CN107301921A - A kind of preparation method of three-dimensional Activated Graphite alkene nanometer sheet - Google Patents
A kind of preparation method of three-dimensional Activated Graphite alkene nanometer sheet Download PDFInfo
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- CN107301921A CN107301921A CN201710453837.5A CN201710453837A CN107301921A CN 107301921 A CN107301921 A CN 107301921A CN 201710453837 A CN201710453837 A CN 201710453837A CN 107301921 A CN107301921 A CN 107301921A
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- -1 Activated Graphite alkene Chemical class 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 82
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 13
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 10
- 239000012190 activator Substances 0.000 claims abstract description 6
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 6
- 229920005862 polyol Polymers 0.000 claims abstract description 6
- 150000003077 polyols Chemical class 0.000 claims abstract description 6
- 238000002203 pretreatment Methods 0.000 claims abstract description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 229910002804 graphite Inorganic materials 0.000 claims description 30
- 239000010439 graphite Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 230000001186 cumulative effect Effects 0.000 claims description 17
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 16
- 239000000194 fatty acid Substances 0.000 claims description 16
- 229930195729 fatty acid Natural products 0.000 claims description 16
- 239000003610 charcoal Substances 0.000 claims description 15
- 239000012895 dilution Substances 0.000 claims description 15
- 238000010790 dilution Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 239000000428 dust Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 12
- 239000004575 stone Substances 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 229910000000 metal hydroxide Inorganic materials 0.000 claims 1
- 150000004692 metal hydroxides Chemical class 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 37
- 229910021389 graphene Inorganic materials 0.000 abstract description 24
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 description 18
- 238000000034 method Methods 0.000 description 16
- 238000001914 filtration Methods 0.000 description 13
- 150000001336 alkenes Chemical group 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 150000004679 hydroxides Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
-
- 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
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a kind of preparation method of three-dimensional Activated Graphite alkene nanometer sheet.The preparation method includes the selection and pre-treatment of S1. carbon sources；S2. the selection of activator, three-dimensional structure template and catalyst precursor；S3. presoma mixed processing；S4. heat treatment is covered；S5. product is post-processed.The present invention, as the carbon source of graphene nanometer sheet, largely reduces the preparation cost of material using widely used polyol-based non-ionic surfactant；Using cheap alkali metal hydroxide simultaneously as activator, three-dimensional structure template and catalyst precursor, it radically simplify synthesis step and reduce the preparation cost of material；It using heat treatment technics is covered, can implement in common Muffle furnace, be adapted to large-scale production.Preparation technology of the present invention is simple, it is easy to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of graphene nanometer sheet in energy storage material and application, more particularly to a kind of three-dimensional
The preparation method and applications of Activated Graphite alkene nanometer sheet.
Background technology
Lithium ion battery and ultracapacitor are two kinds of important class of electrochemical energy accumulating device.The former passes through electrification
Reaction storage energy is learned, higher energy density can be shown；And the latter can be provided by electric double layer process storage energy
Higher power density.Ultracapacitor also has the advantages that non-maintaining, long lifespan, has been widely used in many portable electrics
Sub- equipment.It is always long-term main struggle mesh developing high energy ultracapacitor used for electric vehicle, specific capacitance high electrode material
Mark.Activated carbon is a kind of most common ultracapacitor（Double layer capacitor）Electrode material, with loose structure, low price and
The advantages of can be mass.However, the specific surface area of conventional carbon is small, electrical conductivity is low, and chemical stability is not enough, prevent its from
Meet the newest stored energy application requirement of long period, high reliability and high-energy-density.
Two-dimensional graphene material turns into the electrochemical energy storage electrode material of a new generation by excellent physicochemical characteristics.
The surface-active site of height exposure and graphene, class graphene（Such as ultra-thin carbon nanosheet）Unique electronic structure, can be lithium
Ion battery and ultracapacitor provide high power capacity.Three-dimensional grapheme structure（Three be connected with each other by graphene nanometer sheet
Tie up structure）, tempting application prospect is shown in sustainable energy storage with its unique structure and form.Novel three-dimensional stone
Black alkene structure has two advantages in electro-chemical systems：（i）The network structure of connected graphene nanometer sheet can prevent stone
Black alkene nanometer sheet aggregation,（ii）The macroporous structure of interconnection is that electron transmission and ion diffusion provide favourable channel.Therefore, it is three-dimensional
Graphene-structured can significantly improve the specific capacitance of ultracapacitor.
