CN115206687A - Super-hydrophilic ionic liquid microporous-rich nanofiber electrode material and preparation method and application thereof - Google Patents
Super-hydrophilic ionic liquid microporous-rich nanofiber electrode material and preparation method and application thereof Download PDFInfo
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 55
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
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Images
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—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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- 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
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Abstract
The invention discloses a super-hydrophilic ionic liquid microporous-rich nanofiber electrode material and a preparation method and application thereof, wherein the preparation method comprises the following steps: ultrasonically dispersing carbon nano tubes in deionized water, adding a phenol source, stirring and dissolving, then adding an aldehyde source for phenolic condensation, and performing suction filtration and washing to obtain graphite carbon @ phenolic resin nano fibers with a core-shell structure; carbonizing in inert atmosphere to obtain graphite carbon @ amorphous carbon nanofiber; under inert atmosphere, mixing graphite carbon @ amorphous carbon nanofiber and an activating agent, and carbonizing and activating to obtain the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material. According to the electrode material provided by the invention, the conductivity and electrochemical properties of the material are synergistically improved by the conductive inner core carbon nano tube and the in-situ doped nitrogen atom, and the microporous carbon fiber has a super-hydrophilic liquid surface and shows high specific capacitance, high specific energy density, excellent rate capability and cycling stability when being used as a super capacitor electrode material.
Description
Technical Field
The invention relates to the technical field of electrochemical energy storage, in particular to a super-hydrophilic ionic liquid microporous-rich nanofiber electrode material and a preparation method and application thereof.
Background
In order to adapt to the development of modern intelligent electronic equipment, a super capacitor with high specific energy density and high specific power density is designed. As a member of carbon family, the one-dimensional carbon nanotube has high mechanical strength and excellent conductivity, can realize rapid axial electron transmission in a supercapacitor, and shows high frequency response; however, their specific surface area is generally below 1000m 2 g -1 And rarely simply used as a capacitor electrode material. Meanwhile, the surface of the one-dimensional carbon nanofiber has rich defect active sites, rapid radial ion diffusion can be realized in the supercapacitor, and excellent electrode/electrolyte interface wettability is shown. Therefore, in the prior art, a composite structure of carbon nanotubes and carbon nanofibers is mostly adopted, so that efficient electron ion double conduction can be met in the charging and discharging processes, however, the problem of low compaction density of the carbon nanofibers used as electrode materials of the super capacitor generally exists.
At present, carbon nanofibers are mainly obtained by a template method and an electrospinning method. The group of subjects of the remaining teachers (Small 2019, 1904310) uses resorcinol and formaldehyde as carbon sources and tetraethyl silicate as silicon sources to assemble on carbon nanotubes to obtain composite carbon nanofibers, wherein the silicon template needs to be removed by subsequent etching. The Suzuki teacher topic group (Sci. Bull.2019,64, 1617-1624) uses hexadecyl trimethyl ammonium bromide as a soft template and inducer, and carries out hydrothermal reaction at 85 ℃ to obtain carbon nanofibers, and the specific capacitance is 380 Fg under the current density of 1A g-1 in 6M KOH electrolyte -1 The energy density is 12.4Wh kg -1 The power density is 130W kg -1 . However, both the soft template method and the hard template method involve the preparation cost and the removal cost of the template, and the process is tedious, time-consuming and labor-consuming. Project group of building official literature (Energy environ. Sci.,2017,10, 1777-1783) embedding imidazole molecular sieve in polyacrylonitrile by electrospinning to obtain porous carbon nanofiber, H2M 2 SO 4 In an electrolyte，1A g -1 The specific capacity under the current density is 307 Fg -1 The energy density is 10.96W h kg -1 The power density is 25000W kg -1 However, the method has the advantages of complex synthesis, low spinning efficiency, high cost and large pollution, and is not suitable for large-scale popularization.
