CN110265646B - Nitrogen-doped graphene-like activated carbon material and preparation method and application thereof - Google Patents
Nitrogen-doped graphene-like activated carbon material and preparation method and application thereof Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention relates to a nitrogen-doped graphene-like activated carbon material and a preparation method and application thereof, belonging to the technical field of materials, wherein the preparation method of the material comprises the following steps: the preparation method comprises the steps of mixing melamine and L-cysteine, carrying out ball milling to obtain a precursor, carbonizing the precursor in an inert atmosphere, and cooling to room temperature to obtain the nitrogen-doped graphene-like activated carbon material, wherein the nitrogen-doped graphene-like activated carbon material which is large in specific surface area, specific in pore volume and chemical bond composition can be obtained by reasonably regulating the mass ratio of the melamine to the L-cysteine in the preparation process. The lithium-sulfur battery based on the material has long cycle stability, excellent rate capability and high charge-discharge reversible specific capacity. The material has simple preparation process, easy operation and low cost, is suitable for industrial production and has great commercial prospect.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a nitrogen-doped graphene-like activated carbon material and a preparation method and application thereof.
Background
Due to its ultra-high theoretical specific capacity (1675mAh/g) and energy density (2600 Wh/kg), lithium sulfur batteries are considered to be one of the most promising new generation energy storage systems. In addition, the active substance sulfur in the lithium-sulfur battery also has the advantages of rich source, low price, environmental friendliness and the like. However, there are still a series of problems that seriously impede the commercialization of lithium sulfur batteries. First, the active material sulfur and the discharge product Li of the battery 2 Poor S conductivity results in low utilization of sulfur and reduced reaction kinetics. Secondly, polysulfide intermediate product in the charging and discharging process has high solubility in electrolyte, so that the polysulfide shuttles back and forth between the anode and the cathode of the battery in the charging and discharging process to cause a shuttle effect, which not only reduces the coulombic efficiency of the battery, but also reduces the coulombic efficiency of the battery when the polysulfideShuttling to the negative electrode can also react with lithium metal, affecting the reactivity of the negative electrode. To this end, many solutions have been devised to overcome these difficulties, such as: protecting the metal lithium cathode, modifying the diaphragm, and adding additives and the like into the electrolyte. In addition to this, a great deal of work has been focused on the preparation of positive electrode materials. Loading sulfur into different cathode materials is considered to be the most effective in slowing down the shuttle effect and improving the performance of the battery.
In recent years, carbon materials have attracted much attention because of their excellent electrical conductivity, good mechanical ductility, abundant pore structures, and adjustable specific surface area. Although the physical interaction between the carbon material and polysulfide is weak, pure carbon material cannot inhibit the occurrence of shuttle effect, and the most used carrier material is carbon material with nano structure at present, the interaction between the carbon material and polysulfide can be effectively improved by increasing the specific surface area, controlling the pore structure, introducing hetero atoms into the carbon skeleton, and the like.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a nitrogen-doped graphene-like activated carbon material; the second purpose is to provide a nitrogen-doped graphene-like activated carbon material; the third purpose is to provide the application of the nitrogen-doped graphene-like activated carbon material as a lithium-sulfur battery positive electrode material.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a preparation method of a nitrogen-doped graphene-like activated carbon material comprises the following steps:
and mixing melamine and L-cysteine, performing ball milling to obtain a precursor, further carbonizing in an inert atmosphere, and cooling to room temperature to obtain the nitrogen-doped graphene-like activated carbon material.
Preferably, the mass ratio of the melamine to the L-cysteine is 1-10: 1.
Preferably, the time for ball milling is 2-10 h.
Preferably, the inert atmosphere is one or more of argon, nitrogen, helium or neon.
Preferably, the cooling to room temperature after carbonization is specifically to heat up to 600-1500 ℃ at the rate of 1-5 ℃/min, then keep for 1-3h, and then cool down to room temperature at the rate of 1-5 ℃/min.
2. The nitrogen-doped graphene-like activated carbon material prepared by the method.
3. The nitrogen-doped graphene-like activated carbon material is applied as a lithium-sulfur battery positive electrode material.