In view of the excellent performance of three-dimensional grapheme material and wide prospect, explore the efficient of synthesis three-dimensional grapheme material
Synthetic method, with important scientific meaning and practical value.Currently, the preparation method of three-dimensional grapheme material mainly has two
Kind：（1）The three-dimensional grapheme knot that is mutually related is obtained by hydrothermal reduction and self assembling process by presoma of graphene oxide
Structure；（2）Using nickel foam as three-dimensional template and catalytic substrate the three of self-supporting is obtained by chemical vapor deposition and removing template process
Tie up graphene-structured.Obviously, above-mentioned multistep preparation process is cumbersome and power consumption is higher, is difficult to realize three-dimensional grapheme material
Mass production.Particularly, device therefor is complicated and expensive, and the exploitation to subsequent material brings great difficulty
Topic.In consideration of it, a kind of cheap, simple preparation method of exploitation is heavy to closing to promoting the industrialization of three-dimensional grapheme material to play
The effect wanted.
The content of the invention
The purpose of the present invention be overcome the shortcomings of prior art exist there is provided a kind of system of three-dimensional Activated Graphite alkene nanometer sheet
Preparation Method, solving the step of current three-dimensional Activated Graphite alkene nanometer piece preparation method faces, complicated, equipment is expensive, it is numerous to operate
The problems such as trivial, difficult batch production.
The above-mentioned purpose of the present invention is achieved by the following technical programs：
A kind of preparation method of three-dimensional Activated Graphite alkene nanometer sheet, comprises the following steps：
S1. the selection and pre-treatment of carbon source：Selection polyol-based non-ionic surfactant is carbon source, and is dissolved with solvent
And dilution；
S2. the selection of activator, three-dimensional structure template and catalyst precursor：Select alkali metal hydroxide simultaneously as activation
Agent, three-dimensional structure template and catalyst precursor；
S3. presoma mixed processing：By the nonionic surfactant and step S2 alkali metal hydrogen-oxygen after step S1 pre-treatments
Compound carries out high-speed stirred mixing and vacuum drying；
S4. heat treatment is covered：Mixture obtained by step S3 is positioned in graphite crucible, above adjustment sample volume and sample
Volume of air, close the lid, with charcoal carbon dust bury be heat-treated；
S5. product is post-processed：Product after step S4 is heat-treated is collected, removal of impurities, washing, filtered, be drying to obtain three-dimensional
Activated Graphite alkene nanometer sheet.
The carbon source of the invention that widely used polyol-based non-ionic surfactant is used as graphene nanometer sheet, very
The preparation cost of material is reduced in big degree；Activator is used as using cheap alkali metal hydroxide simultaneously（Alkali metal hydrogen
The chemical activation of oxide can improve material specific surface area）, three-dimensional structure template（Alkali metal hydroxide is in pyroprocess
The percarbonate particle of generation can be used as three-dimensional structure template）And catalyst（Alkali metal hydroxide is generated after air oxidation
Alkali metal oxide can be used as graphited catalyst）Presoma, radically simplify synthesis step and reduces material
The preparation cost of material；It using heat treatment technics is covered, can implement in common Muffle furnace, be adapted to large-scale production.
Preferably, polyol-based non-ionic surfactant described in S1 is sorbitan fatty acid ester, polyoxyethylene mistake
One or both of water Span.
Solvent for use is dissolved and diluted described in S1 includes the one or more in distilled water, ethanol, acetone.
Preferably, alkali metal hydroxide described in step S2 be sodium hydroxide, potassium hydroxide, lithium hydroxide in one kind or
Two or more mixing.
Preferably, the mass ratio of nonionic surfactant and alkali metal hydroxide described in step S3 is 1：0.5~3.0.
Preferably, the temperature being heat-treated described in step S4 is 600 ~ 900 DEG C, and the heat time is 30 min ~ 120min, heating
Speed is 1 ~ 10 DEG C/min.
Preferably, sample volume is the air body above the 20% of crucible cumulative volume, sample in graphite crucible described in step S4
Product is the 20% ~ 80% of crucible cumulative volume.
Preferably, removal of impurities described in step S5 refers to utilize salt acid soak products therefrom, the concentration of hydrochloric acid used for 0.5 ~
2mol/L, soak time is 0.5 ~ 2h.
