CN105502386A - Preparation method of microporous carbon nanosheets - Google Patents

Preparation method of microporous carbon nanosheets Download PDF

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Publication number
CN105502386A
CN105502386A CN201510948418.XA CN201510948418A CN105502386A CN 105502386 A CN105502386 A CN 105502386A CN 201510948418 A CN201510948418 A CN 201510948418A CN 105502386 A CN105502386 A CN 105502386A
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nanometer sheet
carbon
microporous carbon
carbon nanometer
template
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CN105502386B (en
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王延忠
薛超瑞
***
刘洋
刘炜
常青
董英鸽
胡胜亮
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North University of China
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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
    • H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C01P2006/17—Pore diameter distribution
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention discloses a preparation method of microporous carbon nanosheets. The microporous carbon nanosheets serve as an electrode material of supercapacitors. According to the method, water soluble inorganic salt NaCl serves as a template, and glucose, sucrose or cellulose serves as a carbon precursor; the surface of the cubic NaCl crystal template is evenly coated with a carbon source, and the NaCl template is removed through deionized water after high-temperature carbonization so that two-dimensional carbon nanosheets can be obtained; after KOH is used for high-temperature activation, potassium compounds are removed by adding dilute hydrochloric acid, and the high-specific-surface-area microporous carbon nanosheets with the thickness being dozens of nanometers are obtained. The microporous carbon nanosheets serve as the electrode material of the supercapacitors and have large specific capacitance, high rate capacity and excellent cyclic stability. Besides, the technology is simple, cost is low, and the preparation method of the microporous carbon nanosheets is suitable for industrial application.

Description

A kind of preparation method of microporous carbon nanometer sheet
Technical field
The invention belongs to new energy materials research field, relate to a kind of preparation method of high specific surface micro-pore carbon nanosheet and its application in ultracapacitor.
Background technology
Ultracapacitor is as a kind of Novel energy storage apparatus, owing to having, power density is high, fast charging and discharging, have extended cycle life, the series of advantages such as operating temperature range is wide, safety non-pollution, have broad application prospects in mobile communication, information technology, consumer electronics, electromobile, aerospace and science and techniques of defence etc., be considered to a kind of desirable chemical power source.The performance of ultracapacitor depends primarily on the specific surface area of electrode used therein material, pore size distribution, microstructure and conductivity etc.At present, commercialization ultracapacitor mainly utilizes gac as electrode materials.Compare other carbon materials, absorbent charcoal material has that specific surface area is large, abundant raw material source, low cost and other advantages.But the activated carbon granule prepared due to traditional method larger (50 ~ 200 μm), which increases the diffusion length of electrolyte ion, thus causes the performance of electrical condenser to reduce.
Carbon nanosheet, as the New Two Dimensional carbon nanomaterial of a kind graphene-structured, because it has higher specific surface area, excellent conductivity, is widely used in electrochemical energy storage and electrocatalysis field.The thickness of carbon nanosheet is generally between 10 ~ 100nm, thus significantly reduces the diffusion length of electrolyte ion.Compared with grapheme material, carbon nanosheet preparation cost is low, not easily reunites, and is considered to a kind of desirable electrode material for super capacitor.
Summary of the invention
The present invention aim to provide a kind of simple, cost is low, the preparation method of the microporous carbon nanometer sheet of high-specific surface area, when the carbon nanosheet prepared by the method is for electrode of super capacitor, electrical condenser shows good chemical property.
The invention provides a kind of preparation method of microporous carbon nanometer sheet, with water-soluble NaCl inorganic salt for template, glucose, sucrose or cellulosic one are carbon source, and after high temperature cabonization, washing removing inorganic salt template, obtains the Two-dimensional Carbon nanometer sheet of 50 ~ 200nm thickness; Then utilize KOH to activate, acquisition specific surface area is 1756 ~ 2212m 2g -1, pore volume is 0.64 ~ 1.21cm 3g -1microporous carbon nanometer sheet.