Based on the design, the design and synthesis of the composite carbon nanofiber electrode material with a simple synthesis strategy, high compaction density and high electrochemical performance have important significance.
Disclosure of Invention
In view of the above, the invention provides a super-hydrophilic ionic liquid microporous-rich nanofiber electrode material, and a preparation method and an application thereof, so as to solve the problems of low compaction density and poor electrochemical performance when the existing composite carbon nanofiber acts on an electrode.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a super-hydrophilic ionic liquid microporous-rich nanofiber electrode material comprises the following steps:
s1, ultrasonically dispersing carbon nano tubes in deionized water, adding a phenol source, stirring and dissolving, then adding an aldehyde source for phenolic condensation, and performing suction filtration and washing to obtain graphite carbon @ phenolic resin nano fibers with a core-shell structure;
s2, carbonizing the graphite carbon @ phenolic resin nano fiber in an inert atmosphere to obtain graphite carbon @ amorphous carbon nano fiber;
and S3, mixing the graphite carbon @ amorphous carbon nanofiber with an activating agent in an inert atmosphere, and carbonizing and activating to obtain the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material.
According to the scheme, in the step S1, the mass ratio of the carbon nano tube to the phenol source to the aldehyde source is (0.005-0.05): 1:1.5.
according to the scheme, the phenol source comprises one of m-aminophenol, o-aminophenol and p-aminophenol, and the aldehyde source comprises formaldehyde or acetaldehyde.
According to the scheme, in the step S1, the reaction temperature of the phenolic aldehyde condensation reaction is 20-100 ℃, and the reaction time is 10-60min.
According to the scheme, in the step S2, the carbonization conditions comprise: 500-1400 deg.C, carbonization time 100-200min, and heating rate 2-10 deg.C for min -1 。
According to the scheme, in the step S3, the mass ratio of the carbon nano fiber to the activating agent is in the range of 1.
According to the scheme, the activating agent comprises potassium hydroxide or potassium bicarbonate.
According to the scheme, in the step S3, the carbonization and activation conditions comprise: the activation temperature is 700-800 deg.C, the activation time is 60-180min, and the heating rate is 2-5 deg.C for min -1 。
On the basis of the scheme, the second purpose of the invention is to provide a super-hydrophilic ionic liquid microporous nanofiber electrode material which is prepared by the preparation method of the super-hydrophilic ionic liquid microporous nanofiber electrode material.
On the basis of the scheme, the third purpose of the invention is to provide the application of the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material as a super capacitor active material.
Compared with the prior art, the invention has the following advantages:
(1) The super-hydrophilic ionic liquid microporous-rich nanofiber electrode material has a compact 3D framework and high compaction density, and can realize rapid electron ion double conduction by taking the carbon nanotube as a conductive inner core and the microporous-rich carbon as a capacitor shell; meanwhile, the carbon fiber rich in micropores has a super-ionophilic liquid surface, the contact angle is almost zero, and the size of the micropores is slightly larger than the size of ions in an ionic liquid electrolyte, so that the carbon fiber has high specific capacitance, high specific energy density, excellent rate capability and cycle stability when being used as an electrode material of a super capacitor.
(2) The preparation method provided by the invention is simple to operate, short in preparation time, low in cost, simple and green in synthesis process, and free from template removal; in addition, the reaction is carried out in a pure water system, no organic solvent is added, and the method is suitable for industrial production.