The invention has the beneficial effects that: the invention provides a nitrogen-doped graphene activated carbon material and a preparation method and application thereof. In addition, the S-containing functional group in the L-cysteine can promote the formation of a C-S-C bond between the melamine and the L-cysteine, can also serve as a template to enable the final product to contain rich pore structures, and can obtain the nitrogen-doped graphene activated carbon material with large specific surface area, specific pore volume and chemical bond composition by reasonably regulating and controlling the mass ratio of the melamine to the L-cysteine in the preparation process. The lithium-sulfur battery based on the material has long cycle stability, excellent rate capability and high charge-discharge reversible specific capacity. The material has simple preparation process, easy operation and low cost, is suitable for industrial production and has great commercial prospect.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For a better understanding of the objects, aspects and advantages of the present invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
fig. 1 is a scanning electron microscope image of the nitrogen-doped graphene-like activated carbon material obtained in example 1; (in FIG. 1, a is a scanning electron micrograph at 10000 times magnification, and in FIG. 1, b is a scanning electron micrograph at 30000 times magnification)
Fig. 2 is a transmission electron microscope image of the nitrogen-doped graphene-like activated carbon material obtained in example 1;
fig. 3 is an XRD spectrum of the nitrogen-doped graphene-like activated carbon material obtained in example 1;
fig. 4 is a Raman spectrum of the nitrogen-doped graphene-like activated carbon material obtained in example 1;
fig. 5 is a graph showing adsorption and desorption curves of the nitrogen-doped graphene-like activated carbon material obtained in example 1;
fig. 6 is a pore size distribution diagram of the nitrogen-doped graphene-like activated carbon material obtained in example 1;
fig. 7 is an XPS spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 1; (a in FIG. 7 is a surface element analysis full spectrum of the nitrogen-doped graphene-based activated carbon material, b in FIG. 7 is a high-resolution C1s spectrum of the nitrogen-doped graphene-based activated carbon material, C in FIG. 7 is a high-resolution N1s spectrum of the nitrogen-doped graphene-based activated carbon material, and d in FIG. 7 is a high-resolution O1s spectrum of the nitrogen-doped graphene-based activated carbon material)
Fig. 8 is a scanning electron microscope image of the nitrogen-doped graphene-based activated carbon material obtained in example 2; (in FIG. 8, a is a scanning electron microscope image magnified 10000 times and b is a scanning electron microscope image magnified 30000 times)
Fig. 9 is a transmission electron microscope photograph of the nitrogen-doped graphene-like activated carbon material obtained in example 2;
fig. 10 is an XRD spectrum of the nitrogen-doped graphene-like activated carbon material obtained in example 2;
fig. 11 is a nitrogen adsorption/desorption graph and a pore size distribution graph of the nitrogen-doped graphene-based activated carbon material obtained in example 2; (in FIG. 11, a is a nitrogen adsorption/desorption graph, and in FIG. 11, b is a pore diameter distribution graph)
Fig. 12 is an XPS spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 2; (a in FIG. 12 is a surface element analysis full spectrum of the nitrogen-doped graphene-based activated carbon material, b in FIG. 12 is a high-resolution C1s spectrum of the nitrogen-doped graphene-based activated carbon material, C in FIG. 12 is a high-resolution N1s spectrum of the nitrogen-doped graphene-based activated carbon material, and d in FIG. 12 is a high-resolution O1s spectrum of the nitrogen-doped graphene-based activated carbon material)
Fig. 13 is a scanning electron microscope photograph of the nitrogen-doped graphene-like activated carbon material obtained in example 3; (in FIG. 13, a is a scanning electron micrograph at 10000 times magnification, and in FIG. 13, b is a scanning electron micrograph at 30000 times magnification)
Fig. 14 is a transmission electron microscope photograph of the nitrogen-doped graphene-like activated carbon material obtained in example 3;
fig. 15 is an XRD spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 3;
fig. 16 is a nitrogen adsorption/desorption graph and a pore size distribution graph of the nitrogen-doped graphene-based activated carbon material obtained in example 3; (in FIG. 16, a is a nitrogen adsorption/desorption graph, and in FIG. 16, b is a pore size distribution graph)
Fig. 17 is an XPS spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 3; (a in FIG. 17 is a surface element analysis full spectrum of the nitrogen-doped graphene-based activated carbon material, b in FIG. 17 is a high-resolution C1s spectrum of the nitrogen-doped graphene-based activated carbon material, C in FIG. 17 is a high-resolution N1s spectrum of the nitrogen-doped graphene-based activated carbon material, and d in FIG. 17 is a high-resolution O1s spectrum of the nitrogen-doped graphene-based activated carbon material)
FIG. 18 is a graph of the cycle performance at 0.2C for the assembled lithium sulfur half cell of example 4;
FIG. 19 is a graph of the cycle performance at 1C for the assembled lithium sulfur half cell of example 4;
FIG. 20 is a graph of rate performance of the assembled lithium sulfur half cell of example 4;
fig. 21 is a CV plot at different scan rates for the assembled lithium sulfur half cell of example 4.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
Preparation of nitrogen-doped graphene-like activated carbon material
Mixing melamine and L-cysteine according to the mass ratio of 10:1 of the melamine to the L-cysteine, carrying out ball milling for 5h to obtain a precursor, heating the precursor to 900 ℃ at the speed of 2 ℃/min in the protection of argon, keeping the temperature for 3h, and then cooling to room temperature at the speed of 2 ℃/min to obtain the nitrogen-doped graphene-like activated carbon material.
