CN105788885A - Process for preparing camellia petal based sulfur and nitrogen co-doping draped nanosheet by explosion method and fabrication method of supercapacitor electrode - Google Patents
Process for preparing camellia petal based sulfur and nitrogen co-doping draped nanosheet by explosion method and fabrication method of supercapacitor electrode Download PDFInfo
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—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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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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Abstract
The invention belongs to the field of preparation of a biomass based carbon material, and particularly discloses a process for a preparing camellia petal based sulfur and nitrogen co-doping draped nanosheet by an explosion method and a fabrication method of a supercapacitor electrode. The process comprises the following steps of pre-processing raw materials; preparing the camellia petal based sulfur and nitrogen co-doping draped nanosheet, in which a nitrogen source, a sulfur source and an ignition material are added into camellia petal powder after pre-processed and are uniformly mixed, the mixture is placed in a reactor, the temperature is maintained at 700-900 DEG C, and reaction is continued for1-3 hours under the protection of an inertia gas; and post-processing the product. The camellia petal having a sheet-shaped structure is adopted as a carbon source, the nitrogen source, the sulfur source and the ignition material are added to generate sharp reaction similar to explosion in a high temperature so as to tear the camellia petal into carbon nanosheets, and meanwhile, carbonization of the camellia petal and sulfur and nitrogen co-doping are achieved. The fabrication method is simple and is low in cost and high in production efficiency, energy sources are saved, and the product has favorable electrochemical performance.
Description
Technical field
The invention belongs to the preparation field of biomass-based material with carbon element, be specifically related to the preparation method that a kind of explosion method prepares Flos Camelliae Japonicae petal base sulfur, the technique of nitrogen co-doped fold carbon nanosheet and electrode of super capacitor.
Background technology
Ultracapacitor is a kind of Novel energy storage apparatus, the feature such as it has, and specific capacitance is big, the charging interval is short, long service life, good temp characteristic and environmental protection.It bridges the function of the high energy storage of the high-power output of conventional electrostatic capacitor and battery/fuel cell, it is believed that be future ideality electrochmical power source, so having broad application prospects and huge economic benefit.In electrode material for super capacitor, the earliest and most widely used be various forms of material with carbon elements.
Super capacitor carbon electrode material develops into widely studied at present carbon fiber, CNT and Graphene etc. gradually from the activated carbon that specific surface area the earliest is big.Graphene is a kind of Two-dimensional Carbon material, and due to the two-dimensional structure of its uniqueness, therefore big specific surface area, good electric conductivity are widely used and the energy storage field such as super capacitor, lithium battery, sode cell, lithium-air battery.But what expensive, the shortcoming such as productivity is low, poor ductility, preparation process are loaded down with trivial details of grapheme material was very big limits its application in actual industrial.In recent years, there is the carbon nanosheet being similar to graphene-structured (lamella structure) and present some physics being similar to Graphene and chemical property too, as having high conductivity, big specific surface area, excellent chemical stability etc..Scientists, by introducing the assorted elements such as N, P, S, improves its machinery, conduction and chemical property significantly.But the preparation of Graphene also exists so far: series of problems such as cost height, complex process, environment are unfriendly.The reinforcement gradually of people's environmental consciousness, garbage recycling consciousness in the last few years, biomass carbon is increasingly becoming study hotspot as energy storage device electrode materials such as ultracapacitor, lithium electricity.
In prior art, utilizing the method that biomass carbon prepares carbon nanosheet to be mainly plasma enhanced chemical vapor deposition method, arc discharge method, template etc., these methods not only equipment requirements is higher, and the yield of product is relatively low.Additionally, the cost of material is also the factor of required consideration.
Therefore a kind of raw material sources of exploitation is extensive, and technique with low cost and simple is carried out scale and prepared N, S or two kinds of element codope carbon nanosheets have very important using value.