Drawings
In order to more clearly illustrate the present invention or the technical solutions in the prior art, some figures needed to be used in the embodiments or the description in the prior art will be briefly described below, and it is obvious that the figures in the following description are some embodiments of the present invention, and other figures can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a diagram of a synthetic mechanism of the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material;
FIG. 2 is SEM (a) and TEM (b, c) of core-shell structure graphite carbon @ phenolic resin nanofiber, SEM (d) and TEM (e, f) of core-shell structure graphite carbon @ amorphous nitrogen-doped carbon nanofiber, SEM (g) and TEM (h, i) of super-hydrophilic ionic liquid microporous-rich nanofiber and EDS (j) of example 1 of the present invention;
FIG. 3 is an XRD pattern of nitrogen-doped porous carbon materials according to examples 1, 2 and 3 of the present invention;
FIG. 4 is a Raman spectrum of a nitrogen-doped porous carbon material according to examples 1, 2 and 3 of the present invention;
FIG. 5 is a graph showing adsorption/desorption curves and pore size distribution curves of nitrogen-doped porous carbon materials according to examples 1, 2 and 3 of the present invention;
FIG. 6 is an XPS spectrum of the electrode material of the super-hydrophilic ionic liquid microporous-rich nanofiber according to example 1 of the present invention;
FIG. 7 is a graph showing wettability tests of nitrogen-doped porous carbon materials according to examples 1, 2 and 3 of the present invention;
FIG. 8 is a cyclic voltammogram of the electrode material of the microporous-rich nanofiber with super-hydrophilic ionic liquid according to example 1 of the present invention;
FIG. 9 is a cyclic voltammogram of the nitrogen-doped porous carbon materials according to examples 1, 2 and 3 of the present invention;
FIG. 10 is a charge-discharge curve diagram of the super-philic ionic liquid microporous-rich nanofiber electrode material in example 1 of the present invention at different current densities;
FIG. 11 is a graph showing the rate curves of nitrogen-doped porous carbon materials according to examples 1, 2 and 3 of the present invention;
FIG. 12 is a cycle curve of the superhydrophilic ionic liquid microporous-rich nanofiber electrode material described in example 1 of the present invention;
fig. 13 is SEM images (a, d) of phenolic resin microspheres, nitrogen-doped carbon microspheres, and microporous nitrogen-doped carbon microspheres according to example 3 of the present invention;
FIG. 14 is a graph showing the charge and discharge curves of the carbon nanotubes after carbonization and activation according to example 4 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
It should be noted that in the description of the embodiments herein, the description of the term "some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Throughout this specification, the schematic representations of the terms used above do not necessarily refer to the same implementation or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The term "in.
The embodiment of the invention provides a preparation method of a super-hydrophilic ionic liquid microporous-rich nanofiber electrode material, which comprises the following steps:
s1, ultrasonically dispersing carbon nano tubes in deionized water in a pure water system, adding a small amount of phenol source, stirring and dissolving, then adding an aldehyde source for phenolic condensation, and performing suction filtration and washing to obtain gray graphite carbon @ phenolic resin nano fibers with a core-shell structure;
s2, carbonizing the graphite carbon @ phenolic resin nanofiber with the core-shell structure in one step in an inert atmosphere to obtain black graphite carbon @ amorphous carbon nanofiber with the core-shell structure;
and S3, mixing the black core-shell structure graphite carbon @ amorphous carbon nanofiber with an activating agent in an inert atmosphere, and carbonizing and activating to obtain the black core-shell structure graphite carbon @ microporous carbon-rich nanofiber, namely the super-hydrophilic ionic liquid microporous carbon-rich nanofiber electrode material.
With reference to fig. 1, the synthesis mechanism of the super-philic ionic liquid microporous nanofiber electrode material is as follows: the carbon nano tube modified by the surface oxygen functional group can be uniformly dispersed in an aqueous solution due to the action of a hydrogen bond, when m-aminophenol and formaldehyde are added, the uniformly dispersed carbon nano tube modified by the surface oxygen functional group can be used as a heterogeneous nucleation site to effectively reduce a phenolic condensation nucleation barrier, and under the action of the hydrogen bond, the graphite carbon @ phenolic resin nano fiber with a core-shell structure is grown along the surface of the carbon nano tube in a coating manner; because the surface of the fiber is rich in amino and hydroxyl functional groups, the three-dimensional fiber framework is compressed to become dense under the action of hydrogen bond acting force in the carbonization process, and finally, the compressed microporous-rich three-dimensional carbon framework nanofiber electrode material can be obtained through activation.