Compared with prior art, the present invention has the advantages that：
（1）The present invention, as the carbon source of graphene nanometer sheet, is largely dropped using polyol-based non-ionic surfactant
The low preparation cost of material.
（2）The present invention is used as activator simultaneously using cheap alkali metal hydroxide（The chemistry of alkali metal hydroxide
Activation can improve material specific surface area）, three-dimensional structure template（The carbonate that alkali metal hydroxide is generated in pyroprocess
Particulate can be used as three-dimensional structure template）And catalyst（The alkali metal oxidation that alkali metal hydroxide is generated after air oxidation
Thing can be used as graphited catalyst）Presoma, radically simplify synthesis step and reduces the preparation cost of material.
（3）What the present invention was used, which cover heat treatment technics, belongs to non-inert gas heat treatment technics, in common Muffle furnace
It can implement, be adapted to extensive preparation, solve the complicated, equipment of the step of current three-dimensional Activated Graphite alkene nanometer sheet faces and hold high
It is expensive, cumbersome, the problems such as hardly possible is produced in batches.
Brief description of the drawings
Fig. 1 is the schematic diagram that the present invention prepares three-dimensional Activated Graphite alkene nanometer sheet device therefor device：1 Muffle furnace, 2 wood
Charcoal carbon dust, 3 graphite crucibles, 4 air, 5 samples.
Fig. 2 is the X ray diffracting spectrum of three-dimensional Activated Graphite alkene nanometer sheet prepared by embodiment 1.
Fig. 3 is the scanning electron microscope diagram piece of three-dimensional Activated Graphite alkene nanometer sheet prepared by embodiment 1.
Fig. 4 is that the cyclic voltammetric of three-dimensional Activated Graphite alkene nanometer sheet electrode material for super capacitor prepared by embodiment 1 is bent
Line, sweep speed is 50,100,200,500,1000 mV/s.
Fig. 5 is the constant current charge-discharge of three-dimensional Activated Graphite alkene nanometer sheet electrode material for super capacitor prepared by embodiment 1
Curve, current density be 1,2,3,4,5A/g.
Embodiment
The present invention is further expalined explanation with reference to specific embodiments and the drawings, it describes more specific and detailed
Carefully, but can not therefore and be interpreted as the limitation to the scope of the claims of the present invention, as long as using equivalent substitution or the shape of equivalent transformation
The technical scheme that formula is obtained, all should be included within the protection domain of the claims in the present invention.
Embodiment 1
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 800 DEG C, and the heat time is 60min, and programming rate is 5 DEG C/min.Finally by the catalysate of gained
It is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional activity stone is made with distilling water washing, filtering, drying
Black alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 800nm, and thickness is about
20nm, material specific surface area is 2360 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 205 F g-1.Fig. 2 is the X-ray diffracting spectrum of material prepared by embodiment 1.Fig. 3 is material prepared by embodiment 1
Scanning electron microscope image.Fig. 4 is the cyclic voltammetry curve of material prepared by embodiment 1.Fig. 5 is prepared by embodiment 1
The constant current charge-discharge curve of material.
