CN110797535B - Preparation method of nitrogen-cobalt-oxygen tri-doped network carbon material used as potassium ion battery cathode - Google Patents
Preparation method of nitrogen-cobalt-oxygen tri-doped network carbon material used as potassium ion battery cathode Download PDFInfo
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Abstract
The invention discloses a preparation method of a nitrogen-cobalt-oxygen tri-doped network carbon material used as a potassium ion battery cathode, which takes a polymer network synthesized in situ in a liquid crystal/epoxy monomer/photoinitiator system as a precursor and adopts a simple and easy carbonization-doping method to prepare the nitrogen-cobalt-oxygen tri-doped network carbon material; the nitrogen-cobalt-oxygen tri-doped network carbon material is used as a potassium ion battery cathode material to be applied to manufacture the button cell, the network carbon material is applied to the aspect of the potassium ion battery cathode material, and the carbon material, particularly an amorphous hard carbon material, has the advantages of good chemical stability, conductivity, thermal stability, low cost, larger interplanar spacing, carbon structure which is not easy to expand and the like.
Description
Technical Field
The invention belongs to the technical field of nitrogen-cobalt-oxygen tri-doped network carbon materials, and particularly relates to a preparation method of a nitrogen-cobalt-oxygen tri-doped network carbon material used as a potassium ion battery cathode.
Background
The lithium ion battery as a typical representative of electrochemical energy storage has the characteristics of light weight, high energy density, long cycle life, excellent rate performance and the like, plays an increasingly important role in devices such as smart grids and mobile electronics, and gradually develops to the field of large-scale energy storage. However, the lithium resources are distributed unevenly around the world, the reserves are limited, and the price is high, so that the application demand of human beings for large-scale energy storage cannot be met by the lithium ion battery alone in the future. On the other hand, the focus of scaled energy storage applications is low cost, rather than high energy density. Therefore, it is necessary to develop energy storage systems which are rich in resources and can replace lithium ion batteries.
Sodium and potassium ion batteries have received increasing attention as promising energy storage devices that can replace lithium ion batteries due to their wide range of resources. Potassium, sodium and lithium of the lithium ion battery are all elements of a first main group and have similar physicochemical properties; lithium is only 18ppm worldwide, far below 22700ppm for sodium and 18400ppm for potassium, and the price of the carbonate corresponding to sodium and potassium is far below that of lithium carbonate. Second, the atomic radius of potassium ion is larger than that of sodium ion, but the reduction potential of potassium ion is-2.93V, lower than-2.7V of sodium ion, and closer to-3.04 of lithium ion in terms of atomic mass and radius. Therefore, in theoretical analysis, potassium ion batteries have higher energy density and discharge voltage than sodium ion batteries. In addition, potassium ions have much weaker Lewis acid than sodium ions and have stronger desolvation capacity. Therefore, potassium ion batteries are receiving increasing attention from researchers.
The working principle of the potassium ion battery is similar to that of the lithium ion battery, and the potassium ion battery belongs to a rocking chair type battery: during charging, potassium ions are extracted from the positive electrode and embedded into the negative electrode, and electrons are provided to the negative electrode by an external circuit to compensate charges; on the contrary, during discharging, potassium ions are extracted from the negative electrode and inserted into the positive electrode, and electrons are provided to the positive electrode from an external circuit to compensate charges. That is, the potassium ion battery realizes the conversion and storage of electric energy and chemical energy by the cyclic and reciprocal intercalation and deintercalation of potassium ions between electrode materials. The research of the potassium storage electrode material is a key technology of the potassium ion battery, and the structure and the performance of the electrode material directly determine the electrochemical performance and the application prospect of the potassium ion battery. In the negative electrode material field, carbon materials, especially amorphous hard carbon materials, are considered to be one of the most promising practical electrode materials due to their advantages of good chemical stability, electrical conductivity, thermal stability, low cost, large interplanar spacing, and carbon structure that is not easily expanded.
