CN105502386B - A kind of preparation method of micropore carbon nanosheet - Google Patents
A kind of preparation method of micropore carbon nanosheet Download PDFInfo
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- CN105502386B CN105502386B CN201510948418.XA CN201510948418A CN105502386B CN 105502386 B CN105502386 B CN 105502386B CN 201510948418 A CN201510948418 A CN 201510948418A CN 105502386 B CN105502386 B CN 105502386B
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Abstract
The invention discloses a kind of preparation method of micropore carbon nanosheet, and it is used as the electrode material of ultracapacitor.This method is to utilize water-soluble inorganic salt NaCl to be template, and glucose, sucrose or cellulose are carbon matrix precursor；Carbon source is uniformly wrapped in after a cube NaCl crystal templates surface, high temperature cabonization, and removing NaCl templates using deionized water obtains two-dimentional carbon nanosheet；Then use after KOH high-temperature activations, plus watery hydrochloric acid removes potassium compound, it is tens nanometers of micropore carbon nanosheet to obtain high-specific surface area and thickness；As electrode material for super capacitor, with larger specific capacitance, high rate performance and excellent cyclical stability.In addition, present invention process is simple, and it is with low cost, suitable for commercial Application.
Description
Technical field
The invention belongs to new energy materialses research field, it is related 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, due to power density height, fast charging and discharging, cycle life
The series of advantages such as length, the wide, safety non-pollution of operating temperature range, in mobile communication, information technology, consumer electronics, electronic vapour
Had broad application prospects in terms of car, Aero-Space and science and techniques of defence, it is considered to be a kind of preferable electrochmical power source.It is super
The performance of capacitor depends primarily on specific surface area, pore-size distribution, microstructure and electric conductivity of electrode used therein material etc..Mesh
Before, commercialization ultracapacitor is mainly used as electrode material by the use of activated carbon.Compared to other carbon materials, absorbent charcoal material have than
Surface area is big, raw material sources are abundant, low cost and other advantages.But because the activated carbon granule of conventional method preparation is than larger（50~
200 μm）, which increase the diffusion length of electrolyte ion, so that causing the performance of capacitor reduces.
Carbon nanosheet as a species graphene-structured New Two Dimensional carbon nanomaterial, due to its have higher ratio table
Area, excellent electric conductivity, are widely used in electrochemical energy storage and electro-catalysis field.The thickness of carbon nanosheet is generally 10
Between ~ 100 nm, so as to significantly reduce the diffusion length of electrolyte ion.Compared with grapheme material, prepared by carbon nanosheet
Cost is low, is difficult to reunite, it is considered to be a kind of preferable electrode material for super capacitor.
The content of the invention
The present invention is intended to provide a kind of simple, cost is low, high-specific surface area micropore carbon nanosheet preparation method, pass through
When carbon nanosheet prepared by this method is used for electrode of super capacitor, capacitor shows good chemical property.
The invention provides a kind of preparation method of micropore carbon nanosheet, using water-soluble NaCl inorganic salts as template, grape
After sugar, one kind of sucrose or cellulose are carbon source, high temperature cabonization, washing removes inorganic salts template, obtains 50 ~ 200 nm thickness
Two-dimentional carbon nanosheet；Then activated using KOH, acquisition specific surface area is 1756 ~ 2212 m2 ·g-1, pore volume be 0.64 ~ 1.21
cm3·g-1Micropore carbon nanosheet.
The preparation method of the micropore carbon nanosheet, comprises the following steps：
（1）The one kind for taking glucose, sucrose or cellulose is carbon source, using water-soluble NaCl inorganic salts as template, is dissolved in
In ionized water, 30 ~ 60 min are stirred, in 80 ~ 120 DEG C of drying；
The quality proportioning of the carbon source and NaCl templates is：1:1~1:6；The amount that deionized water is used per 1g carbon sources is 5 ~ 50
mL；
（2）Said mixture is taken, in N2Under protection, then 500 ~ 600 DEG C of 1 ~ 3 h of pre- carbonization remove nothing with deionized water
Machine salt template, filtering, 80 ~ 120 DEG C of dryings obtain two-dimentional carbon nanosheet；
（3）Carbon nanosheet and KOH are well mixed, in N2Under protection, 700 ~ 900 DEG C of 1 ~ 3 h of activation, with 0.1 ~ 2 M
HCl removes impurity, and filtering, 80 ~ 110 DEG C of dryings obtain final products；
The mass ratio of the carbon nanosheet and KOH is 1:1~1：4.