Summary of the invention
It is an object of the invention to provide the preparation method that a kind of explosion method prepares the electrode of Flos Camelliae Japonicae petal base sulfur, the technique of nitrogen co-doped fold carbon nanosheet and a kind of ultracapacitor, above-mentioned technique has simply, reproducible, with low cost, advantages of environment protection, and the electrode of the Flos Camelliae Japonicae petal base sulfur of preparation, nitrogen co-doped fold carbon nanosheet and super capacitor has good chemical property.
Above-mentioned purpose is to be achieved through the following technical solutions: a kind of explosion method prepares the technique of Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, comprises the steps:
(1): the pretreatment of raw material: Flos Camelliae Japonicae petal is carried out, dries, mechanical activation comminution, then sieve；
(2): Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet preparation: in Flos Camelliae Japonicae petal powder after pretreatment, add nitrogenous source, sulfur source and detonator mix homogeneously; mixture is put in reactor; maintain temperature at 700～900 DEG C, sustained response 1～3h under inert gas shielding；
(3): Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet post processing: treat that temperature drops to room temperature, take out Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, washing, dry.
The present invention adopts the Flos Camelliae Japonicae petal with laminated structure to be carbon source, utilize the laminated structure that Flos Camelliae Japonicae petal is special, occur like under high temperature after adding nitrogenous source, sulfur source and detonator the vigorous reaction of blast stratiform Flos Camelliae Japonicae petal is torn the carbonization for realizing Flos Camelliae Japonicae petal while carbon nanosheet and sulfur, nitrogen co-doped.The present invention adopts explosion method, adopts mode one step once heated to realize above-mentioned technical purpose, and preparation method is simple, and cost is low, and production efficiency is high and saves the energy.
Flos Camelliae Japonicae petal base sulfur prepared by the present invention, nitrogen co-doped fold carbon nanosheet, introduce sulfur, nitrogen-atoms in the carbon skeleton of porous carbon nanometer sheet, makes graphite microcrystal plane layer in carbon-coating produce many dislocations, bends, offing normal etc. has the defective bit of unpaired electron；Simultaneously sulfur, nitrogen-atoms introducing make material surface have alkalescence, can reinforcing material surface wettability, improve material property.The Flos Camelliae Japonicae petal base sulfur prepared by present invention process, nitrogen co-doped fold carbon nanosheet, owing to it has high specific surface area, having short ion transport distance and appropriate doping, therefore this material has good electrochemical energy storage performance, after tested, its specific surface area reaches 1100～1500m2g-1, total pore volume is 0.61～0.91cm3g-1, sulfur content 0.6～2%, nitrogen content 2～5%；Test result indicate that, using its electrode of super capacitor prepared to have high specific capacitance, desirable fake capacitance, high cyclical stability, performance is better than ultracapacitor performance and the most of the nitrogen doped porous carbon material of commercial activated carbon.
As preferably, further technical scheme is: described nitrogenous source, sulfur source and detonator are Ammonium persulfate..Ammonium persulfate. quickly decomposes to give off oxygen as detonator when higher temperature, along with the rising of temperature, decomposition reaction speed is accelerated, and reaches explosion limit during high temperature, Flos Camelliae Japonicae petal and Ammonium persulfate. and its catabolite are blasted reaction, realize the carbonization of Flos Camelliae Japonicae petal and sulfur, nitrogen co-doped simultaneously.
Further technical scheme is: the mass ratio of described Flos Camelliae Japonicae petal powder and Ammonium persulfate. is 1:0.5～1.5.
Further technical scheme is: the mass ratio of described Flos Camelliae Japonicae petal powder and Ammonium persulfate. is 1:1.
Further technical scheme is: described sulfur source is Ammonium persulfate., and described nitrogenous source is Ammonium persulfate. and other ammonium salts.Should be appreciated that other can resolve into the ammonium salt of ammonia under the high temperature conditions all can as nitrogenous source.
Further technical scheme is: described ammonium salt is one or more in ammonium nitrate, percarbonic acid ammonium and ammonium hydrogen carbonate.Ammonium nitrate, percarbonic acid ammonium and ammonium hydrogen carbonate high temperature easily decompose generation ammonia, and the ammonia of generation is prone to the reaction of Flos Camelliae Japonicae petal generation N doping in explosive reaction.
