and compared with tradition energy storage device, it has higher energy density and power density, longer service life cycle, advantages of environment protection simultaneously.Along with the development of science and technology in recent years, ultracapacitor is gradually increased in the application trend of the aspects such as crane, fork truck, new-energy automobile, common electronic facility and factory's stand-by power supply.But, the electric conductivity of super capacitor material is poor, be related to ultracapacitor key property as the uneven problem common with electrolyte contacts face unstable properties etc. of Topical Dispersion.Electrode is to determine ultracapacitor performance most critical factor, therefore the research of electrode material always this field academia and the focus of industrial quarters.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of graphene/manganese dioxide composite material strengthens mixed type electrode material of specific capacity and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of graphene/manganese dioxide composite material strengthens the mixed type electrode material of specific capacity, is prepared by the raw materials in: Retinervus Luffae Fructus 60-63, Semen Sterculiae Lychnophorae 37-40, distilled water are appropriate, zinc chloride 39.5-40, lithium chloride 8-8.5, powdery graphite oxide 14-16, liquid nitrogen 18-20, nano titanium oxide 2-3, potassium permanganate 30-33, dehydrated alcohol 15-17, ptfe emulsion 9-10.
A kind of graphene/manganese dioxide composite material of the present invention strengthens the mixed type electrode material of specific capacity, following concrete grammar be prepared from:
(1) by Retinervus Luffae Fructus under being passed through nitrogen protection, being warming up to 800 DEG C with the heating rate of 5 DEG C/min, insulation carbonization naturally cooled to room temperature after 1 hour, pulverized, and crossed 200 mesh sieves stand-by;Remove shell after Semen Sterculiae Lychnophorae is soaked in the distilled water of 5 times amount expansion and obtain Semen Sterculiae Lychnophorae suspension with crust, above-mentioned 200 mesh powder are added thereto, after stirring, add zinc chloride, lithium chloride, be spray-dried after ultrasonic 2 hours, obtain mixed-powder;
(2) mixed-powder is put in horizontal pipe furnace; under the protection being passed through nitrogen; it is incubated 2 hours at a temperature of 1000 DEG C; after being cooled to room temperature, product is put in the distilled water of 2 times amount and filter after ultrasonic 1.5 hours; the filter cake obtained is put in vacuum drying oven and dry, obtain plant base porous carbon material;
(3) being placed in by powdery graphite oxide in the Muffle furnace of 900 DEG C in the crucible after preheating, powdery graphite oxide expands rapidly, and the graphite oxide after expanding is poured into rapidly in liquid nitrogen, stirs, obtains Graphene stand-by;Disperse graphene in the distilled water of 5 times amount, ultrasonic 2 hours, it is subsequently adding potassium permanganate, after stirring 60 minutes with the speed of 600 revs/min, it is slowly added dropwise dehydrated alcohol, after dripping complete follow-up continuous stirring 60 minutes, reactant sucking filtration is taken filter cake, wash to neutrality, obtain Graphene/manganese dioxide compound material at 100 DEG C in drying;
(4) ptfe emulsion will add the distilled water of 5 times amount, stir and add, after being completely dispersed uniformly, Graphene/manganese dioxide compound material that step (3) obtains, stir 30 minutes with the speed mechanical of 600 revs/min, obtain mixed material;
(5) the plant base porous carbon material that step (2) is obtained, mixed material and remaining residual components mix homogeneously that step (4) obtains are put in stirred tank, after stirring 1.5 hours with the speed of 1000 revs/min, material is transferred in rubber mill, the slurry obtaining 400 mesh is ground with the speed of 200 revs/min, then slurry is coated with on a current collector uniformly, it is vacuum dried 6 hours under conditions of temperature 110-120 DEG C, on desktop electric tablet machine, under the pressure of 10MPa, tabletting is carried out after taking-up, dry to constant weight at a temperature of 80 DEG C and get final product in being placed again into vacuum drying oven after cutting.
The invention have the advantage that the present invention uses the plant component such as Retinervus Luffae Fructus, Semen Sterculiae Lychnophorae as carbon source, resource natural reproducible, reduce the dependence to fossil energy, and utilize zinc chloride and lithium chloride salt-mixture as activator, not only solve and utilize the shortcoming of perishable reaction vessel in activation of potassium hydroxide technique, and the plant base porous carbon material prepared has the distribution of optimized pore structure and hole dimension, has good chemical property, technique is simple simultaneously, and feasibility is high.