Embodiment 2
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 100g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 800 DEG C, and the heat time is 60min, and programming rate is 5 DEG C/min.Finally by the catalysate of gained
It is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional activity stone is made with distilling water washing, filtering, drying
Black alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 600nm, and thickness is about
30nm, material specific surface area is 1870 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 169 F g-1。
Embodiment 3
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 300g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 800 DEG C, and the heat time is 60min, and programming rate is 5 DEG C/min.Finally by the catalysate of gained
It is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional activity stone is made with distilling water washing, filtering, drying
Black alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 500nm, and thickness is about
25nm, material specific surface area is 2250 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 194 F g-1。
Embodiment 4
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 20% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 800 DEG C, and the heat time is 60min, and programming rate is 5 DEG C/min.Finally by the catalysate of gained
It is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional activity stone is made with distilling water washing, filtering, drying
Black alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 500nm, and thickness is about
40nm, material specific surface area is 2420 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 202 F g-1。
Embodiment 5
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 80% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 800 DEG C, and the heat time is 60min, and programming rate is 5 DEG C/min.Finally by the catalysate of gained
It is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional activity stone is made with distilling water washing, filtering, drying
Black alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 900nm, and thickness is about
15nm, material specific surface area is 1990 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 184 F g-1。
Embodiment 6
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 600 DEG C, and the heat time is 60min, and programming rate is 5 DEG C/min.Finally by the catalysate of gained
It is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional activity stone is made with distilling water washing, filtering, drying
Black alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 700nm, and thickness is about
30nm, material specific surface area is 1910 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 186 F g-1。
Embodiment 7
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 900 DEG C, and the heat time is 60min, and programming rate is 5 DEG C/min.Finally by the catalysate of gained
It is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional activity stone is made with distilling water washing, filtering, drying
Black alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 600nm, and thickness is about
30nm, material specific surface area is 2060 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 189 F g-1。
Embodiment 8
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
Upper air volume is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and is heat-treated,
The temperature of heat treatment is 800 DEG C, and the heat time is 30min, and programming rate is 5 DEG C/min.Finally the catalysate of gained is entered
Row is collected, and is 1h with 1mol/L hydrochloric acid soak times, then three-dimensional Activated Graphite is made with distilling water washing, filtering, drying
Alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 800nm, and thickness is about
20nm, material specific surface area is 2160 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 201 F g-1。
Embodiment 9
100g sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g potassium hydroxide is added, enters
Row high-speed stirred is mixed and is dried in vacuo.The mixture of gained is positioned over the adjustable graphite crucible of a volume, sample after charging
The volume of air of top is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace and carries out hot place
Reason, the temperature of heat treatment is 800 DEG C, and the heat time is 120min, and programming rate is 5 DEG C/min.Finally the catalysis of gained is produced
Thing is collected, and is 1h with 1mol/L hydrochloric acid soak times, then is made three-dimensional active with distilling water washing, filtering, drying
Graphene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 700nm, and thickness is about
20nm, material specific surface area is 2190 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 198 F g-1。
Embodiment 10
100g polyoxyethylene sorbitan fatty acid esters are dissolved with 500ml distilled water and dilution is handled, 200g hydrogen is added
Potassium oxide, carries out high-speed stirred mixing and vacuum drying.The mixture of gained is positioned over the adjustable graphite crucible of a volume, filled
Volume of air after material above sample is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace
It is heat-treated, the temperature of heat treatment is 800 DEG C, the heat time is 60min, programming rate is 5 DEG C/min.Finally by gained
Catalysate is collected, and is 1h with 1mol/L hydrochloric acid soak times, then is made three with distilling water washing, filtering, drying
Tie up Activated Graphite alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet prepared by the above method, wherein graphene width is about 900nm, and thickness is about
10nm, material specific surface area is 2490 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Compare under current density
Capacity is 224 F g-1。
Embodiment 11
100g polyoxyethylene sorbitan fatty acid esters are dissolved with 500ml ethanol and dilution is handled, 50g hydroxides are added
Sodium, carries out high-speed stirred mixing and vacuum drying.The mixture of gained is positioned over the adjustable graphite crucible of a volume, after charging
Volume of air above sample is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace progress
Heat treatment, the temperature of heat treatment is 600 DEG C, and the heat time is 100min, and programming rate is 1 DEG C/min.Last urging gained
Change product to be collected, and be 2h with 0.5mol/L hydrochloric acid soak times, then three are made with distilling water washing, filtering, drying
Tie up Activated Graphite alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet material prepared by the above method, wherein graphene width is about 2000nm, thick
Degree is about 200nm, and material specific surface area is 795m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Electric current is close
The lower specific capacity of degree is 86F g-1。
Embodiment 12
100g polyoxyethylene sorbitan fatty acid esters are handled with 500ml acetone solutions and dilution, 50g hydroxides are added
Lithium, carries out high-speed stirred mixing and vacuum drying.The mixture of gained is positioned over the adjustable graphite crucible of a volume, after charging
Volume of air above sample is the 50% of cumulative volume, covers graphite lid, is buried with charcoal carbon dust, is positioned over Muffle furnace progress
Heat treatment, the temperature of heat treatment is 900 DEG C, and the heat time is 60min, and programming rate is 10 DEG C/min.Last urging gained
Change product to be collected, and be 0.5h with 2mol/L hydrochloric acid soak times, then three are made with distilling water washing, filtering, drying
Tie up Activated Graphite alkene nanometer sheet.