Further technical scheme is: described detonator and nitrogenous source are one or more in ammonium nitrate, percarbonic acid ammonium and Ammonium persulfate..Ammonium nitrate, percarbonic acid ammonium and Ammonium persulfate. are not only heated and easily decompose, and simultaneously during higher temperatures, are all easily caused explosive reaction.
Further technical scheme is: the reaction temperature in described step (2) is 800 DEG C.Under lot of experiment validation, this reaction temperature product performance it is further preferred that.
Further technical scheme is: the response time in described step (2) is 2h.So, on the one hand ensureing that reaction is sufficiently conducted, be unlikely to the response time on the other hand long and reduce economic benefit and efficiency.
Further technical scheme is: described noble gas is nitrogen or argon；
Further technical scheme is: the order number of the sieve used that sieves in described step (1) is 60 orders；So, ensure on the one hand material fineness, be unlikely to particle diameter on the other hand too small and waste material.
Further technical scheme is: have the step of a compacting before the mixture reaction in described step (2), and so, the structure that can make this mixture is relatively compact, reaction of just blasting after being increased to target temperature.It is pointed out that after being increased to some temperature, ammonium salt acutely decomposes, and discharges a large amount of gas and is freely overflowed by space, thus results in and do not reach explosion limit and cause reacting unsuccessfully if the mixture structure participating in reaction is not fine and close.
Further technical scheme is: described reactor is tube furnace.
For reaching above-mentioned technical purpose, the preparation method that present invention also offers the electrode of a kind of ultracapacitor, first it is the Flos Camelliae Japonicae petal base sulfur that a kind of explosion method described in the conductive agent of 1:0.5～1.5:7～9, binding agent and above-mentioned any one prepares Flos Camelliae Japonicae petal base sulfur, prepared by the technique of nitrogen co-doped fold carbon nanosheet, nitrogen co-doped fold carbon nanosheet mix homogeneously by mass ratio, add solvent furnishing muddy, the conductive substrates that above-mentioned slurry is coated on is dried, compacting under pressure 10～20Mp, prepares into electrode of super capacitor.
As preferably, further technical scheme is: described conductive agent includes a kind of or arbitrarily two or more combination in acetylene black, carbon black, Delanium, native graphite, flake graphite, vapor phase method grown carbon fiber, CNT, metal dust and metallic fiber.
Further technical scheme is: described binding agent includes that politef, Kynoar, polyethylene, polypropylene, polyacrylamide, Ethylene-Propylene-Diene copolymer resins, styrene butadiene ribber, polybutadiene, fluorubber, polycyclic oxygen second is rare, a kind of or arbitrarily two or more combination in polyvinylpyrrolidone, polyester resin, acrylic resin, phenolic resin, epoxy resin, polyvinyl alcohol and hydroxypropyl cellulose.
Further technical scheme is: described solvent includes a kind of or arbitrarily two or more combination in water, alcohols, polyalcohols, terpenoid, dimethyl carbonate, diethyl carbonate, ethyl acetate and methyl propionate.
Further technical scheme is: described conductive agent is acetylene black, and described binding agent is politef, and described solvent is water, and described conductive substrates is nickel foam.
Further technical scheme is: described conductive agent, binding agent and above-mentioned arbitrary a kind of explosion method prepares Flos Camelliae Japonicae petal base sulfur, the mass ratio of Flos Camelliae Japonicae petal base sulfur prepared by the technique of nitrogen co-doped fold carbon nanosheet, nitrogen co-doped fold carbon nanosheet is 1:1:8.
Further technical scheme is: described pressure is 15MPa.
Further technical scheme is: the method for described coating includes a kind of or arbitrarily two or more combination in dip-coating method, knife coating, spin-coating method, spraying process, silk screen print method and suspended particles dip coating.
Further technical scheme is: described conductive substrates be sized to 1 square centimeter.