Specifically, in step S1, the mass ratio of the carbon nanotubes, the phenol source and the aldehyde source is (0.005-0.05): 1.5. The phenol source comprises one of m-aminophenol, o-aminophenol and p-aminophenol, and the aldehyde source comprises formaldehyde or acetaldehyde. Further, the phenol source is preferably m-aminophenol, and the aldehyde source is preferably formaldehyde.
Wherein, in order to improve the reaction efficiency, the reaction temperature of the phenolic aldehyde condensation reaction is 20-100 ℃, and the reaction time is 10-60min.
The core-shell structure is a microporous nano structure, so that the specific surface area is greatly improved, and the wettability between the electrolyte and the electrode material is improved; in addition, the core-shell structure forms a three-dimensional interweaving net structure, which is beneficial to the rapid transmission of electrons and ions in the electrode material in the oxygen reduction process, and further improves the specific capacitance of the electrode material.
Specifically, in step S2, the conditions of the one-step carbonization include: 500-1400 deg.C, carbonization time 100-200min, and heating rate 2-10 deg.C for min -1 . Preferably, the carbonization temperature is 800 ℃, the carbonization time is 120min, and the heating rate is 2 ℃ for min -1 。
The doping of nitrogen element can improve the active site and show better performance, and the conductivity and electrochemical performance of the material are improved by the cooperation of the conductive core carbon nano tube and the in-situ doped nitrogen atom.
In step S3, the mass ratio of the carbon nanofibers to the activator is in the range of 1.
Further, the carbonization activation conditions include: the activation temperature is 700-800 deg.C, the activation time is 60-180min, and the heating rate is 2-5 deg.C for min -1 . Preferably, the activation temperature is 750 deg.C, the activation time is 120min, and the heating rate is 3 deg.C for min -1 。
Therefore, the preparation process provided by the invention is simple and green, a template does not need to be removed, and the cost is low; in addition, the reaction is carried out in a pure water system, no organic solvent is added, and the method is suitable for industrial production.
On the basis of the scheme, the invention further provides a super-hydrophilic ionic liquid microporous nanofiber electrode material which is prepared by adopting the preparation method of the super-hydrophilic ionic liquid microporous nanofiber electrode material.
On the basis of the scheme, the invention further provides an application of the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material as a super capacitor active material.
The super-hydrophilic ionic liquid microporous-rich nanofiber electrode material provided by the invention has a compact 3D framework and high compaction density, the carbon nanotube is used as a conductive core, the microporous carbon is used as a capacitor shell, the conductivity and the electrochemistry of the material are improved by the carbon nanotube of the conductive core and the nitrogen atom doped in situ in a synergistic manner, and the rapid electron ion double conduction can be realized; meanwhile, the carbon fiber rich in micropores has developed micropores and mesopores, the size of the micropores is slightly larger than the size of ions in the ionic liquid electrolyte, the contact angle with the electrolyte is almost zero, and the carbon fiber has a super-hydrophilic ionic liquid surface and shows high specific capacitance, high specific energy density, excellent rate capability and stable cycle performance when used as an electrode material of a super capacitor.
On the basis of the above embodiments, the present invention is further illustrated by the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by mass.