The present invention is at homemade graphene sheet layer more compound with plant base porous charcoal by manganese dioxide load by certain reactions steps, under synergism, improves specific capacity and the electrical conductivity of material;Electrode material of the present invention has good energy density and power density after making ultracapacitor.
Detailed description of the invention
A kind of graphene/manganese dioxide composite material strengthens the mixed type electrode material of specific capacity, is made up of the raw material of following weight portion (kilogram): Retinervus Luffae Fructus 60, Semen Sterculiae Lychnophorae 37, distilled water are appropriate, zinc chloride 39.5, lithium chloride 8, powdery graphite oxide 14, liquid nitrogen 18, nano titanium oxide 2, potassium permanganate 30, dehydrated alcohol 15, ptfe emulsion 9.
A kind of graphene/manganese dioxide composite material of the present invention strengthens the mixed type electrode material of specific capacity, following concrete grammar be prepared from:
(1) by Retinervus Luffae Fructus under being passed through nitrogen protection, being warming up to 800 DEG C with the heating rate of 5 DEG C/min, insulation carbonization naturally cooled to room temperature after 1 hour, pulverized, and crossed 200 mesh sieves stand-by;Remove shell after Semen Sterculiae Lychnophorae is soaked in the distilled water of 5 times amount expansion and obtain Semen Sterculiae Lychnophorae suspension with crust, above-mentioned 200 mesh powder are added thereto, after stirring, add zinc chloride, lithium chloride, be spray-dried after ultrasonic 2 hours, obtain mixed-powder;
(2) mixed-powder is put in horizontal pipe furnace; under the protection being passed through nitrogen; it is incubated 2 hours at a temperature of 1000 DEG C; after being cooled to room temperature, product is put in the distilled water of 2 times amount and filter after ultrasonic 1.5 hours; the filter cake obtained is put in vacuum drying oven and dry, obtain plant base porous carbon material;
(3) being placed in by powdery graphite oxide in the Muffle furnace of 900 DEG C in the crucible after preheating, powdery graphite oxide expands rapidly, and the graphite oxide after expanding is poured into rapidly in liquid nitrogen, stirs, obtains Graphene stand-by;Disperse graphene in the distilled water of 5 times amount, ultrasonic 2 hours, it is subsequently adding potassium permanganate, after stirring 60 minutes with the speed of 600 revs/min, it is slowly added dropwise dehydrated alcohol, after dripping complete follow-up continuous stirring 60 minutes, reactant sucking filtration is taken filter cake, wash to neutrality, obtain Graphene/manganese dioxide compound material at 100 DEG C in drying;
(4) ptfe emulsion will add the distilled water of 5 times amount, stir and add, after being completely dispersed uniformly, Graphene/manganese dioxide compound material that step (3) obtains, stir 30 minutes with the speed mechanical of 600 revs/min, obtain mixed material;
(5) the plant base porous carbon material that step (2) is obtained, mixed material and remaining residual components mix homogeneously that step (4) obtains are put in stirred tank, after stirring 1.5 hours with the speed of 1000 revs/min, material is transferred in rubber mill, the slurry obtaining 400 mesh is ground with the speed of 200 revs/min, then slurry is coated with on a current collector uniformly, it is vacuum dried 6 hours under conditions of temperature 110 DEG C, on desktop electric tablet machine, under the pressure of 10MPa, tabletting is carried out after taking-up, dry to constant weight at a temperature of 80 DEG C and get final product in being placed again into vacuum drying oven after cutting.
In described embodiment, the electrode of preparation is as working electrode, metallic nickel is colelctor electrode, politef is barrier film, with 2mol/L potassium hydroxide as electrolyte, in the range of 1.2-2.5V, under constant current (5mA), it is circulated test, at room temperature determines that its capacity is 1.66F by charging and discharging curve, internal resistance is 1.53m Ω, and circulation volume conservation rate is 98.5%.