In sum; the present invention utilizes Flos Camelliae Japonicae petal cheap and easy to get to be raw material; utilize the architectural feature that it is special; by mixing with nitrogenous source, sulfur source and detonator after simple pretreatment; under inert gas shielding, carry out carbonization and sulfur, nitrogen co-doped, obtain that there is the Flos Camelliae Japonicae petal base sulfur of large specific surface area and superelevation pore volume, nitrogen co-doped fold carbon nanosheet.It addition, experiments verify that, the motor of the ultracapacitor of preparation shows good chemical property and higher cycle efficieny ratio.The present invention is with low cost, technique is simple, is conducive to industrialization.
Accompanying drawing explanation
The accompanying drawing constituting the part of the present invention is used for providing a further understanding of the present invention, and the schematic description and description of the present invention is used for explaining the present invention, is not intended that inappropriate limitation of the present invention.
Fig. 1 is Flos Camelliae Japonicae petal base sulfur in embodiment 1, nitrogen co-doped fold carbon nanosheet SEM and TEM figure；
Fig. 2 is Flos Camelliae Japonicae petal base sulfur in embodiment 1, nitrogen co-doped fold carbon nanosheet BET adsorption curve figure；
Fig. 3 is Flos Camelliae Japonicae petal base sulfur in embodiment 1, nitrogen co-doped fold carbon nanosheet XPS figure；
Fig. 4 is that the ratio electric capacity of electrode of super capacitor prepared by Flos Camelliae Japonicae petal base sulfur in embodiment 1, nitrogen co-doped fold carbon nanosheet is along with current density change curve chart；
Fig. 5 is Flos Camelliae Japonicae petal base sulfur in embodiment 1, nitrogen co-doped fold carbon nanosheet ultracapacitor cycle performance figure；
Fig. 6 is Flos Camelliae Japonicae petal base sulfur in embodiment 1, the test of nitrogen co-doped fold carbon nanosheet lithium battery high rate performance.
Detailed description of the invention
Describing the present invention below in conjunction with accompanying drawing, the description of this part is only exemplary and explanatory, and protection scope of the present invention should not have any restriction effect.Additionally, the description that those skilled in the art are according to presents, it is possible to the feature in embodiment in presents and in different embodiment is carried out respective combination.
Embodiment 1
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh 2g lower part of screen to divide and put into Achates with 2g Ammonium persulfate. simultaneously and grind in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under nitrogen protection; react; temperature is maintained at 800 DEG C, continues 2h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Its specific surface area reaches 1500m after tested2g-1, total pore volume is 0.91cm3g-1, sulfur content 2%, nitrogen content 5%；
From a, b in Fig. 1, scanning electron microscope in different multiplying can be seen that this uniformity, and known fold stratiform nanometer sheet is successfully synthesized out: from c, d is known, projecting Electronic Speculum figure in different multiplying and can be seen that this nanometer sheet has a lot of balloon-shaped structure, being conducive to increasing specific surface area thus improving chemical property.
Fig. 2 is Type-IV type nitrogen adsorption curve, and this Flos Camelliae Japonicae petal base sulfur provable, nitrogen co-doped fold carbon nanosheet material have higher specific surface area, and have micropore and mesoporous distribution
Fig. 3 is Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet XPS figure, can be seen that the peak of obvious sulfur, nitrogen element in the figure, it was demonstrated that this carbon nanosheet has successfully been doped with nitrogen sulfur heteroatom.
By according to the acetylene black of 1:1:8 ratio, politef, Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet mix homogeneously, add water furnishing muddy, knife coating uniform application is adopted to dry in the nickel foam of a square centimeter, 15Mp compacting, prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is up to 275Fg–1。
As shown in Figure 4, along with the increase of electric current density, also more little than electric capacity decreasing value, i.e. the electrode performance of electric capacity prepared by this material not substantially decay under adding high current density, at 20Ag-1Electric current density under, still can keep reaching 240Fg than electric capacity–1Left and right, illustrates that Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet have higher meso-hole structure, adds material with carbon element with putting the contact area solving matter and reduces the resistance that ion spreads, thus improving its capacitive property.
