CN110028053A - A kind of preparation method and applications of high nitrogen doped amount nano cages material - Google Patents
A kind of preparation method and applications of high nitrogen doped amount nano cages material Download PDFInfo
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- CN110028053A CN110028053A CN201910406251.2A CN201910406251A CN110028053A CN 110028053 A CN110028053 A CN 110028053A CN 201910406251 A CN201910406251 A CN 201910406251A CN 110028053 A CN110028053 A CN 110028053A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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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
-
- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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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- 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 belongs to electrode material for super capacitor technical fields, more particularly to a kind of preparation method and applications of high nitrogen doped amount nano cages material, the present invention is using sucrose as carbon source, using dicyandiamide as nitrogen source, using potassium chloride as template, high temperature cabonization is handled after ball milling in ball mill, make to obtain the material that carbon is wrapped in potassium chloride surface, it is placed in impregnate and can dissolve potassium chloride, remove potassium chloride template, obtain nitrogen-doped carbon nanocages material, present invention process is simple, it is suitble to large-scale industrial production, and go removing template without strong acid or strong base solution, direct water impregnates, it is environmentally protective, obtained nano cages material can be used as electrode material for super capacitor, with excellent capacitance characteristic, rectangle possessed by ideal capacitance electrode material is presented in cyclic voltammetry curve, specific capacitance energy under 2mV/s scanning speed Reach 238F/g.
Description
Technical field
The invention belongs to electrode material for super capacitor technical fields, and in particular to a kind of high nitrogen doped amount nano cages material
The preparation method and applications of material.
Background technique
Supercapacitor is also known as electrochemical capacitor, is that one kind between classic flat-plate capacitor and secondary cell is new
Type energy storage device.Supercapacitor has many advantages, such as that power density is high relative to traditional secondary battery, has extended cycle life, Ke Yizuo
For the electrical source of power of electronic equipment and electric car, thus it is with a wide range of applications.Active carbon is as electrode material at present
Supercapacitor have been carried out commercialization, and be widely used in numerous areas.But due to the mesoporous ratio of active carbon
It is low, and there is no macropore, it is poor with the super capacitor high rate performance that active carbon does electrode.In recent years, nitrogen-doped carbon material is as super
Grade electrode for capacitors is by more and more extensive concern.The nitrogen-doped carbon material as electrode material for super capacitor of open report
Preparation method also difference.
Chinese patent 201811602004.1 is open to report a kind of nitrogen-doped carbon material and preparation method thereof.Utilize trimerization
For cyanamide as raw material, three of them chlorine activity is different, reacts at three temperatures with the amino of p-phenylenediamine respectively, building three
Piperazine network structure is prepared with three-dimensional porous nitrogen-doped carbon material.
Chinese patent 201711206128.3 is open to report a kind of method for preparing nitrogen-doped carbon aeroge, is with bean dregs
Carbon source, the concentrated sulfuric acid are hydrolyst, and bean dregs and the concentrated sulfuric acid are mixed evenly, and form carbon sol presoma.It is again that carbon is molten
Glue is diluted with water, and handles to obtain tan precipitate through microwave hydrothermal, filters, is dry, final high temperature cabonization obtains the carbon gas of N doping
Gel.
Therefore, it is very necessary that one kind at low cost, simple process, the good nitrogen-doped carbon material of capacitive property are found.
Summary of the invention
It is an object of that present invention to provide a kind of preparation method of high nitrogen doped amount nano cages material, raw material is easy to get cost
It is low, simple process；Present invention simultaneously provides obtained high nitrogen doped amount nano cages materials in the application in supercapacitor,
It can be used as electrode material, there is good capacitive property.
The preparation method of high nitrogen doped amount nano cages material of the present invention, comprising the following steps:
(1) it using sucrose, potassium chloride, dicyandiamide as raw material, is placed in ball milling in ball grinder and obtains solid powder；
(2) solid powder is placed in quartz boat, is then placed in the tube furnace equipped with quartz ampoule, is passed through inert gas,
Heating carries out high temperature cabonization processing, is cooled to room temperature, obtains head product；
(3) head product is put into water and is impregnated, filtered, dry to obtain finished product.
Sucrose, potassium chloride, dicyandiamide mass ratio be 1:0.01~100:0.1~10.
Raw material Ball-milling Time is 0.1~12h, and ball, material mass ratio control are in 1~100:1 when ball milling.
Inert gas is one of nitrogen, argon gas or helium or a variety of, and flow velocity of the inert gas in tube furnace is 20
~100mLmin-1.
Tube furnace heating rate is 1~20 DEG C of min-1, and 500~1000 DEG C of high temperature cabonization temperature, soaking time is
0.01-20h。
The time impregnated in water be 0.1~for 24 hours, water temperature be 10~100 DEG C.
Nitrogen content is 1~12at.% in obtained high nitrogen doped amount nano cages finished material.
The application of high nitrogen doped amount nano cages material obtained by the present invention, as electrode material in supercapacitor
Application, have good capacitive property.
Compared with prior art, the present invention having the advantages that.