Example 1
The embodiment provides a preparation method of a super-hydrophilic ionic liquid microporous-rich nanofiber electrode material, which comprises the following steps:
1) Dispersing 25mg of carbon nano tube in 300mL of deionized water, adding 2.475g of m-aminophenol to dissolve, adding 3.42mL of formaldehyde to react for 0.5h, and obtaining gray core-shell structure graphite carbon @ phenolic resin nano fiber (CNT @ APF) after suction filtration, washing and drying;
2) Carbonizing dried CNT @ APF at 800 deg.C for 2h under nitrogen atmosphere, and heating at 2 deg.C for min -1 Obtaining black core-shell structure graphite carbon @ amorphous nitrogen-doped carbon nanofiber (CNT @ NC);
3) Mixing CNT @ NC and KOH according to the mass ratio of 1 -1 Washing the activated sample with dilute hydrochloric acid to remove impurities, and then washing with water to be neutral to obtain the super-hydrophilic ionic liquid microporous nanofiber electrode material-black core-shell structure graphite carbon @ microporous nitrogen-rich doped carbon nanofiber (CNT @ NC-A).
Example 2
The embodiment provides a preparation method of a nanofiber electrode material, which comprises the following steps:
1) Dispersing 25mg of carbon nano tube in 300mL of deionized water, adding 2.475g of m-aminophenol to dissolve, adding 3.42mL of formaldehyde to react for 0.5h, and obtaining gray core-shell structure graphite carbon @ phenolic resin nano fiber (CNT @ APF) after suction filtration, washing and drying;
2) Carbonizing dried CNT @ APF at 800 deg.C for 2h under nitrogen atmosphere, and heating at 2 deg.C for min -1 Obtaining black graphite carbon @ amorphous nitrogen-doped carbon nanofiber (CNT @ NC) with a core-shell structure.
The difference between the electrode material prepared in this embodiment and the electrode material prepared in embodiment 1 is that the graphite carbon @ amorphous nitrogen-doped carbon nanofiber with the core-shell structure is not activated by potassium hydroxide.
Example 3
The embodiment provides a preparation method of a nanofiber electrode material, which comprises the following steps:
1) Adding 2.475g of m-aminophenol into 300mL of deionized water, dissolving, adding 3.42mL of formaldehyde, reflecting for 0.5h, and obtaining yellow phenolic resin microspheres (APF) after suction filtration, washing and drying;
2) Carbonizing the dried APF at 800 deg.C for 2h under nitrogen atmosphere, and heating at 2 deg.C for min -1 Obtaining black nitrogen-doped carbon microspheres (NCS);
3) Mixing NCS and KOH according to the mass ratio of 1 -1 And washing the activated sample with dilute hydrochloric acid to remove impurities, and then washing the sample with water to be neutral to obtain the black microporous nitrogen-doped carbon microsphere (NCS-A).
By taking the microporous nanofiber electrode material prepared in example 1 as an example, morphology and structure characterization were performed on CNT @ APF, CNT @ NC and CNT @ NC-A, and the result graphs shown in FIGS. 2-7 were obtained.
FIG. 2 shows SEM and TEM images (se:Sub>A, b, c) of CNT @ APF, SEM and TEM images (d, f) of CNT @ NC, SEM and TEM images (g, h, i) of CNT @ NC-A, and EDS spectrum (j), and it can be seen from FIG. 2 that the synthesized graphitic carbon @ phenolic resin nanofiber CNT @ APF is in se:Sub>A cross-linked state, the fiber size is about 60nm, the diameter of the core layer carbon nanotube is 5-10nm, and the three-dimensional network porosity is large at this time. In the carbonization process, adjacent fibers approach each other under the action of hydrogen bond, the occupation ratio of useless cavities is reduced, the network compactness is improved, and the fiber diameter is slightly reduced. After the activation treatment, the fiber diameter does not change much due to the excellent thermal stability and etching resistance of the phenolic resin-based carbon, but a rich microporous structure is formed inside the fiber. The C and O elements are uniformly distributed on the fiber, and the N elements are distributed relatively less at the carbon nano tube, so that the distribution of the carbon nano tube in the fiber is reflected.
To further illustrate the effect of the addition of carbon nanotubes on the superhydrophilic ionic liquid microporous nanofiber electrode material, the data in table 1 were obtained by comparing the synthesis yield, carbonization yield, and activation yield of porous carbon spheres and porous carbon fibers.