At present, various types of potassium ion battery negative electrode materials, such as graphite, nitrogen-doped graphene, Prussian blue, transition metal composite materials and the like, are widely researched and applied. The early methods for synthesizing graphite intercalation compound complexes (GICs) comprise two-region gas phase synthesis or alkali metal solvation and the like, the metal potassium-graphite intercalation compounds at different stages can be obtained by the methods, and the potassium storage/potassium removal process of graphite in a potassium ion battery is realized by phase transformation generated at different stages, so that the charging/discharging process of the potassium ion battery is realized. The base graphite material or the carbon material is doped with the mixed elements, so that the surface defects of the carbon material are caused, the active sites of the carbon material are further improved, the potassium storage performance and the stability of the carbon material are enhanced, and the stability of the potassium ion battery is finally improved.
Based on the thought, the patent invents a novel preparation method of nitrogen-cobalt-oxygen tri-doped network carbon material used as a potassium ion battery cathode, and aims to provide experimental basis and theoretical guidance for preparing a high-performance potassium ion battery.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrogen-cobalt-oxygen tri-doped network carbon material used as a potassium ion battery cathode, which has the advantages of readily available raw materials, simple preparation method and high operation controllability.
The purpose of the invention is realized as follows: firstly, synthesizing a polymer network with uniform size in situ in a liquid crystal/epoxy monomer/photoinitiator system; thirdly, preparing the nitrogen-cobalt-oxygen tri-doped network carbon material by taking the synthesized polymer network as a precursor and adopting a simple and easy carbonization-doping method; and finally, taking the nitrogen-cobalt-oxygen tri-doped network carbon material as a negative electrode material of the potassium ion battery to be applied to manufacture the button cell.
As a better choice of the technical proposal, the precursor of the epoxy resin type polymer network for preparing the nitrogen-cobalt-oxygen tri-doped network carbon material is selected from liquid crystal epoxy monomers,
as a better choice of the above technical solution, the carbonization-doping method for preparing a nitrogen-cobalt-oxygen tri-doped network carbon material comprises the following specific steps:
a preparation method of a nitrogen-cobalt-oxygen tri-doped network carbon material used as a negative electrode of a potassium ion battery comprises the following steps:
a: in a liquid crystal/epoxy monomer/photoinitiator system, a photopolymerization-induced phase separation method is utilized to prepare a polymer network in situ, and the thickness and the size of the prepared polymer network are adjustable according to different precursor contents;
b: taking the polymer network obtained in the step a as a precursor, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving the heat for 1-3 hours to obtain a smooth network-shaped carbon material;
c: b, uniformly mixing and grinding the smooth network-shaped carbon material obtained in the step b and melamine powder according to the mass ratio of 2:1, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving heat for 1-3 hours to obtain a nitrogen-doped network-shaped carbon material with a rough surface;
d: dispersing 30mg of the nitrogen-doped and rough-surface network-shaped carbon material obtained in the step c in 60mL of methanol, and performing ultrasonic dispersion for 20 min; adding a cobalt acetylacetonate-methanol solution with a certain concentration into the solution, violently stirring for 24h, centrifuging, washing the obtained powder with methanol, vacuum-drying, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace under the nitrogen atmosphere, and preserving the temperature for 1-3 h to obtain the nitrogen-cobalt-oxygen tri-doped network carbon material.
As a better choice of the technical scheme, the size of the prepared nitrogen-cobalt-oxygen tri-doped network carbon material is adjustable between 2 and 8 mu m.
As a better choice of the technical scheme, the specific surface area of the prepared nitrogen-cobalt-oxygen tri-doped network carbon material is more than 300 m2/g, and the carbon material has a mesoporous/macroporous composite hierarchical pore structure.
As a better choice of the above technical solution, the method for manufacturing the button cell by using the nitrogen-cobalt-oxygen tri-doped network carbon material as the negative electrode material of the potassium ion battery comprises the following specific steps:
(1) dispersing the prepared nitrogen-cobalt-oxygen tri-doped network carbon material, conductive carbon black and adhesive polyvinylidene fluoride in an N-methyl pyrrolidone solution according to the mass ratio of 70:20:10, fully mixing to form uniform paste, and uniformly coating the paste on a copper foil substrate; drying the coated electrode slice in a vacuum drying oven at 60 +/-20 ℃ for 6 hours, pressing by using a powder tablet press, and cutting into a circular electrode slice with the diameter of 8 mm to serve as a test electrode;
(2) the metal potassium is taken as a counter electrode, the glass fiber material is taken as a diaphragm, and the CR2032 button cell is assembled in an argon glove box with the water and oxygen contents less than 0.1 ppm; the electrolyte used was a 0.8M solution of potassium hexafluorophosphate in ethylene carbonate/diethyl carbonate.