As shown in Figure 5, along with the increase recycling number of times, its capacity retention declines and inconspicuous, after circulating 10,000 times, capacity retention is still about 98%, it was demonstrated that the electrode of Flos Camelliae Japonicae petal base sulfur prepared by the present invention, nitrogen co-doped fold carbon nanosheet and ultracapacitor prepared therefrom has superior cycle performance.
Additionally, when Flos Camelliae Japonicae petal base sulfur prepared by the use present invention, nitrogen co-doped fold carbon nanosheet are as Anode of lithium cell material, also obvious advantage is embodied, as shown in Figure 6, this anode material first discharge specific capacity is up to 1600mAh/g, under 10A/g high current density, its specific capacity still has 200mAh/g, hence it is evident that be better than commercial graphite electrode.
Embodiment 2
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh 2g lower part of screen to divide and put into Achates with 2g Ammonium persulfate. simultaneously and grind in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under nitrogen protection; react; temperature is maintained at 700 DEG C, continues 2h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Its specific surface area reaches 1122m after tested2g-1, total pore volume is 0.61cm3g-1。
By according to the acetylene black of 1:1:8 ratio, politef, Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet mix homogeneously, add water furnishing muddy, knife coating uniform application is adopted to dry in the nickel foam of a square centimeter, 20Mp compacting, prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is 229Fg–1。
Embodiment 3
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh 2g lower part of screen to divide and put into Achates with 2g Ammonium persulfate. simultaneously and grind in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under nitrogen protection; react; temperature is maintained at 900 DEG C, continues 2h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Its specific surface area reaches 1563m after tested2g-1, total pore volume is 0.95cm3g-1, it is necessary to explanation, under this condition, product yield is non-normally low, below 10%.
By according to the acetylene black of 1:1:8 ratio, politef, Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet mix homogeneously, add water furnishing muddy, dip-coating method uniform application is adopted to dry in the nickel foam of a square centimeter, 10Mp compacting, prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is 174Fg–1。
Embodiment 4
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh 2g lower part of screen to divide and put into Achates with 1g Ammonium persulfate. simultaneously and grind in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under argon shield; react; temperature is maintained at 800 DEG C, continues 2h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Its specific surface area reaches 659m after tested2g-1, total pore volume is 0.36cm3g-1。
By according to the acetylene black of 1:1:8 ratio, politef, Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet mix homogeneously, add water furnishing muddy, silk screen print method uniform application is adopted to dry in the nickel foam of a square centimeter, 15Mp compacting, prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is 162Fg–1。
Embodiment 5
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh 2g lower part of screen to divide and put into Achates with 3g Ammonium persulfate. simultaneously and grind in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under argon shield; react; temperature is maintained at 800 DEG C, continues 1h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Industry is tested its specific surface area and is reached 1122m2g-1, total pore volume is 0.62cm3g-1, it is necessary to explanation, under this condition, product yield is non-normally low, below 10%.
By according to the acetylene black of 1:0.5:8 ratio, politef, Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet mix homogeneously, add water furnishing muddy, suspended particles dip coating uniform application is adopted to dry in the nickel foam of a square centimeter, 10Mp compacting, prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is 195Fg–1。
Embodiment 6
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh that 2g lower part of screen is divided, 2g percarbonic acid ammonium and 0.5g Ammonium persulfate. are put into Achates simultaneously and ground in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under nitrogen protection; react; temperature is maintained at 800 DEG C, continues 2h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Its specific surface area reaches 1012m after tested2g-1, total pore volume is 0.58cm3g-1。
By according to the acetylene black of 1:1.5:7 ratio, politef, Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet mix homogeneously, add water furnishing muddy, spraying process uniform application is adopted to dry in the nickel foam of a square centimeter, 15Mp compacting, prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is 155Fg–1。
Embodiment 7
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh that 2g lower part of screen is divided, 2g ammonium nitrate and 0.5g Ammonium persulfate. are put into Achates simultaneously and ground in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under nitrogen protection; react; temperature is maintained at 800 DEG C, continues 2h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Its specific surface area reaches 1368m after tested2g-1, total pore volume is 0.88cm3g-1。
By according to the acetylene black of 1:1:9 ratio, politef, Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet mix homogeneously, add water furnishing muddy, spin-coating method uniform application is adopted to dry in the nickel foam of a square centimeter, 15Mp compacting, prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is 212Fg–1。
Embodiment 8
After collecting that the Flos Camelliae Japonicae petal washing that the biomass material come withers is dry, pulverizing, cross 60 mesh sieves, take lower part of screen and divide.Weigh that 2g lower part of screen is divided, 1g ammonium hydrogen carbonate and 1g Ammonium persulfate. are put into Achates and ground in alms bowl and mill; so as to be sufficiently mixed; homogeneous mixture is transferred in magnetic boat the compacting of medication spoon; put into and tube furnace is warming up to reaction target temperature under argon shield; react; temperature is maintained at 800 DEG C, continues 1h, forms sulfur and nitrogen co-doped fold carbon nanosheet.