The performance of micropore carbon nanosheet product according to obtained by the above method：The thickness of carbon nanosheet is 50 ~ 200 nm, than
Surface area has reached 1756 ~ 2212 m2 ·g-1With the cm of pore volume 0.64 ~ 1.213 ·g-1.The carbon nanosheet is used as ultracapacitor
Electrode material when, evaluate its chemical property in conventional three-electrode system, platinized platinum is that, to electrode, saturation calomel is reference electricity
Pole, electrolyte is that 6 M KOH are 1 Ag in current density-1When, specific capacitance reaches 221 ~ 308 Fg-1。
Beneficial effects of the present invention：
（1）Present invention process is simple, with low cost, suitable for commercial Application；
（2）Compared with conventional template, water-soluble inorganic salt is cheap and easily removes；
（3）The thickness of carbon nanosheet is regulated and controled by the addition of inorganic salts, shortens the diffusion length of electrolyte ion, improves
Capacitive property.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of the gained micropore carbon nanosheet of embodiment 1；
Fig. 2 is the stereoscan photograph of the gained micropore carbon nanosheet of embodiment 2；
Fig. 3 is the transmission electron microscope photo of the gained micropore carbon nanosheet of embodiment 2；
Fig. 4 is the N of micropore carbon nanosheet obtained by Examples 1 and 22The adsorption-desorption figure profile of equilibrium；
Fig. 5 is the graph of pore diameter distribution of micropore carbon nanosheet obtained by Examples 1 and 2；
Fig. 6 be Examples 1 and 2 in 6 M KOH electrolyte, sweep speed be 50 mVs-1Cyclic voltammetry it is bent
Line；
Fig. 7 is micropore carbon nanosheet obtained by Examples 1 and 2 in 1 Ag-1Charging and discharging curve；
Fig. 8 is the gained micropore carbon nanosheet of embodiment 2 in 5 Ag-13000 circulation capacitive properties of discharge and recharge.
Embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment 1（Comparative example）：
Weigh 2g glucose to add in 50 mL deionized waters, at room temperature the min of magnetic agitation 30, then in 100 DEG C of dryings
10 h；Mixture after drying is transferred in ceramic crucible, tube furnace is placed in, in N2Under protection, 500 DEG C of 2 h of carbonization；Take 1g institutes
Obtain carbon material to be sufficiently mixed with 4 g KOH stirrings, tube furnace is placed in, in N2Under protection, 800 DEG C of 1 h of carbonization；By gained carbon material
10 h in 0.1 M HCl solutions are immersed in, are filtered, in 100 DEG C of vacuum drying, micro-pore carbon material are obtained.The specific surface area of carbon material
For 927 m2g-1, pore volume is 0.31 cm3g-1。
NaCl templates are not used in the present embodiment.
After testing, using the carbon nanosheet as the electrode material of ultracapacitor, specific capacitance is in 6 M KOH electrolyte
184 F g-1(current density is 1 Ag-1)；In the Ag of current density 5-1Under, after 3000 constant current charge-discharge circulations, than
Electric capacity retention is 79.6%.
Fig. 1 shows the stereoscan photograph of micropore carbon nanosheet obtained by the present embodiment；It can be seen that without adding NaCl moulds
During plate, there is no carbon nanosheet in carbon material.
The N of micropore carbon nanosheet obtained by the present embodiment2The adsorption-desorption profile of equilibrium, pore-size distribution, cyclic voltammetry are bent
Line and charging and discharging curve refer to Fig. 4 ~ Fig. 7.