As a better choice of the above technical scheme, the button cell prepared by using the nitrogen-cobalt-oxygen tri-doped network carbon material as the negative electrode material of the potassium ion battery is subjected to constant current charging and discharging on a blue battery tester, and the electrochemical performance of the material is tested, wherein the test result is as follows:
1) in the aspect of specific capacity: after the nitrogen-cobalt-oxygen tri-doped network-shaped carbon material is circulated for 100 circles under the current density of 50 mA/g, the coulombic efficiency of the battery is 89%, the capacity of the battery is 214.9 mAh/g, and the battery shows higher specific capacity;
2) and (3) stability: after the nitrogen-cobalt-oxygen tri-doped network carbon material is circulated for 200 circles under the current density of 50 mA/g, the capacity is as high as 172.1 mAh/g, the coulombic efficiency is as high as 99%, and the electrode material is stable in structure and good in battery circulation stability.
The invention has the technical effects and advantages that: the network carbon material is applied to the negative electrode material of the potassium ion battery, and the carbon material, especially the amorphous hard carbon material, has the advantages of good chemical stability, conductivity, thermal stability, low cost, larger crystal face spacing, carbon structure which is not easy to expand and the like.
Drawings
FIG. 1 is a scanning electron micrograph of a polymer network precursor used in example 1;
FIG. 2 is a scanning electron micrograph of the nitrogen-cobalt-oxygen tri-doped reticulated carbon material prepared in example 2;
FIG. 3 is an X-ray diffraction pattern of the nitrogen-cobalt-oxygen tri-doped reticulated carbon material prepared in example 2;
FIG. 4 is a graph of the electrochemical performance of the N-Co-O tri-doped network carbon material prepared in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The examples of the present invention employ the following exemplary preparation method, which comprises the steps of:
a preparation method of a nitrogen-cobalt-oxygen tri-doped network carbon material used as a negative electrode of a potassium ion battery comprises the following steps:
a: in a liquid crystal/epoxy monomer/photoinitiator system, a photopolymerization-induced phase separation method is utilized to prepare a polymer network in situ, and the thickness and the size of the prepared polymer network are adjustable according to different precursor contents;
b: taking the polymer network obtained in the step a as a precursor, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving the heat for 1-3 hours to obtain a smooth network-shaped carbon material;
c: b, uniformly mixing and grinding the smooth network-shaped carbon material obtained in the step b and melamine powder according to the mass ratio of 2:1, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving heat for 1-3 hours to obtain a nitrogen-doped network-shaped carbon material with a rough surface;
d: dispersing 30mg of the nitrogen-doped and rough-surface network-shaped carbon material obtained in the step c in 60mL of methanol, and performing ultrasonic dispersion for 20 min; adding a cobalt acetylacetonate-methanol solution with a certain concentration into the solution, violently stirring for 24h, centrifuging, washing the obtained powder with methanol, vacuum-drying, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace under the nitrogen atmosphere, and preserving the temperature for 1-3 h to obtain the nitrogen-cobalt-oxygen tri-doped network carbon material.
The method for manufacturing the button cell by taking the nitrogen-cobalt-oxygen tri-doped network-shaped carbon material as the negative electrode material of the potassium ion cell comprises the following specific steps:
(1) dispersing the prepared nitrogen-cobalt-oxygen tri-doped network carbon material, conductive carbon black and adhesive polyvinylidene fluoride in an N-methyl pyrrolidone solution according to the mass ratio of 70:20:10, fully mixing to form uniform paste, and uniformly coating the paste on a copper foil substrate; drying the coated electrode slice in a vacuum drying oven at 60 +/-20 ℃ for 6 hours, pressing by using a powder tablet press, and cutting into a circular electrode slice with the diameter of 8 mm to serve as a test electrode;
(2) the metal potassium is taken as a counter electrode, the glass fiber material is taken as a diaphragm, and the CR2032 button cell is assembled in an argon glove box with the water and oxygen contents less than 0.1 ppm; the electrolyte used was a 0.8M solution of potassium hexafluorophosphate in ethylene carbonate/diethyl carbonate.