Claims (2)
1. the mixed type electrode material of a graphene/manganese dioxide composite material enhancing specific capacity, it is characterized in that, be prepared by the raw materials in: Retinervus Luffae Fructus 60-63, Semen Sterculiae Lychnophorae 37-40, distilled water are appropriate, zinc chloride 39.5-40, lithium chloride 8-8.5, powdery graphite oxide 14-16, liquid nitrogen 18-20, nano titanium oxide 2-3, potassium permanganate 30-33, dehydrated alcohol 15-17, ptfe emulsion 9-10.
2. strengthen the mixed type electrode material of specific capacity according to a kind of graphene/manganese dioxide composite material described in claims 1, it is characterised in that be prepared from by following concrete grammar:
(1) by Retinervus Luffae Fructus under being passed through nitrogen protection, being warming up to 800 DEG C with the heating rate of 5 DEG C/min, insulation carbonization naturally cooled to room temperature after 1 hour, pulverized, and crossed 200 mesh sieves stand-by;Remove shell after Semen Sterculiae Lychnophorae is soaked in the distilled water of 5 times amount expansion and obtain Semen Sterculiae Lychnophorae suspension with crust, above-mentioned 200 mesh powder are added thereto, after stirring, add zinc chloride, lithium chloride, be spray-dried after ultrasonic 2 hours, obtain mixed-powder;
(2) mixed-powder is put in horizontal pipe furnace; under the protection being passed through nitrogen; it is incubated 2 hours at a temperature of 1000 DEG C; after being cooled to room temperature, product is put in the distilled water of 2 times amount and filter after ultrasonic 1.5 hours; the filter cake obtained is put in vacuum drying oven and dry, obtain plant base porous carbon material;
(3) being placed in by powdery graphite oxide in the Muffle furnace of 900 DEG C in the crucible after preheating, powdery graphite oxide expands rapidly, and the graphite oxide after expanding is poured into rapidly in liquid nitrogen, stirs, obtains Graphene stand-by;Disperse graphene in the distilled water of 5 times amount, ultrasonic 2 hours, it is subsequently adding potassium permanganate, after stirring 60 minutes with the speed of 600 revs/min, it is slowly added dropwise dehydrated alcohol, after dripping complete follow-up continuous stirring 60 minutes, reactant sucking filtration is taken filter cake, wash to neutrality, obtain Graphene/manganese dioxide compound material at 100 DEG C in drying;
(4) ptfe emulsion will add the distilled water of 5 times amount, stir and add, after being completely dispersed uniformly, Graphene/manganese dioxide compound material that step (3) obtains, stir 30 minutes with the speed mechanical of 600 revs/min, obtain mixed material;
(5) the plant base porous carbon material that step (2) is obtained, mixed material and remaining residual components mix homogeneously that step (4) obtains are put in stirred tank, after stirring 1.5 hours with the speed of 1000 revs/min, material is transferred in rubber mill, the slurry obtaining 400 mesh is ground with the speed of 200 revs/min, then slurry is coated with on a current collector uniformly, it is vacuum dried 6 hours under conditions of temperature 110-120 DEG C, on desktop electric tablet machine, under the pressure of 10MPa, tabletting is carried out after taking-up, dry to constant weight at a temperature of 80 DEG C and get final product in being placed again into vacuum drying oven after cutting.
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Citations (3)
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CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
CN104362001A (en) * | 2014-11-28 | 2015-02-18 | 西北师范大学 | Method for preparing manganese dioxide/graphene/porous carbon (MnO2/rGO/C) composite material and application of MnO2/rGO/C composite material to supercapacitor as electrode material |
CN104882294A (en) * | 2015-04-03 | 2015-09-02 | 安徽江威精密制造有限公司 | Porous straw-based electrode material with high specific surface area and method of preparation |
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Patent Citations (3)
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CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
CN104362001A (en) * | 2014-11-28 | 2015-02-18 | 西北师范大学 | Method for preparing manganese dioxide/graphene/porous carbon (MnO2/rGO/C) composite material and application of MnO2/rGO/C composite material to supercapacitor as electrode material |
CN104882294A (en) * | 2015-04-03 | 2015-09-02 | 安徽江威精密制造有限公司 | Porous straw-based electrode material with high specific surface area and method of preparation |
Non-Patent Citations (1)
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Application publication date: 20160928 |