TABLE 1 yield table for nitrogen-doped porous carbon materials
As can be seen from Table 1, the addition of trace amount of carbon nanotubes not only increases the conductivity of the material and induces the transformation of the nucleation growth of the resin from three-dimensional to one-dimensional, but also improves the yield of the precursor, increases the heat stability and the etching resistance of the resin material, and improves the yield of the final product of the porous carbon fiber (CNT @ NC-A) by 43.1% relative to the porous carbon sphere (NCS-A) under the same conditions.
FIG. 3 is an XRD pattern of nitrogen-doped porous carbon materials described in examples 1, 2 and 3, and it can be seen from FIG. 3 that two large peaks at 24 ° and 43 ° for CNT @ NC-A prepared in example 1, CNT @ NC-A prepared in example 2 and NCS-A prepared in example 3 correspond to diffraction of amorphous carbon at (002) and (100) crystal planes, illustrating the amorphous structure. The diffraction peak intensities of NCS-A and CNT @ NC-A subjected to activation treatment were reduced relative to CNT @ NC.
FIG. 4 is se:Sub>A Raman diagram of nitrogen-doped porous carbon materials described in examples 1, 2 and 3, and it can be seen from FIG. 4 that CNT @ NC-A prepared in example 1 and CNT @ NC prepared in example 2 were 1360cm in 1360cm -1 And 1580cm -1 Corresponding to the amorphous peak and graphitization peak typical of carbon material, wherein the G peak intensity is high due to the existence of carbon nano tube and is 2700cm -1 There is a typical 2D peak. NCS-A prepared in example 3 was found to be 1360cm -1 And 1580cm -1 The ratio of the amorphous peak (D peak) to the graphitized peak (G peak) corresponding to the typical carbon material is about 1 due to the absence of the carbon nanotubes, which indicates that the activated material has a certain graphitization degree while maintaining an amorphous structure.
FIG. 5 is se:Sub>A graph showing the absorption/desorption curves and pore size distribution curves of the nitrogen-doped porous carbon materials of examples 1, 2 and 3, and it can be seen from FIG. 5 that the specific surface arese:Sub>A of the CNT @ NC-A material prepared in example 1 reaches 2059m2g -1 The pore volume of the micropores was 0.69cm3g -1 Has abundant micropore and mesoporous structures, the micropore size is slightly larger than the ion size in the ionic liquid electrolyte,all the pore channels are ion accessible effective pores. The specific surface area of the CNT @ NC material prepared in example 2 reaches 358m 2g -1 The pore volume of the micropores was 0.04cm 3g -1 This indicates that the micropores were not developed without activation. The specific surface arese:Sup>A of the NCS-A material prepared in example 3 reaches 770m2g -1 The micropore volume of the porous glass is 0.24cm3g -1 And has abundant micropores.
FIG. 6 is an XPS spectrum of the electrode material CNT @ NC-A of the super-hydrophilic ionic liquid microporous-rich nanofiber prepared in example 1, and as can be seen from FIG. 6, the material CNT @ NC-A has the compositions of C (91.80 at.%), N (3.24 at.%), and O (4.96 at.%), the electrochemical performance is greatly improved due to the high nitrogen content, and in addition, through peak separation fitting, N species mainly exist in the form of pyrrole nitrogen.