The preparation method of described microporous carbon nanometer sheet, comprises the following steps:
(1) getting glucose, sucrose or cellulosic one is carbon source, with water-soluble NaCl inorganic salt for template, is dissolved in deionized water, stirs 30 ~ 60min, 80 ~ 120 DEG C of oven dry;
The quality proportioning of described carbon source and NaCl template is: 1:1 ~ 1:6; Every 1g carbon source uses the amount of deionized water to be 5 ~ 50mL;
(2) said mixture is got, at N 2under protection, 500 ~ 600 DEG C of pre-carbonization 1 ~ 3h, then by deionized water removing inorganic salt template, filter, 80 ~ 120 DEG C of dryings, obtain Two-dimensional Carbon nanometer sheet;
(3) carbon nanosheet and KOH are mixed, at N 2under protection, 700 ~ 900 DEG C of activation 1 ~ 3h, remove impurity with 0.1 ~ 2MHCl, filter, 80 ~ 110 DEG C of dryings, obtain the finished product;
The mass ratio of described carbon nanosheet and KOH is 1:1 ~ 1:4.
Performance according to the microporous carbon nanometer sheet product of aforesaid method gained: the thickness of carbon nanosheet is 50 ~ 200nm, and specific surface area reaches 1756 ~ 2212m 2g -1with pore volume 0.64 ~ 1.21cm 3g -1.When this carbon nanosheet is used as the electrode materials of ultracapacitor, evaluate its chemical property at conventional three-electrode system, platinized platinum is to electrode, and saturated calomel is reference electrode, and electrolytic solution is 6MKOH is 1Ag in current density -1time, ratio capacitance reaches 221 ~ 308Fg -1.
Of the present invention beneficial effect:
(1) present invention process is simple, with low cost, is suitable for industrial application;
(2) compare with conventional template, water-soluble inorganic salt is cheap and easily remove;
(3) by the thickness of the add-on regulation and control carbon nanosheet of inorganic salt, shorten the diffusion length of electrolyte ion, improve capacitive property.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of embodiment 1 gained microporous carbon nanometer sheet;
Fig. 2 is the stereoscan photograph of embodiment 2 gained microporous carbon nanometer sheet;
Fig. 3 is the transmission electron microscope photo of embodiment 2 gained microporous carbon nanometer sheet;
Fig. 4 is the N of embodiment 1 and 2 gained microporous carbon nanometer sheet 2the adsorption-desorption figure profile of equilibrium;
Fig. 5 is the graph of pore diameter distribution of embodiment 1 and 2 gained microporous carbon nanometer sheet;
Fig. 6 be embodiment 1 and 2 in 6MKOH electrolytic solution, scanning speed is 50mVs -1cyclic voltammetry curve;
Fig. 7 is that embodiment 1 and 2 gained microporous carbon nanometer sheet is at 1Ag -1charging and discharging curve;
Fig. 8 is that embodiment 2 gained microporous carbon nanometer sheet is at 5Ag -1discharge and recharge 3000 circulation capacitive properties.
Embodiment
Further illustrate the present invention below by embodiment, but be not limited to following examples.
Embodiment 1(comparative example):
Taking 2g glucose adds in 50mL deionized water, and room temperature lower magnetic force stirs 30min, then at 100 DEG C of dry 10h; Mixture after drying is transferred in ceramic crucible, is placed in tube furnace, at N 2under protection, 500 DEG C of carbonization 2h; Get 1g gained carbon material to stir with 4gKOH and fully mix, be placed in tube furnace, at N 2under protection, 800 DEG C of carbonization 1h; Gained carbon material is immersed in 10h in 0.1MHCl solution, filters, 100 DEG C of vacuum-dryings, obtain micro-pore carbon material.The specific surface area of carbon material is 927m 2g -1, pore volume is 0.31cm 3g -1.
NaCl template is not used in the present embodiment.
After testing, using this carbon nanosheet as the electrode materials of ultracapacitor, in 6MKOH electrolytic solution, ratio capacitance is 184Fg -1(current density is 1Ag -1); At current density 5Ag -1under, after 3000 constant current charge-discharge circulations, ratio capacitance retention is 79.6%.
Fig. 1 shows the stereoscan photograph of the present embodiment gained microporous carbon nanometer sheet; Can see when not adding NaCl template, in carbon material, there is no carbon nanosheet.