The three-dimensional Activated Graphite alkene nanometer sheet material prepared by the above method, wherein graphene width is about 3000 nm, thick
Degree is about 250 nm, and material specific surface area is 887 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Electric current
Specific capacity is 82F g under density-1。
Comparative example 1
100g polyoxyethylene sorbitan fatty acid esters are handled with 500ml acetone solutions and dilution, 50g hydroxides are added
Lithium, carries out high-speed stirred mixing and vacuum drying.The mixture of gained is positioned over the adjustable graphite crucible of a volume, after charging
Volume of air above sample is the 50% of cumulative volume, covers graphite lid, is positioned over Muffle furnace and is heat-treated, heat treatment
Temperature is 900 DEG C, and the heat time is 60min, and programming rate is 10 DEG C/min.Finally the catalysate of gained is collected,
And be 0.5h with 2mol/L hydrochloric acid soak times, then three-dimensional Activated Graphite alkene nanometer is made with distilling water washing, filtering, drying
Piece.
The three-dimensional Activated Graphite alkene nanometer sheet material prepared by the above method, wherein graphene width is about 5000 nm, thick
Degree is about 2000 nm, and material specific surface area is 150 m2 g-1；Applied to the electrode material of ultracapacitor, in 1 A g-1Electric current
Specific capacity is 17 F g under density-1。
Claims (8)
1. a kind of preparation method of three-dimensional Activated Graphite alkene nanometer sheet, it is characterised in that comprise the following steps：
S1. the selection and pre-treatment of carbon source：Selection polyol-based non-ionic surfactant is carbon source, and is dissolved with solvent
And dilution；
S2. the selection of activator, three-dimensional structure template and catalyst precursor：Select alkali metal hydroxide simultaneously as activation
Agent, three-dimensional structure template and catalyst precursor；
S3. presoma mixed processing：By the nonionic surfactant and step S2 alkali metal hydrogen-oxygen after step S1 pre-treatments
Compound is mixed and is dried in vacuo；
S4. heat treatment is covered：Mixture obtained by step S3 is positioned in graphite crucible, above adjustment sample volume and sample
Volume of air, close the lid, with charcoal carbon dust bury be heat-treated；
S5. product is post-processed：Product after step S4 is heat-treated is collected, removal of impurities, washing, filtered, be drying to obtain three-dimensional
Activated Graphite alkene nanometer sheet.
2. the preparation method of three-dimensional Activated Graphite alkene nanometer sheet according to claim 1, it is characterised in that many described in step S1
First alcohol type nonionic surfactant is one kind in sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester
Or two kinds.
3. the preparation method of three-dimensional Activated Graphite alkene nanometer sheet according to claim 1, it is characterised in that dilute described in step S1
It is the one or more in distilled water, ethanol, acetone to release solvent.
4. the preparation method of three-dimensional Activated Graphite alkene nanometer sheet according to claim 1, it is characterised in that alkali described in step S2
Metal hydroxides is that one or both of sodium hydroxide, potassium hydroxide, lithium hydroxide are mixed above.
5. the preparation method of three-dimensional Activated Graphite alkene nanometer sheet according to claim 1, it is characterised in that non-described in step S3
The mass ratio of ionic surface active agent and alkali metal hydroxide is 1：0.5~3.0.
6. the preparation method of three-dimensional Activated Graphite alkene nanometer sheet according to claim 1, it is characterised in that hot described in step S4
The temperature of processing is 600 ~ 900 DEG C, and the heat time is 30 min ~ 120min, and programming rate is 1 ~ 10 DEG C/min.
7. the preparation method of three-dimensional Activated Graphite alkene nanometer sheet according to claim 1, it is characterised in that stone described in step S4
Sample volume is that the volume of air above the 20% of crucible cumulative volume, sample is the 20% ~ 80% of crucible cumulative volume in black crucible.
8. the preparation method of three-dimensional Activated Graphite alkene nanometer sheet according to claim 1, it is characterised in that removed described in step S5
Miscellaneous to refer to utilize salt acid soak products therefrom, the concentration of hydrochloric acid used is 0.5 ~ 2mol/L, and soak time is 0.5 ~ 2h.
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| EP2687483A1 (en) * | 2012-07-16 | 2014-01-22 | Basf Se | Graphene containing nitrogen and optionally iron and/or cobalt |
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