FIG. 7 and FIG. 9 are cyclic voltammograms of wettability testing graphs of nitrogen-doped porous carbon materials described in examples 1, 2 and 3, respectively, and it can be seen from FIG. 7 that the initial contact angle of the CNT @ NC-A material prepared in example 1 in contact with the electrolyte is 39.6 degrees, the contact angle after 4min is 0 degrees, the material is in se:Sub>A completely wetted state, and good interface wettability greatly facilitates the exertion of electrochemical properties. The initial contact angle of the cnt @ nc material prepared in example 2 in contact with the electrolyte was 59.9 °, and the contact angle did not change much after 4min, indicating that the electrode material of this example is intrinsically wet with the electrolyte, but shows less than ideal capacitance performance due to less developed micropores and limited wettability (fig. 9). The initial contact angle of the NCS-se:Sup>A material prepared in example 3 in contact with the electrolyte was 85.3 °, and the contact angle after 4min was 58.0 °, indicating that the electrode material of this example is wet with the electrolyte by nature, but shows inferior capacitance performance to that of example 1 because the spherical structure is inferior in wettability with the electrolyte to the three-dimensional network structure and the specific surface arese:Sup>A is small (fig. 9).
The application of the super-hydrophilic liquid microporous-rich carbon nanofiber electrode material prepared in example 1 as a supercapacitor electrode material is as follows: the electrode slice is manufactured by adopting super-hydrophilic liquid microporous carbon nanofiber as an active material, acetylene black as a conductive agent and PTFE as a binder in a mass ratio of 8:1:1 mixing in mortar, pressing into electrode sheet, and separatingSeed liquid EMIMBF 4 And a cellulose diaphragm is adopted as an electrolyte to assemble the button cell. By analogy, the electrode materials prepared in examples 2 and 3 were also assembled into batteries. Electrochemical testing was performed on the assembled button cells, respectively, to obtain the results shown in fig. 8-12.
FIG. 8 is se:Sub>A cyclic voltammetry graph of the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material CNT @ NC-A prepared in example 1, and it can be seen from FIG. 8 that the super-hydrophilic ionic liquid microporous-rich carbon nanofiber shows se:Sub>A rectangular-like shape at different scanning speeds, indicating the electrochemical capacitance behavior thereof.
FIG. 9 is se:Sub>A cyclic voltammogram of the nitrogen-doped porous carbon materials described in examples 1, 2 and 3, and it can be seen from FIG. 9 that the capacitance of the CNT @ NC-A assembled battery prepared in example 1 is much higher than that of the CNT @ NC-assembled battery prepared in example 2 with activation, and higher than that of the NCS-A prepared in example 3 without adding carbon nanotubes, in terms of cyclic voltammogram arese:Sub>A.
FIGS. 10 and 12 are the charge-discharge curve and the cycle curve of the super-philic ionic liquid microporous nanofiber electrode material CNT @ NC-A prepared in example 1 at different current densities, respectively, and it can be seen from FIG. 10 that at 1 Ag -1 Under the current density, the super-hydrophilic liquid microporous-rich carbon nanofiber has the weight of 219F g -1 Specific capacitance of 10 ag -1 At current densities of (a) and (b), the capacity retention after 20000 cycles was as high as 95% (fig. 12), thanks to the good wettability of the electrode/electrolyte interface. According to a further conversion, the energy density is 108.8Wh kg -1 The power density can reach 946.3W kg -1 。
FIG. 11 is se:Sub>A graph showing the rate curves of nitrogen-doped porous carbon materials described in examples 1, 2 and 3. From FIG. 11, it can be seen that the CNT @ NC-A battery prepared in example 1 is at 50 ag -1 The specific capacitance under the current density is still as high as 160 Fg -1 Much higher than the cnt @ nc cell prepared in example 2 and the NCS-se:Sup>A cell prepared in example 3, the superior rate performance benefits from nitrogen doping and the efficient electron-ion double conduction of the structure.
Fig. 13 is SEM pictures (se:Sup>A, d) of the APF of the phenolic resin microsphere described in example 3, SEM pictures (b, e) of the NCS, and SEM pictures (c, f) of the NCS-se:Sup>A, and it can be seen from fig. 13 that the phenolic resin microsphere is se:Sup>A monodisperse microsphere with se:Sup>A diameter of 600nm, se:Sup>A small molecule precursor escapes during carbonization, the resin shrinks to obtain se:Sup>A monodisperse carbon microsphere with se:Sup>A diameter of 500nm, and the nitrogen-doped carbon microsphere remains in se:Sup>A stable monodisperse state under the etching action of alkali during activation, and the size is 450nm.