Embodiment 2
Weigh 2 g glucose and 4 g NaCl are added in 50 mL deionized waters, at room temperature the min of magnetic agitation 30, then
In 100 DEG C of dry 10 h；Mixture after drying is transferred in ceramic crucible, tube furnace is placed in, in N2Under protection, 500 DEG C of carbon
Change 2 h；Gained carbon material is immersed in 10 h in 80 DEG C of deionized waters and removes NaCl, filtering, in 100 DEG C of vacuum drying, obtains carbon
Nanometer sheet material；Take 1 g carbon nanosheets to stir with 4 g KOH to be sufficiently mixed, tube furnace is placed in, in N2Under protection, 800 DEG C of carbonizations
1 h；Gained carbon material is immersed in 10 h in 0.1 M HCl solutions, filtered, in 100 DEG C of vacuum drying, microporous carbon nanometer is obtained
Sheet material.
The specific surface area of carbon nanosheet is 2212 m2·g-1, pore volume is 1.21 cm3·g-1。
After testing, using the carbon nanosheet as the electrode material of ultracapacitor, specific capacitance is in 6 M KOH electrolyte
308 F·g-1(current density is 1 Ag-1), in the Ag of current density 5-1Under, after 3000 constant current charge-discharge circulations,
Specific capacitance retention is 95.6%.
Fig. 2 shows the stereoscan photograph of micropore carbon nanosheet obtained by the present embodiment, shows to add after NaCl templates,
Sheet carbon material structure is obtained, thickness is 50 ~ 100 nm.Transmission electron microscope photo（Fig. 3）Further demonstrate and obtain carbon nanometer
Chip architecture.
Fig. 4 ~ Fig. 7 contrasts the N for showing Examples 1 and 2 products obtained therefrom2Adsorption-desorption balances defect, pore-size distribution, followed
Ring volt-ampere test curve and charging and discharging curve figure, the surface area for showing to add acquisition carbon nanosheet material after NaCl templates reach
2212 m2·g-1, this is far above the specific surface area without the carbon material for adding NaCl templates（927 m2·g-1）.High-specific surface area
Carbon nanosheet structure result in excellent capacitive property（Fig. 6 and Fig. 7）.
Fig. 8 shows that micropore carbon nanosheet is in 5 Ag obtained by the present embodiment-13000 circulation capacitive properties of discharge and recharge, than
Electric capacity retention is 95.6%, shows that the material has good electrochemical stability.
Embodiment 3
Weigh 2 g glucose and 8 g NaCl are added in 50 mL deionized waters, at room temperature the min of magnetic agitation 30, then
In 100 DEG C of dry 10 h；Mixture after drying is transferred in ceramic crucible, tube furnace is placed in, in N2Under protection, 500 DEG C of carbon
Change 2 h；Gained carbon material is immersed in 10 h in 80 DEG C of deionized waters and removes NaCl, filtering, in 100 DEG C of vacuum drying, obtains carbon
Nanometer sheet material；Take 1 g carbon nanosheets to stir with 4 g KOH to be sufficiently mixed, tube furnace is placed in, in N2Under protection, 800 DEG C of carbonizations
1 h；Gained carbon material is immersed in 10 h in 0.1 M HCl solutions, filtered, in 100 DEG C of vacuum drying, microporous carbon nanometer is obtained
Sheet material.
The specific surface area of carbon nanosheet is 2000 m2·g-1, pore volume is 1.0 cm3·g-1。
After testing, using the carbon nanosheet as the electrode material of ultracapacitor, specific capacitance is in 6 M KOH electrolyte
288 F g-1(current density is 1 A g-1), in the A g of current density 5-1Under, after being circulated through 3000, specific capacitance retention
For 92.6%.
Embodiment 4
Weigh 2g glucose and 12g NaCl are added in 50 mL deionized waters, at room temperature the min of magnetic agitation 30, then
In 100 DEG C of dry 10 h；Mixture after drying is transferred in ceramic crucible, tube furnace is placed in, in N2Under protection, 500 DEG C of carbon
Change 2 h；Gained carbon material is immersed in 10 h in 80 DEG C of deionized waters and removes NaCl, filtering, in 100 DEG C of vacuum drying, obtains carbon
Nanometer sheet material；Take 1 g carbon nanosheets to stir with 4 g KOH to be sufficiently mixed, tube furnace is placed in, in N2Under protection, 800 DEG C of carbon
Change 1 h；Gained carbon material is immersed in 10 h in 0.1 M HCl solutions, filtered, in 100 DEG C of vacuum drying, microporous carbon is obtained and receives
Rice sheet material.The specific surface area of carbon nanosheet is 1756 m2·g-1, pore volume is 0.64 cm3·g-1.After testing, with the carbon
Nanometer sheet is as the electrode material of ultracapacitor, and specific capacitance is 221 Fg in 6 M KOH electrolyte-1(current density is
1 A· g-1), in the A g of current density 5-1Under, after being circulated through 3000, specific capacitance retention is 80.6%.