Fig. 1 is a scanning electron microscope photograph of the nitrogen-doped graphene-based activated carbon material obtained in example 1, wherein a in fig. 1 is a scanning electron microscope photograph magnified 10000 times and b in fig. 1 is a scanning electron microscope photograph magnified 30000 times, and it can be seen from fig. 1 that the material has a graphene-like sheet structure.
Fig. 2 is a transmission electron microscope photograph of the nitrogen-doped graphene-based activated carbon material obtained in example 1, and it can be seen from fig. 2 that the material has a continuous sheet-like structure.
Fig. 3 is an XRD spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 1, and as can be seen from fig. 3, characteristic peaks at 26 ° and 44 ° 2 θ angles in the spectrum correspond to (002) and (100) crystal planes of a graphitized structure, respectively, while a relatively broad peak appearing between 20 ° and 30 ° is a typical amorphous carbon peak type, which proves that the material is a typical activated carbon material.
FIG. 4 is a Raman spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 1, and it can be seen from FIG. 4 that the material has a D peak and a G peak typical of activated carbon materials, and I D /I G The value of (A) is 1.51, which indicates that the material has many defects and active sites.
FIG. 5 is a nitrogen adsorption/desorption graph of the nitrogen-doped graphene-based activated carbon material obtained in example 1, and it can be seen from FIG. 5 that the specific surface area of the material is 304m 2 /g。
Fig. 6 is a pore size distribution diagram of the nitrogen-doped graphene-based activated carbon material obtained in example 1, and it can be seen from fig. 6 that the pore size of the material is intensively distributed in the range of 3 to 5 nm.
Fig. 7 is an XPS spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 1, wherein a in fig. 7 is a surface elemental analysis full spectrum of the nitrogen-doped graphene-based activated carbon material; in fig. 7, b is a high-resolution C1s spectrogram of the nitrogen-doped graphene-like activated carbon material; in fig. 7, c is a high-resolution N1s spectrogram of the nitrogen-doped graphene-like activated carbon material; in fig. 7, d is a high-resolution O1s spectrogram of the nitrogen-doped graphene-like activated carbon material, and as can be seen from fig. 7, the material mainly comprises C, N and O.
Example 2
Preparation of nitrogen-doped graphene-like activated carbon material
Mixing melamine and L-cysteine according to the mass ratio of 5:1 of the melamine to the L-cysteine, carrying out ball milling for 10h to obtain a precursor, heating the precursor to 1500 ℃ at the speed of 5 ℃/min in the protection of nitrogen, then keeping the temperature for 1h, and then cooling to room temperature at the speed of 5 ℃/min to obtain the nitrogen-doped graphene-like activated carbon material.
Fig. 8 is a scanning electron microscope photograph of the nitrogen-doped graphene-like activated carbon material obtained in example 2, wherein a in fig. 8 is a scanning electron microscope photograph magnified 10000 times and b in fig. 8 is a scanning electron microscope photograph magnified 30000 times, and it is understood from fig. 8 that the material has a graphene-like sheet structure.
Fig. 9 is a transmission electron microscope photograph of the nitrogen-doped graphene-based activated carbon material obtained in example 2, and as can be seen from fig. 9, the material has a continuous sheet-like structure.
Fig. 10 is an XRD spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 2, and as can be seen from fig. 10, characteristic peaks at 26 ° and 44 ° 2 θ angles in the spectrum correspond to (002) and (100) crystal planes of a graphitized structure, respectively, while a relatively broad peak appearing between 20 ° and 30 ° is a typical amorphous carbon peak type, which proves that the material is a typical activated carbon material.