In conclusion, the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material prepared by the method has the advantages that the size of the microporous carbon fiber is 40nm, and the specific surface area can reach 2059m2g -1 The prepared electrode sheet has the surface density of 2.6g cm -2 The ionic liquid electrolyte has excellent wettability (theta-0 DEG) to the ionic liquid electrolyte, and shows high specific capacitance, high specific energy-power density, excellent rate capability and stable cycle performance when being used as a super capacitor electrode material.
Example 4
The embodiment provides a preparation method of a carbon nanotube, which comprises the following steps:
dispersing 100mg of carbon nano tubes in 1200mL of deionized water, filtering, washing, drying, carbonizing at 800 ℃ for 2h in nitrogen atmosphere, and raising the temperature rate at 2 ℃ for min -1 And then mixing the activated carbon powder with KOH according to the mass ratio of 1 -1 . The activated sample was washed with dilute hydrochloric acid to remove impurities, and then washed with water to neutrality, resulting in black activated carbon nanotubes (CNT-a).
FIG. 14 is a graph showing the charge and discharge curves of the carbon nanotube CNT-A after the carbonization and activation in example 4, as seen from FIG. 14, at 1 Ag -1 Under the current density, the specific capacitance of the activated carbon nano tube is 25.2 Fg -1 Exhibiting extremely limited capacitive performance.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (10)
1. A preparation method of a super-hydrophilic ionic liquid microporous-rich nanofiber electrode material is characterized by comprising the following steps:
s1, ultrasonically dispersing carbon nano tubes in deionized water, adding a phenol source, stirring and dissolving, then adding an aldehyde source for phenolic condensation, and performing suction filtration and washing to obtain graphite carbon @ phenolic resin nano fibers with a core-shell structure;
s2, carbonizing the graphite carbon @ phenolic resin nanofiber in an inert atmosphere to obtain graphite carbon @ amorphous carbon nanofiber;
and S3, mixing the graphite carbon @ amorphous carbon nanofiber with an activating agent in an inert atmosphere, and carbonizing and activating to obtain the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material.
2. The production method according to claim 1, wherein in step S1, the mass ratio of the carbon nanotube, the phenol source, and the aldehyde source is (0.005-0.05): 1:1.5.
3. the method of claim 1 or 2, wherein the phenol source comprises one of m-aminophenol, o-aminophenol and p-aminophenol, and the aldehyde source comprises formaldehyde or acetaldehyde.
4. The method according to claim 3, wherein in step S1, the reaction temperature of the phenolic aldehyde condensation reaction is 20 to 100 ℃ and the reaction time is 10 to 60min.
5. The production method according to claim 1, wherein in step S2, the carbonization conditions include: the carbonization temperature is 500-1400 ℃, the carbonization time is 100-200min, and the heating rate is 2-10 ℃ for min -1 。
6. The production method according to claim 1, wherein in step S3, the mass ratio of the carbon nanofibers and the activating agent is in the range of 1.
7. The method of claim 6, wherein the activator comprises potassium hydroxide or potassium bicarbonate.
8. The production method according to claim 6, wherein in step S3, the carbonization activation conditions include: the activation temperature is 700-800 deg.C, the activation time is 60-180min, and the heating rate is 2-5 deg.C for min -1 。
9. A super-hydrophilic ionic liquid microporous nanofiber electrode material, which is characterized by being prepared by the preparation method of the super-hydrophilic ionic liquid microporous nanofiber electrode material as claimed in any one of claims 1-8.
10. The application of the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material obtained by the preparation method according to any one of claims 1-8 or the super-hydrophilic ionic liquid microporous-rich nanofiber electrode material according to claim 9 as an active material of a super capacitor.
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