From embodiment 1 ~ 4 as can be seen that in identical carbon source（Experiment uses glucose）, identical activator（Experiment is adopted
Use potassium hydroxide）, identical quality proportioning and during identical preparation technology, NaCl templates are added using the present invention and obtain height
Specific surface area two dimension carbon nanosheet, and be not added with NaCl templates and then obtain traditional activated carbon；Prepared carbon nanosheet ratio is not added with
Activated carbon specific surface area prepared by template is from 927 m2·g-1Increase to 2212 m2·g-1, pore volume is from 0.31 cm3·g-1Increase
To 1.21 cm3·g-1.When being used as electrode of super capacitor, capacitor is being 1 A g than electric current-1When, specific capacitance is from 184 F
·g-1Increase to 308 F g-1.Show possess higher specific surface area, pore volume and more preferably using the activated carbon for preparing of the present invention
Chemical property.
Embodiment 5
Weigh 2 g sucrose and 4g NaCl are added in 30 mL deionized waters, at room temperature magnetic agitation 10 min, Ran Hou
120 DEG C of 5 h of drying；Mixture after drying is transferred in ceramic crucible, tube furnace is placed in, in N2Under protection, 600 DEG C of carbonizations 1
h；Gained carbon material is immersed in 10 h in 100 DEG C of deionized waters and removes NaCl, filtering, in 120 DEG C of vacuum drying, obtains carbon nanometer
Sheet material；Take 1 g carbon nanosheets to stir with 4 g KOH to be sufficiently mixed, tube furnace is placed in, in N2Under protection, 900 DEG C of 1 h of carbonization；
Gained carbon material is immersed in 10 h in 1 M HCl solutions, filtered, in 100 DEG C of vacuum drying, microporous carbon nanometer sheet material is obtained.
The specific surface area of carbon nanosheet is 2156 m2·g-1, pore volume is 1.16 cm3·g-1.After testing, using the carbon nanosheet as
The electrode material of ultracapacitor, specific capacitance is 298 Fg in 6 M KOH electrolyte-1(current density is 1 Ag-1),
In the Ag of current density 5-1Under, after being circulated through 3000, specific capacitance retention is 93.6%.
Embodiment 6
Weigh 2g celluloses and 4g NaCl are added in 30 mL deionized waters, at room temperature magnetic agitation 60 min, Ran Hou
120 DEG C of 10 h of drying；Mixture after drying is transferred in ceramic crucible, tube furnace is placed in, in N2Under protection, 550 DEG C of carbonizations 3
h；Gained carbon material is immersed in 10 h in 80 DEG C of deionized waters and removes NaCl, filtering, in 100 DEG C of vacuum drying, obtains carbon nanometer
Sheet material；Take 1 g carbon nanosheets to stir with 4 g KOH to be sufficiently mixed, tube furnace is placed in, in N2Under protection, 800 DEG C of 1 h of carbonization；
Gained carbon material is immersed in 8 h in 2 M HCl solutions, filtered, in 110 DEG C of vacuum drying, microporous carbon nanometer sheet material is obtained.
The specific surface area of carbon nanosheet is 2089 m2·g-1, pore volume is 1.13 cm3·g-1.After testing, using the carbon nanosheet as
The electrode material of ultracapacitor, specific capacitance is 287 Fg in 6 M KOH electrolyte-1(current density is 1 Ag-1),
In the Ag of current density 5-1Under, after being circulated through 3000, specific capacitance retention is 92.4%.