The N of the present embodiment gained microporous carbon nanometer sheet 2the adsorption-desorption profile of equilibrium, pore size distribution, cyclic voltammetry curve and charging and discharging curve refer to Fig. 4 ~ Fig. 7.
Embodiment 2
Take 2g glucose and 4gNaCl adds in 50mL deionized water, room temperature lower magnetic force stirs 30min, then at 100 DEG C of dry 10h; Mixture after drying is transferred in ceramic crucible, is placed in tube furnace, at N 2under protection, 500 DEG C of carbonization 2h; Gained carbon material is immersed in 10h in 80 DEG C of deionized waters and removes NaCl, filter, 100 DEG C of vacuum-dryings, obtain carbon nanosheet material; Get 1g carbon nanosheet to stir with 4gKOH and fully mix, be placed in tube furnace, at N 2under protection, 800 DEG C of carbonization 1h; Gained carbon material is immersed in 10h in 0.1MHCl solution, filters, 100 DEG C of vacuum-dryings, obtain microporous carbon nanometer sheet material.
The specific surface area of carbon nanosheet is 2212m 2g -1, pore volume is 1.21cm 3g -1.
After testing, using this carbon nanosheet as the electrode materials of ultracapacitor, in 6MKOH electrolytic solution, ratio capacitance is 308Fg -1(current density is 1Ag -1), at current density 5Ag -1under, after 3000 constant current charge-discharge circulations, ratio capacitance retention is 95.6%.
Fig. 2 shows the stereoscan photograph of the present embodiment gained microporous carbon nanometer sheet, and after showing to add NaCl template, obtain sheet carbon material structure, thickness is 50 ~ 100nm.Transmission electron microscope photo (Fig. 3) further demonstrates and obtains carbon nanosheet structure.
Fig. 4 ~ Fig. 7 contrast shows the N of embodiment 1 and 2 products obtained therefrom 2adsorption-desorption balance defect, pore size distribution, cyclic voltammetry curve and charging and discharging curve figure, the surface-area obtaining carbon nanosheet material after showing to add NaCl template reaches 2212m 2g -1, this is far above the specific surface area (927m of carbon material not adding NaCl template 2g -1).The carbon nanosheet structure of high-specific surface area result in excellent capacitive property (Fig. 6 and Fig. 7).
Fig. 8 shows the present embodiment gained microporous carbon nanometer sheet at 5Ag -1discharge and recharge 3000 circulation capacitive properties, ratio capacitance retention is 95.6%, shows that this material has good electrochemical stability.
Embodiment 3
Take 2g glucose and 8gNaCl adds in 50mL deionized water, room temperature lower magnetic force stirs 30min, then at 100 DEG C of dry 10h; Mixture after drying is transferred in ceramic crucible, is placed in tube furnace, at N 2under protection, 500 DEG C of carbonization 2h; Gained carbon material is immersed in 10h in 80 DEG C of deionized waters and removes NaCl, filter, 100 DEG C of vacuum-dryings, obtain carbon nanosheet material; Get 1g carbon nanosheet to stir with 4gKOH and fully mix, be placed in tube furnace, at N 2under protection, 800 DEG C of carbonization 1h; Gained carbon material is immersed in 10h in 0.1MHCl solution, filters, 100 DEG C of vacuum-dryings, obtain microporous carbon nanometer sheet material.
The specific surface area of carbon nanosheet is 2000m 2g -1, pore volume is 1.0cm 3g -1.
After testing, using this carbon nanosheet as the electrode materials of ultracapacitor, in 6MKOH electrolytic solution, ratio capacitance is 288Fg -1(current density is 1Ag -1), at current density 5Ag -1under, after 3000 circulations, ratio capacitance retention is 92.6%.