FIG. 11 is a nitrogen adsorption and desorption graph of the nitrogen-doped graphene-like activated carbon material obtained in example 2And a pore size distribution diagram, wherein a in FIG. 11 is a nitrogen adsorption and desorption graph, and as can be seen from a in FIG. 11, the specific surface area of the material is 252m 2 (ii)/g; b in FIG. 11 is a distribution diagram of the pore diameter, and as can be seen from b in FIG. 11, the pore diameter of the material is distributed in a concentrated manner from 3 nm to 5 nm.
Fig. 12 is an XPS spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 2, wherein a in fig. 12 is a surface elemental analysis full spectrum of the nitrogen-doped graphene-based activated carbon material; in fig. 12, b is a high-resolution C1s spectrogram of the nitrogen-doped graphene-like activated carbon material; in fig. 12, c is a high-resolution N1s spectrogram of the nitrogen-doped graphene-like activated carbon material; in fig. 12, d is a high-resolution O1s spectrogram of the nitrogen-doped graphene-like activated carbon material, and as can be seen from fig. 12, the material mainly comprises C, N and O.
Example 3
Preparation of nitrogen-doped graphene-like activated carbon material
Mixing melamine and L-cysteine according to the mass ratio of 1:1 of the melamine to the L-cysteine, carrying out ball milling for 2h to obtain a precursor, heating the precursor to 600 ℃ at the speed of 1 ℃/min in the protection of helium, then keeping the temperature for 2h, and then cooling to room temperature at the speed of 1 ℃/min to obtain the nitrogen-doped graphene-like activated carbon material.
Fig. 13 is a scanning electron microscope photograph of the nitrogen-doped graphene-like activated carbon material obtained in example 3, wherein a in fig. 13 is a scanning electron microscope photograph at 10000 times, and b in fig. 13 is a scanning electron microscope photograph at 30000 times, and it is understood from fig. 13 that the material has a graphene-like sheet structure.
Fig. 14 is a transmission electron microscope photograph of the nitrogen-doped graphene-based activated carbon material obtained in example 3, and as can be seen from fig. 14, the material has a continuous sheet-like structure.
Fig. 15 is an XRD spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 3, and as can be seen from fig. 15, characteristic peaks at 26 ° and 44 ° 2 θ angles in the spectrum correspond to (002) and (100) crystal planes of a graphitized structure, respectively, while a relatively broad peak appearing between 20 ° and 30 ° is a typical amorphous carbon peak type, which proves that the material is a typical activated carbon material.
FIG. 16 is a drawing showingA nitrogen adsorption and desorption graph and a pore diameter distribution graph of the nitrogen-doped graphene-based activated carbon material obtained in example 3, wherein a in fig. 16 is a nitrogen adsorption and desorption graph, and as can be seen from a in fig. 16, the specific surface area of the material is 132m 2 (ii)/g; b in FIG. 16 is a distribution diagram of the pore diameter, and as can be seen from b in FIG. 16, the pore diameter of the material is distributed in a concentrated manner from 3 nm to 5 nm.
Fig. 17 is an XPS spectrum of the nitrogen-doped graphene-based activated carbon material obtained in example 3, wherein a in fig. 17 is a surface elemental analysis full spectrum of the nitrogen-doped graphene-based activated carbon material; in fig. 17, b is a high-resolution C1s spectrogram of the nitrogen-doped graphene-like activated carbon material; in fig. 17, c is a high-resolution N1s spectrogram of the nitrogen-doped graphene-like activated carbon material; in fig. 17, d is a high-resolution O1s spectrogram of the nitrogen-doped graphene-like activated carbon material, and as can be seen from fig. 17, the material mainly comprises C, N and O.
Example 4
A lithium sulfur half cell was assembled with the nitrogen-doped graphene-like carbon material prepared in example 1 as a positive electrode material of a lithium sulfur cell and the resulting cell was tested for relevant electrical properties.