Prepared Flos Camelliae Japonicae petal base sulfur, the washing of nitrogen co-doped fold carbon nanosheet are dried.Its specific surface area reaches 1321m after tested2g-1, total pore volume is 0.83cm3g-1。
nullBy the conductive agent (acetylene black according to 1:1:8 ratio、Carbon black、Delanium、Native graphite、Flake graphite、Vapor phase method grown carbon fiber、CNT、Metal dust、A kind of or arbitrarily two or more with in metallic fiber)、Binding agent (tetrafluoroethene、Kynoar、Polyethylene、Polypropylene、Polyacrylamide、Ethylene-Propylene-Diene copolymer resins、Styrene butadiene ribber、Polybutadiene、Fluorubber、Polycyclic oxygen second is rare、Polyvinylpyrrolidone、Polyester resin、Acrylic resin、Phenolic resin、Epoxy resin、Polyvinyl alcohol、With a kind of or arbitrarily two or more combination in hydroxypropyl cellulose)、Flos Camelliae Japonicae petal base sulfur、Nitrogen co-doped carbon nanosheet mix homogeneously，Add solvent (water、Alcohols、Polyalcohols、Terpenoid、Dimethyl carbonate、Diethyl carbonate、Ethyl acetate、With a kind of or arbitrarily two or more combination in methyl propionate) furnishing muddy，Silk screen print method uniform application is adopted to dry in the nickel foam of a square centimeter，15Mp compacting，Prepare electrode of super capacitor.
After tested, the ratio electric capacity of the electrode of super capacitor of preparation is 210～227Fg–1。
Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet property representation
Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet structural characterization pass through N2Absorption (MicromeriticsTriStarII3020) test.Specific surface area is according to Brunauer-Emmett-Teller (BET) Theoretical Calculation, and pore-size distribution (PSD) adopts the absorption of adsorption isotherm to prop up and adopts Barrett-Joyner-Halenda (BJH) model to calculate.
Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped carbon nanosheet are the method for testing that the electrode of ultracapacitor prepared by raw material
Unipolar capacitive property adopts CHI760D electrochemical workstation three-electrode system to test, and is wherein platinum electrode to electrode, and Hg/HgO is reference electrode, and 6MKOH solution is electrolyte.This example mainly adopts the methods such as cyclic voltammetry (CV), constant current charge-discharge (GC) and electrochemical impedance spectroscopy (EIS) to carry out electrochemical property test.The cyclic voltammetry voltage range of single electrode is set as-1～0V.The electric current density of charge-discharge test is arranged on 0.5～20Ag-1, and voltage range is-1～0V.The ratio electric capacity of material with carbon element is propped up by the electric discharge of constant current charge-discharge, and calculates according to below equation:
C=I/ (mdV/dt)
Wherein I is constant current, and m is the quality of active substance, and dV/dt is the slope calculating gained according to the discharge curve removing voltage drop part.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. the technique that an explosion method prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that comprise the steps:
(1): the pretreatment of raw material: Flos Camelliae Japonicae petal is carried out, dries, mechanical activation comminution, then sieve；
(2): Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet preparation: in Flos Camelliae Japonicae petal powder after pretreatment, add nitrogenous source, sulfur source and detonator mix homogeneously; mixture is put in reactor; maintain temperature at 700～900 DEG C, sustained response 1～3h under inert gas shielding；
(3): Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet post processing: treat that temperature drops to room temperature, take out Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, washing, dry.