(1) raw material sucrose, dicyandiamide, potassium chloride are from a wealth of sources in the present invention, cheap；
(2) present invention is using sucrose as carbon source, and using dicyandiamide as nitrogen source, using potassium chloride as template, the above raw material is in ball mill
High temperature cabonization is handled after middle ball milling, makes to obtain the material that carbon is wrapped in potassium chloride surface, and chlorine can be dissolved by being placed in impregnate
Change potassium, remove potassium chloride template, obtain nitrogen-doped carbon nanocages material, present invention process is simple, is suitble to large-scale industry metaplasia
It produces, and goes removing template without strong acid or strong base solution, direct water impregnates, environmentally protective；
(3) nano cages material nano cages size obtained by the present invention is in 500nm or so, size uniformity, nano cages
Wall thickness is between 2~10nm, 400~650m of specific surface area2·g-1, nitrogen content is 1~12at.%, can be used as supercapacitor
Electrode material has excellent capacitance characteristic, and rectangle possessed by ideal capacitance electrode material is presented in cyclic voltammetry curve,
Specific capacitance under 2mV/s scanning speed can reach 238F/g.
Detailed description of the invention
Scanning electron microscope (SEM) figure of high nitrogen doped amount nano cages electrode material prepared by Fig. 1, the embodiment of the present invention 1；
Nitrogen adsorption-desorption curve of high nitrogen doped amount nano cages electrode material prepared by Fig. 2, the embodiment of the present invention 1；
The cyclic voltammetry curve of high nitrogen doped amount nano cages electrode material prepared by Fig. 3, the embodiment of the present invention 1.
Such as Fig. 1, high nitrogen doped amount nano cages electrode material prepared by the present invention is of uniform size, and cage size is on the left side 500nm
It is right；
Such as Fig. 2, high nitrogen doped amount nano cages electrode material specific surface area 596m obtained by the present invention2g-1；
Such as Fig. 3, the cyclic voltammetry curve of high nitrogen doped amount nano cages electrode material obtained by the present invention presents ideal
Rectangle possessed by capacitance electrode material.
Specific embodiment
Below with reference to embodiment and Figure of description, the present invention will be further described.
Embodiment 1
It weighs 3g sucrose, 18g potassium chloride, 3g dicyandiamide to be put into polytetrafluoro ball grinder, then weighs the Ma of quality 100g
Nao ball is put into ball grinder, ball milling 2h.Solid powder after ball milling is placed in quartz boat, the pipe equipped with quartz ampoule is then placed in
In formula furnace；It is passed through nitrogen inert gas, flow velocity of the inert gas in tube furnace is in 50mL min-1, then with 5 DEG C of min-1's
Temperature is risen to 800 DEG C by heating rate, and high temperature cabonization soaking time is 2h, obtains head product.Obtained head product is soaked with hot water
Bubble processing 8h, then filters, and is placed in baking oven drying at 80 DEG C and for 24 hours, obtains nitrogen-doped carbon nanocages material, nitrogen content is
11.3at%.
Nano cages material made from the present embodiment is pressed into active material: conductive agent (graphite): binder (polytetrafluoroethyl-ne
Alkene)=85:10:5 ratio mixed after be prepared into electrode slice, cyclic voltammetry is carried out in 6M KOH electrolyte, survey
Test result is as shown in figure 3, nano cages electrode material manufactured in the present embodiment cyclic voltammetric under the scanning speed of 100mV/s is bent
Line still keeps preferable rectangular shape, and the specific capacitance under 2mV/s scanning speed can reach 238F/g.
Embodiment 2
It weighs 3g sucrose, 0.3g potassium chloride, 0.3g dicyandiamide to be put into polytetrafluoro ball grinder, then weighs quality 3.6g's
Agate ball is put into ball grinder, ball milling 0.1h.Solid powder after ball milling is placed in quartz boat, is then placed in equipped with quartz ampoule
Tube furnace in；It is passed through nitrogen inert gas, flow velocity of the inert gas in tube furnace is in 20mLmin-1, then with 1 DEG C of min-1
Heating rate temperature is risen to 1000 DEG C, high temperature cabonization soaking time is 0.01h, obtains head product.Obtained head product is used
10 DEG C of hot-water soak processing for 24 hours, then filter, and are placed in baking oven drying at 80 DEG C and for 24 hours, obtain nitrogen-doped carbon nanocages material,
Nitrogen content is 10.9at%.
Embodiment 3
It weighs 3g sucrose, 100g potassium chloride, 30g dicyandiamide to be put into polytetrafluoro ball grinder, then weighs quality 133g's
Agate ball is put into ball grinder, ball milling 12h.Solid powder after ball milling is placed in quartz boat, is then placed in equipped with quartz ampoule
Tube furnace in；It is passed through nitrogen inert gas, flow velocity of the inert gas in tube furnace is in 100mLmin-1, then with 20 DEG C
min-1Heating rate temperature is risen to 500 DEG C, high temperature cabonization soaking time is 0.1h, obtains head product.The head product that will be obtained
0.1h is handled with 100 DEG C of hot-water soaks, is then filtered, drying at 80 DEG C is placed in baking oven and for 24 hours, obtains nitrogen-doped carbon nanocages material
Material, nitrogen content 11.2at%.