Mixing the nitrogen-doped graphene-like activated carbon material prepared in the example 1 with a conductive agent (CNT) and a binder (PVDF) according to a mass ratio of 80:10:10, adding a proper amount of solvent (NMP), grinding the mixture into uniform slurry in an agate mortar, coating the uniform slurry on carbon paper with the diameter of 13mm, then placing the carbon paper on a 60 ℃ blast drying oven to dry for 12 hours to prepare a standby pole piece, then transferring the standby pole piece to a glove box in an argon atmosphere, and dropwise adding polysulfide (Li) on the standby pole piece 2 S 6 And 1M) solution as a positive electrode, a metal lithium sheet as a counter electrode, assembling the coin cell, wherein the model of the coin cell is CR2032, the diaphragm is a polypropylene microporous membrane Celgard 2400, and the electrolyte is 1M LiTFSI solution (the solvent is 1, 3-Dioxolane (DOL) and ethylene glycol dimethyl ether (DME) in a volume ratio of 1: 1). The assembled cell was tested for electrochemical performance on a LAND cell test system at a voltage range of 1.7-2.7V.
Fig. 18 is a cycle performance graph of the lithium-sulfur half-cell assembled in example 4 at 0.2C, and as can be seen from fig. 18, the reversible specific capacity of 910mAh/g is still maintained after the electrode is subjected to a cycle stability test of 400 cycles at 0.2C, and the attenuation rate per cycle is only 0.05%, which indicates that the nitrogen-doped graphene-like activated carbon material has excellent cycle stability.
Fig. 19 is a cycle performance graph of the lithium-sulfur half-cell assembled in example 4 at 1C, and as can be seen from fig. 19, the electrode can still maintain a high specific capacity of 800mAh/g after 500 cycles at 1C, which indicates that the nitrogen-doped graphene-like activated carbon material has significant cycle stability.
Fig. 20 is a rate performance graph of the lithium-sulfur half-cell assembled in example 4, and as can be seen from fig. 20, the specific capacity of the cell gradually decreases in the process of gradually increasing the current density from 0.2C to 2C, and the cell still has a specific capacity of 820mAh/g when the current density is 2C, which indicates that the nitrogen-doped graphene-like activated carbon material has excellent rate performance.
Fig. 21 is a CV graph of the assembled lithium-sulfur half-cell in example 4 at different scanning rates, and it can be seen from fig. 21 that all curves have 4 redox peaks, and as the scanning rate increases, the curves still maintain good shapes, indicating that the nitrogen-doped graphene-like activated carbon material has excellent rate capability.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (6)
1. A preparation method of a nitrogen-doped graphene-like activated carbon material is characterized by comprising the following steps: mixing melamine and L-cysteine, performing ball milling to obtain a precursor, further carbonizing the precursor in an inert atmosphere, and cooling the precursor to room temperature to obtain a nitrogen-doped graphene-like activated carbon material;
the mass ratio of the melamine to the L-cysteine is 1-10: 1.
2. The method of claim 1, wherein the ball milling time is 2 to 10 hours.
3. The method of claim 1, wherein the inert atmosphere is one or more of argon, nitrogen, helium, or neon.
4. The method as claimed in claim 1, wherein the cooling to room temperature after the carbonization is performed by raising the temperature to 1500 ℃ at a rate of 1-5 ℃/min, then maintaining the temperature for 1-3h, and then lowering the temperature to room temperature at a rate of 1-5 ℃/min.
5. A nitrogen-doped graphene-like activated carbon material prepared by the method of any one of claims 1 to 4.
6. Use of the nitrogen-doped graphene-like activated carbon material according to claim 5 as a positive electrode material for a lithium-sulfur battery.
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| AU2014214532A1 (en) * | 2013-02-06 | 2015-08-20 | The Australian National University | Radical orbital switching |
| CN104085874A (en) * | 2014-06-05 | 2014-10-08 | 中国科学院广州地球化学研究所 | Preparation method for doped graphene-like structural nanometer carbon material |
| CN104925796A (en) * | 2015-06-24 | 2015-09-23 | 上海大学 | Preparation method of porous graphene |
| CN106315574A (en) * | 2015-06-29 | 2017-01-11 | 徐海波 | Graphene oxide quantum dots, material formed from same and graphene-like structural substance, and preparation methods |
| JP2017081764A (en) * | 2015-10-22 | 2017-05-18 | 国立大学法人東北大学 | Production method of organically modified carbon material, and organically modified carbon material |
| CN106185890A (en) * | 2016-07-04 | 2016-12-07 | 石河子大学 | A kind of preparation method of porous class Graphene |
| CN106129410A (en) * | 2016-07-18 | 2016-11-16 | 吉科猛 | The class Graphene Carbon Materials of three-dimensional ordered macroporous structure, prepare and apply |
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