Example 1
The specific operation flow for preparing the original polymer network carbon material in example 1 is as follows:
the method comprises the following steps: the names and the proportions of the selected liquid crystal, epoxy monomer and photoinitiator are listed in Table 1, and the size of the prepared polymer network is 5 mu m;
step two: heating the polymer network obtained in the step one to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving the heat for 1-3 hours to obtain a smooth network-shaped carbon material;
step three: dispersing the oxygen-doped polymer carbon material, the conductive carbon black and the adhesive polyvinylidene fluoride obtained in the step two in an N-methyl pyrrolidone solution according to the mass ratio of 70:20:10, fully mixing to form uniform paste, and uniformly coating the paste on a copper foil substrate; drying the coated electrode slice in a vacuum drying oven at 60 +/-20 ℃ for 6 hours, pressing by using a powder tablet press, and cutting into a circular electrode slice with the diameter of 8 mm to serve as a test electrode; the metal potassium is taken as a counter electrode, the glass fiber material is taken as a diaphragm, and the CR2032 button cell is assembled in an argon glove box with the water and oxygen contents less than 0.1 ppm; the electrolyte used was a 0.8M solution of potassium hexafluorophosphate in ethylene carbonate/diethyl carbonate (volume ratio 1: 1).
The microscopic morphology of the network-like carbon material was observed by Scanning Electron Microscopy (SEM), and the results are shown in FIG. 1.
TABLE 1 materials used for preparation of polymeric microspheres in EXAMPLE 1
| Categories | Name (R) | Ratio/%) |
| Liquid crystal display device | LC-0516-N* | 78.5 |
| Epoxy monomer | 2-methyl-1, 4-phenylenebis (4- (4- (oxetan-2-yl) butoxy) benzoate) |
20 |
| Photoinitiator | Bis (4-tert-butylphenyl) iodonium hexafluorophosphate | 1.5 |
Example 2
The specific operation flow of the preparation of the nitrogen-cobalt-oxygen tri-doped network carbon material in example 2 is as follows:
the method comprises the following steps: the names and the proportions of the selected liquid crystal, epoxy monomer and photoinitiator are listed in Table 1. The size of the prepared polymer network is 5 μm;
step two: heating the polymer network obtained in the step one to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving the heat for 1-3 hours to obtain a smooth network-shaped carbon material;
step three: uniformly mixing and grinding the smooth network-shaped carbon material obtained in the step two and melamine powder according to the mass ratio of 2:1, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving heat for 1-3 hours to obtain a nitrogen-doped network-shaped carbon material theta with a rough surface;
step four: dispersing the nitrogen-doped and rough-surface network-shaped carbon material obtained in every 30mg step III in 60mL of methanol, and performing ultrasonic dispersion for 20 min; adding a cobalt acetylacetonate-methanol solution with a certain concentration into the solution, violently stirring for 24h, centrifuging, washing the obtained powder with methanol, vacuum-drying, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace under the nitrogen atmosphere, and keeping the temperature for 1-3 h to obtain the nitrogen-cobalt-oxygen tri-doped network carbon material.
Step five: dispersing the nitrogen-cobalt-oxygen tri-doped network carbon material, the conductive carbon black and the adhesive polyvinylidene fluoride obtained in the third step in an N-methyl pyrrolidone solution according to the mass ratio of 70:20:10, fully mixing to form uniform paste, and uniformly coating the paste on a copper foil substrate; drying the coated electrode slice in a vacuum drying oven at 60 +/-20 ℃ for 6 hours, pressing by using a powder tablet press, and cutting into a circular electrode slice with the diameter of 8 mm to serve as a test electrode; the metal potassium is taken as a counter electrode, the glass fiber material is taken as a diaphragm, and the CR2032 button cell is assembled in an argon glove box with the water and oxygen contents less than 0.1 ppm; the electrolyte used was a 0.8M solution of potassium hexafluorophosphate in ethylene carbonate/diethyl carbonate (volume ratio 1: 1). And assembling to prepare the button cell.