Embodiment 4
It weighs 10g sucrose, 10g potassium chloride, 1g dicyandiamide to be put into polytetrafluoro ball grinder, then weighs the Ma of quality 80g
Nao ball is put into ball grinder, ball milling 6h.Solid powder after ball milling is placed in quartz boat, the pipe equipped with quartz ampoule is then placed in
In formula furnace；It is passed through nitrogen inert gas, flow velocity of the inert gas in tube furnace is in 90mL min-1, then with 2 DEG C of min-1's
Temperature is risen to 600 DEG C by heating rate, and high temperature cabonization soaking time is 0.5h, obtains head product.By 30 DEG C of heat of obtained product
Water immersion treatment 2h, then filters, and is placed in baking oven drying at 80 DEG C and for 24 hours, obtains nitrogen-doped carbon nanocages material, nitrogen content is
5.2at%.
Claims (8)
1. a kind of preparation method of high nitrogen doped amount nano cages material, it is characterised in that: the following steps are included:
(1) it using sucrose, potassium chloride, dicyandiamide as raw material, is placed in ball milling in ball grinder and obtains solid powder；
(2) solid powder is placed in quartz boat, is then placed in the tube furnace equipped with quartz ampoule, is passed through inert gas, heated up
High temperature cabonization processing is carried out, is cooled to room temperature, obtains head product；
(3) head product is put into water and is impregnated, filtered, dry to obtain finished product.
2. the preparation method of high nitrogen doped amount nano cages material according to claim 1, it is characterised in that: sucrose, chlorine
Change potassium, the mass ratio of dicyandiamide is 1:0.01~100:0.1~10.
3. the preparation method of high nitrogen doped amount nano cages material according to claim 1, it is characterised in that: raw material ball milling
Time is 0.1~12h, and ball, material mass ratio control are in 1~100:1 when ball milling.
4. the preparation method of high nitrogen doped amount nano cages material according to claim 1, it is characterised in that: inert gas
For one of nitrogen, argon gas or helium or a variety of, flow velocity of the inert gas in tube furnace is in 20~100mLmin-1。
5. the preparation method of high nitrogen doped amount nano cages material according to claim 1, it is characterised in that: tube furnace liter
Warm rate is 1~20 DEG C of min-1, 500~1000 DEG C of high temperature cabonization temperature, soaking time 0.01-20h.
6. the preparation method of high nitrogen doped amount nano cages material according to claim 1, it is characterised in that: impregnated in water
Time be 0.1~for 24 hours, water temperature be 10~100 DEG C.
7. the preparation method of -6 any high nitrogen doped amount nano cages materials according to claim 1, it is characterised in that: institute
It is 1~12at.% that nitrogen content in high nitrogen doped amount nano cages finished material, which is made,.
8. high nitrogen doped amount carbon obtained by a kind of preparation method of high nitrogen doped amount nano cages material as claimed in claim 7
The application of nanocages material, it is characterised in that: as application of the electrode material in supercapacitor.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110690463A (en) * | 2019-10-23 | 2020-01-14 | 湖南科技大学 | Preparation method of carbon hollow sphere composite material with low platinum loading capacity, product and application |
| CN111508726A (en) * | 2020-06-10 | 2020-08-07 | 广东石油化工学院 | Preparation method of dendritic fiber-shaped hollow nitrogen-doped carbon nanocage for supercapacitor |
| CN113998697A (en) * | 2021-11-03 | 2022-02-01 | 中国矿业大学 | Preparation method of leaf-based nitrogen-doped porous carbon and application of leaf-based nitrogen-doped porous carbon in oxygen reduction electrocatalysis in full pH range |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110690463A (en) * | 2019-10-23 | 2020-01-14 | 湖南科技大学 | Preparation method of carbon hollow sphere composite material with low platinum loading capacity, product and application |
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| CN111508726A (en) * | 2020-06-10 | 2020-08-07 | 广东石油化工学院 | Preparation method of dendritic fiber-shaped hollow nitrogen-doped carbon nanocage for supercapacitor |
| CN111508726B (en) * | 2020-06-10 | 2021-10-08 | 广东石油化工学院 | Preparation method of dendritic fiber-shaped hollow nitrogen-doped carbon nanocage for supercapacitor |
| CN113998697A (en) * | 2021-11-03 | 2022-02-01 | 中国矿业大学 | Preparation method of leaf-based nitrogen-doped porous carbon and application of leaf-based nitrogen-doped porous carbon in oxygen reduction electrocatalysis in full pH range |
| CN113998697B (en) * | 2021-11-03 | 2023-09-29 | 中国矿业大学 | Preparation method of leaf-based nitrogen-doped porous carbon and application of leaf-based nitrogen-doped porous carbon in oxygen reduction electrocatalysis in full pH range |
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