2. the technique that a kind of explosion method according to claim 1 prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that described nitrogenous source, sulfur source and detonator are Ammonium persulfate..
3. the technique that a kind of explosion method according to claim 2 prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that the mass ratio of described Flos Camelliae Japonicae petal powder and Ammonium persulfate. is 1:0.5～1.5.
4. the technique that a kind of explosion method according to claim 3 prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that the mass ratio of described Flos Camelliae Japonicae petal powder and Ammonium persulfate. is 1:1.
5. the technique that a kind of explosion method according to claim 1 prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that described sulfur source is Ammonium persulfate., described nitrogenous source is Ammonium persulfate. and other ammonium salts.
6. the technique that a kind of explosion method according to claim 5 prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that described ammonium salt is one or more in ammonium nitrate, percarbonic acid ammonium and ammonium hydrogen carbonate.
7. the technique that a kind of explosion method according to claim 1 prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that described detonator and nitrogenous source are one or more in ammonium nitrate, percarbonic acid ammonium and Ammonium persulfate..
8. the technique that a kind of explosion method according to claim 1～7 any one prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that the reaction temperature in described step (2) is 800 DEG C.
9. the technique that a kind of explosion method according to claim 8 prepares Flos Camelliae Japonicae petal base sulfur, nitrogen co-doped fold carbon nanosheet, it is characterised in that the response time in described step (2) is 2h；Or described noble gas is nitrogen or argon；Or the order number of the sieve used that sieves in described step (1) is 60 orders；Or before the mixture reaction in described step (2), have the step of a compacting；Or described reactor is tube furnace.
10. the preparation method of the electrode of a ultracapacitor, it is characterized in that, it is the Flos Camelliae Japonicae petal base sulfur that a kind of explosion method described in the conductive agent of 1:0.5～1.5:7～9, binding agent and claim 1～13 any one prepares Flos Camelliae Japonicae petal base sulfur, prepared by the technique of nitrogen co-doped fold carbon nanosheet, nitrogen co-doped fold carbon nanosheet mix homogeneously by mass ratio, add solvent furnishing muddy, the conductive substrates that above-mentioned slurry is coated on is dried, compacting under pressure 10～20Mp, prepares into electrode of super capacitor；Or described conductive agent includes a kind of or arbitrarily two or more combination in acetylene black, carbon black, Delanium, native graphite, flake graphite, vapor phase method grown carbon fiber, CNT, metal dust and metallic fiber；Or described binding agent includes that politef, Kynoar, polyethylene, polypropylene, polyacrylamide, Ethylene-Propylene-Diene copolymer resins, styrene butadiene ribber, polybutadiene, fluorubber, polycyclic oxygen second is rare, a kind of or arbitrarily two or more combination in polyvinylpyrrolidone, polyester resin, acrylic resin, phenolic resin, epoxy resin, polyvinyl alcohol and hydroxypropyl cellulose；Or described solvent includes a kind of or arbitrarily two or more combination in water, alcohols, polyalcohols, terpenoid, dimethyl carbonate, diethyl carbonate, ethyl acetate and methyl propionate；Or described conductive agent is acetylene black, described binding agent is politef, and described solvent is water, and described conductive substrates is nickel foam；Or described in described conductive agent, binding agent and claim 1～13 any one a kind of explosion method prepares Flos Camelliae Japonicae petal base sulfur, the mass ratio of Flos Camelliae Japonicae petal base sulfur prepared by the technique of nitrogen co-doped fold carbon nanosheet, nitrogen co-doped fold carbon nanosheet is 1:1:8；Or described pressure is 15MPa；Or the method for described coating includes a kind of or arbitrarily two or more combination in dip-coating method, knife coating, spin-coating method, spraying process, silk screen print method and suspended particles dip coating；Or described conductive substrates be sized to 1 square centimeter.
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