Embodiment 4
Take 2g glucose and 12gNaCl adds in 50mL deionized water, room temperature lower magnetic force stirs 30min, then at 100 DEG C of dry 10h; Mixture after drying is transferred in ceramic crucible, is placed in tube furnace, at N 2under protection, 500 DEG C of carbonization 2h; Gained carbon material is immersed in 10h in 80 DEG C of deionized waters and removes NaCl, filter, 100 DEG C of vacuum-dryings, obtain carbon nanosheet material; Get 1g carbon nanosheet to stir with 4gKOH and fully mix, be placed in tube furnace, at N 2under protection, 800 DEG C of carbonization 1h; Gained carbon material is immersed in 10h in 0.1MHCl solution, filters, 100 DEG C of vacuum-dryings, obtain microporous carbon nanometer sheet material.The specific surface area of carbon nanosheet is 1756m 2g -1, pore volume is 0.64cm 3g -1.After testing, using this carbon nanosheet as the electrode materials of ultracapacitor, in 6MKOH electrolytic solution, ratio capacitance is 221Fg -1(current density is 1Ag -1), at current density 5Ag -1under, after 3000 circulations, ratio capacitance retention is 80.6%.
As can be seen from embodiment 1 ~ 4, when identical carbon source (experiment adopts glucose), identical activator (experiment adopts potassium hydroxide), identical quality proportioning and identical preparation technology, adopt the present invention to add NaCl template and obtain high-specific surface area Two-dimensional Carbon nanometer sheet, do not add NaCl template and then obtain traditional gac; Prepared carbon nanosheet is than not adding the gac specific surface area of Template preparation from 927m 2g -1be increased to 2212m 2g -1, pore volume is from 0.31cm 3g -1be increased to 1.21cm 3g -1.When being used as electrode of super capacitor, electrical condenser is being 1Ag than electric current -1time, ratio capacitance is from 184Fg -1be increased to 308Fg -1.Show that the gac adopting the present invention to prepare possesses higher specific surface area, pore volume and better chemical property.
Embodiment 5
Take 2g sucrose and 4gNaCl adds in 30mL deionized water, room temperature lower magnetic force stirs 10min, then at 120 DEG C of dry 5h; Mixture after drying is transferred in ceramic crucible, is placed in tube furnace, at N 2under protection, 600 DEG C of carbonization 1h; Gained carbon material is immersed in 10h in 100 DEG C of deionized waters and removes NaCl, filter, 120 DEG C of vacuum-dryings, obtain carbon nanosheet material; Get 1g carbon nanosheet to stir with 4gKOH and fully mix, be placed in tube furnace, at N 2under protection, 900 DEG C of carbonization 1h; Gained carbon material is immersed in 10h in 1MHCl solution, filters, 100 DEG C of vacuum-dryings, obtain microporous carbon nanometer sheet material.The specific surface area of carbon nanosheet is 2156m 2g -1, pore volume is 1.16cm 3g -1.After testing, using this carbon nanosheet as the electrode materials of ultracapacitor, in 6MKOH electrolytic solution, ratio capacitance is 298Fg -1(current density is 1Ag -1), at current density 5Ag -1under, after 3000 circulations, ratio capacitance retention is 93.6%.
Embodiment 6
Take 2g Mierocrystalline cellulose and 4gNaCl adds in 30mL deionized water, room temperature lower magnetic force stirs 60min, then at 120 DEG C of dry 10h; Mixture after drying is transferred in ceramic crucible, is placed in tube furnace, at N 2under protection, 550 DEG C of carbonization 3h; Gained carbon material is immersed in 10h in 80 DEG C of deionized waters and removes NaCl, filter, 100 DEG C of vacuum-dryings, obtain carbon nanosheet material; Get 1g carbon nanosheet to stir with 4gKOH and fully mix, be placed in tube furnace, at N 2under protection, 800 DEG C of carbonization 1h; Gained carbon material is immersed in 8h in 2MHCl solution, filters, 110 DEG C of vacuum-dryings, obtain microporous carbon nanometer sheet material.The specific surface area of carbon nanosheet is 2089m 2g -1, pore volume is 1.13cm 3g -1.After testing, using this carbon nanosheet as the electrode materials of ultracapacitor, in 6MKOH electrolytic solution, ratio capacitance is 287Fg -1(current density is 1Ag -1), at current density 5Ag -1under, after 3000 circulations, ratio capacitance retention is 92.4%.