The average size of the prepared nitrogen-cobalt-oxygen tri-doped network carbon material is 5.62 mu m, the specific surface area is 396.465 m2/g, and the carbon material has a mesoporous/macroporous composite hierarchical pore structure.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of a nitrogen-cobalt-oxygen tri-doped network carbon material used as a negative electrode material of a potassium ion battery is characterized by comprising the following steps: preparing a nitrogen-cobalt-oxygen tri-doped network carbon material by taking a polymer network synthesized in situ in a liquid crystal/epoxy monomer/photoinitiator system as a precursor and adopting a carbonization-doping method;
the preparation method of the nitrogen-cobalt-oxygen tri-doped network carbon material comprises the following steps:
a: in a liquid crystal/epoxy monomer/photoinitiator system, a photopolymerization-induced phase separation method is utilized to prepare a polymer network in situ, and the thickness and the size of the prepared polymer network are adjustable according to different precursor contents;
b: taking the polymer network obtained in the step a as a precursor, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving the heat for 1-3 hours to obtain a smooth network-shaped carbon material;
c: b, uniformly mixing and grinding the smooth network-shaped carbon material obtained in the step b and melamine powder according to the mass ratio of 2:1, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace in the nitrogen atmosphere, and preserving heat for 1-3 hours to obtain a nitrogen-doped network-shaped carbon material with a rough surface;
d: dispersing 30mg of the nitrogen-doped and rough-surface network-shaped carbon material obtained in the step c in 60mL of methanol, and performing ultrasonic dispersion for 20 min; adding a cobalt acetylacetonate-methanol solution with a certain concentration into the solution, violently stirring for 24h, centrifuging, washing the obtained powder with methanol, vacuum-drying, heating to 500 ℃ at the speed of 5 ℃/min in a vacuum tube furnace under the nitrogen atmosphere, and preserving the temperature for 1-3 h to obtain the nitrogen-cobalt-oxygen tri-doped network carbon material.
2. The method for preparing a nitrogen-cobalt-oxygen triple-doped network carbon material according to claim 1, wherein: the size of the nitrogen-cobalt-oxygen tri-doped network carbon material prepared in the step d is adjustable between 2 and 8 mu m.
3. The method for preparing a nitrogen-cobalt-oxygen triple-doped network carbon material according to claim 1, wherein: the specific surface area of the nitrogen-cobalt-oxygen tri-doped network carbon material prepared in the step d is more than 300 m2And/g, and has a mesoporous/macroporous composite hierarchical pore structure.
4. The method for manufacturing the button cell by using the nitrogen-cobalt-oxygen tri-doped network carbon material obtained by the preparation method as the negative electrode material of the potassium ion battery according to any one of claims 1 to 3, is characterized by comprising the following steps:
(1) dispersing the prepared nitrogen-cobalt-oxygen tri-doped network carbon material, conductive carbon black and adhesive polyvinylidene fluoride in an N-methyl pyrrolidone solution according to the mass ratio of 70:20:10, fully mixing to form uniform paste, and uniformly coating the paste on a copper foil substrate; drying the coated electrode slice in a vacuum drying oven at 60 +/-20 ℃ for 6 hours, pressing by using a powder tablet press, and cutting into a circular electrode slice with the diameter of 8 mm to serve as a test electrode;
(2) the metal potassium is taken as a counter electrode, the glass fiber material is taken as a diaphragm, and the CR2032 button cell is assembled in an argon glove box with the water and oxygen contents less than 0.1 ppm; the electrolyte used was a 0.8M solution of potassium hexafluorophosphate in ethylene carbonate/diethyl carbonate.
5. The method for manufacturing the button cell by using the nitrogen-cobalt-oxygen tri-doped network-shaped carbon material as the negative electrode material of the potassium ion battery according to claim 4, wherein the method comprises the following steps: the volume ratio of the ethylene carbonate/diethyl carbonate solution in the step (2) is 1: 1.
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