Claims (4)
1. a kind of preparation method of micropore carbon nanosheet, it is characterised in that：Using water-soluble NaCl inorganic salts as template, glucose,
One kind of sucrose or cellulose is carbon source, after high temperature cabonization, and washing removes inorganic salts template, obtains the two of 50 ~ 200 nm thickness
Tie up carbon nanosheet；Then activated using KOH, obtain micropore carbon nanosheet；
Specifically include following steps：
（1）The one kind for taking glucose, sucrose or cellulose is carbon source, using water-soluble NaCl inorganic salts as template, is dissolved in deionization
In water, 30 ~ 60 min are stirred, in 80 ~ 120 DEG C of drying；
The quality proportioning of the carbon source and NaCl templates is：1:1~1:6；The amount that deionized water is used per 1g carbon sources is 5 ~ 50 mL；
（2）Said mixture is taken, in N2Under protection, then 500 ~ 600 DEG C of 1 ~ 3 h of pre- carbonization remove inorganic salts mould with deionized water
Plate, filtering, 80 ~ 120 DEG C of dryings obtain two-dimentional carbon nanosheet；
（3）Carbon nanosheet and KOH are well mixed, in N2Under protection, 700 ~ 900 DEG C of 1 ~ 3 h of activation are removed with 0.1 ~ 2 M HCl
Decontamination, filtering, 80 ~ 110 DEG C of dryings obtain final products micropore carbon nanosheet；
The mass ratio of the carbon nanosheet and KOH is 1:1~1：4.
2. the preparation method of micropore carbon nanosheet according to claim 1, it is characterised in that：The carbon nanosheet and KOH
Mass ratio be 1：4.
3. the preparation method of micropore carbon nanosheet according to claim 1, it is characterised in that：The micropore carbon nanosheet of gained
Specific surface area be 1756 ~ 2212 m2·g-1, pore volume is 0.64 ~ 1.21 cm3·g-1。
4. the preparation method of micropore carbon nanosheet according to claim 1, it is characterised in that：The micropore carbon nanosheet of gained
As the electrode material of ultracapacitor, its chemical property is evaluated in conventional three-electrode system, platinized platinum is that saturation is sweet to electrode
Mercury is reference electrode, and electrolyte is 6 M KOH, is 1 Ag in current density-1When, specific capacitance reaches 221 ~ 308 Fg-1。
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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 |
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| 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 |
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| CN108529596B (en) * | 2018-07-20 | 2021-11-26 | 广东工业大学 | Preparation method of two-dimensional thin-layer carbon |
| CN108975308A (en) * | 2018-08-08 | 2018-12-11 | 中国林业科学研究院林产化学工业研究所 | A kind of level duct charcoal nanometer sheet and its preparation method and application |
| CN109647474B (en) * | 2018-11-12 | 2020-10-16 | 华中科技大学 | Nitrogen-doped carbon material, preparation and application thereof |
| CN109734473B (en) * | 2019-03-11 | 2021-09-28 | 福州大学 | Porous ceramic and preparation method thereof |
| CN109877342B (en) * | 2019-03-26 | 2020-08-25 | 中国科学技术大学 | Amorphous noble metal nanosheet and preparation method thereof |
| CN110078051B (en) * | 2019-04-30 | 2020-08-04 | 济宁学院 | Preparation method of carbon nanocage material |
| US11757097B2 (en) * | 2020-01-09 | 2023-09-12 | Purdue Research Foundation | Methods for producing functionalized carbon nanosheets and electrochemical energy storage cells with electrodes formed thereof |
| CN112897526A (en) * | 2021-02-05 | 2021-06-04 | 西南大学 | Preparation method and application of porous carbon dot material based on industrial glucose |
| CN114093678B (en) * | 2021-11-24 | 2023-07-14 | 滨州学院 | Preparation method of transition metal phosphide nano-sheet electrode material |
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| US8784764B2 (en) * | 2008-12-15 | 2014-07-22 | Corning Incorporated | Methods for forming activated carbon material for high energy density ultracapacitors |
| CN104876217B (en) * | 2015-06-01 | 2017-10-10 | 北京理工大学 | A kind of preparation method of graphene |
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