Claims (5)

1. the preparation method of a microporous carbon nanometer sheet, it is characterized in that: with water-soluble NaCl inorganic salt for template, glucose, sucrose or cellulosic one are carbon source, after high temperature cabonization, washing removing inorganic salt template, obtains the Two-dimensional Carbon nanometer sheet of 50 ~ 200nm thickness; Then utilize KOH to activate, obtain microporous carbon nanometer sheet.
2. the preparation method of microporous carbon nanometer sheet according to claim 1, is characterized in that: comprise the following steps:
(1) getting glucose, sucrose or cellulosic one is carbon source, with water-soluble NaCl inorganic salt for template, is dissolved in deionized water, stirs 30 ~ 60min, 80 ~ 120 DEG C of oven dry;
The quality proportioning of described carbon source and NaCl template is: 1:1 ~ 1:6; Every 1g carbon source uses the amount of deionized water to be 5 ~ 50mL;
(2) said mixture is got, at N 2under protection, 500 ~ 600 DEG C of pre-carbonization 1 ~ 3h, then by deionized water removing inorganic salt template, filter, 80 ~ 120 DEG C of dryings, obtain Two-dimensional Carbon nanometer sheet;
(3) carbon nanosheet and KOH are mixed, at N 2under protection, 700 ~ 900 DEG C of activation 1 ~ 3h, remove impurity with 0.1 ~ 2MHCl, filter, 80 ~ 110 DEG C of dryings, obtain the finished product microporous carbon nanometer sheet;
The mass ratio of described carbon nanosheet and KOH is 1:1 ~ 1:4.
3. the preparation method of microporous carbon nanometer sheet according to claim 2, is characterized in that: the mass ratio of described carbon nanosheet and KOH is 1:4.
4. the preparation method of microporous carbon nanometer sheet according to claim 1 and 2, is characterized in that: the specific surface area of the microporous carbon nanometer sheet of gained is 1756 ~ 2212m 2g -1, pore volume is 0.64 ~ 1.21cm 3g -1.
5. the preparation method of microporous carbon nanometer sheet according to claim 1 and 2, it is characterized in that: the microporous carbon nanometer sheet of gained is as the electrode materials of ultracapacitor, its chemical property is evaluated at conventional three-electrode system, platinized platinum is to electrode, saturated calomel is reference electrode, electrolytic solution is 6MKOH, is 1Ag in current density -1time, ratio capacitance reaches 221 ~ 308Fg -1.
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CN108520828A (en) * 2018-04-02 2018-09-11 桂林电子科技大学 A kind of high-graphitized more hole carbon nanosheet preparation method and application of two dimension
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CN106185921A (en) * 2016-07-06 2016-12-07 江苏大学 A kind of method and purposes preparing porous carbon materials with NaCl for hard template
CN106185923A (en) * 2016-07-06 2016-12-07 江苏大学 A kind of inorganic salt template auxiliary method preparing porous carbon nano material and application thereof
CN107473201A (en) * 2017-08-22 2017-12-15 邹远升 A kind of anti-corrosion fused salt material and its preparation method and application
CN109956479A (en) * 2017-12-25 2019-07-02 北京化工大学 A kind of hollow microsphere and preparation method thereof
CN108649242A (en) * 2018-03-21 2018-10-12 南京师范大学 The preparation method and its resulting materials of a kind of porous Pt nanometer sheets of two dimension and application
CN108520828A (en) * 2018-04-02 2018-09-11 桂林电子科技大学 A kind of high-graphitized more hole carbon nanosheet preparation method and application of two dimension
CN110386626A (en) * 2018-04-16 2019-10-29 中国科学技术大学 A kind of cobalt protoxide thin slice, preparation method and its decompose the application in water entirely in visible light catalytic
CN108751164A (en) * 2018-05-30 2018-11-06 湘潭大学 Porous carbon nanosheet of red sage petal base class graphene and its preparation method and application
CN108529596A (en) * 2018-07-20 2018-09-14 广东工业大学 A kind of preparation method of dimensional thinlayer carbon
CN108529596B (en) * 2018-07-20 2021-11-26 广东工业大学 Preparation method of two-dimensional thin-layer carbon
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