CN110911650A - Preparation method of three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material - Google Patents
Preparation method of three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material Download PDFInfo
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Abstract
The invention relates to a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material, which comprises the following steps: grinding and mixing nickel salt, a nitrogen-containing organic matter and an SBA-15 mesoporous molecular sieve, heating to 600-1000 ℃ at the speed of 1-20 ℃/min in an oxygen-free atmosphere, and carrying out heat treatment to obtain the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material. The invention has the advantages that: 1. according to the invention, nitrogen doping is introduced into the carbon material in a needle-like manner, so that the conductivity of the material can be improved, additional lithium ions can be added to be inserted into active sites, and the capacity and the cycling stability of the material can be effectively improved; 2. the synthesized negative electrode material has a unique three-dimensional nano structure, provides rich and rapid channels for ion and electron transmission, shortens the diffusion path of lithium ions, and effectively reduces the impedance and the polarization degree; 3. the synthesis method is simple and convenient, and is easy to realize large-scale production.
Description
Technical Field
The application relates to a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material, belonging to the technical field of battery manufacturing.
Background
Two major problems of sustainable development of human society are as follows: the increasing depletion and burning of fossil fuels poses increasingly serious environmental problems. Therefore, the development of new clean energy is imminent, and lithium ion battery systems are expected as new electrochemical energy storage systems. In the field of electric vehicles or hybrid electric vehicles, secondary lithium ion batteries are expected to be widely applied. Although the lithium ion battery has been commercialized from the 80 th 19 th century, the conventional lithium ion battery has reached its bottleneck in increasing energy density through the development of decades, wherein the biggest problem is that the lithium storage capacity of the carbon negative electrode material has reached a limit (theoretical capacity of 372mAh g)-1) The capacity of the graphite carbon negative electrode material is 360mAh g-1It cannot meet the future development requirements of electric automobiles. Most of lithium batteries in the current market are graphite cathode materials, and the energy density of the cathode materials is difficult to improve from the gram capacity and the compaction density of graphite. In addition, the graphite sheet has problems such as easy peeling and unsatisfactory cycle performance. Therefore, the development of lithium ion batteries with higher energy density, particularly negative electrode materials, has very important strategic and practical significance.
In this regard, many researchers have proposed the development of three-dimensional carbon structures and chemical modifications (introduction of heteroatoms) to carbon materials to increase the capacity of the materials and improve the cycling stability. Wherein the three-dimensional carbon structure not only has higher conductivity but also has better mechanical stability. And heteroatom incorporation can provide additional lithium ion intercalation active sites. The invention adopts mesoporous silicon molecular sieve (SBA-15) as a template, nitrogen-containing organic matters as a carbon source and a nitrogen source and a nickel catalyst to synthesize the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material by a heat treatment method. The carbon material obtained by the synthesis method has a unique three-dimensional nano structure, high conductivity and nitrogen content, and can effectively improve the capacity and the cycle stability of the battery.
Disclosure of Invention
Aiming at the problems of the existing synthesis method, the invention provides a feasible synthesis method for synthesizing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material, and the feasibility of large-scale production is realized.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material, which comprises the following steps:
grinding and mixing nickel salt, a nitrogen-containing organic matter and an SBA-15 mesoporous molecular sieve, heating to 600-1000 ℃ at the speed of 1-20 ℃/min in an oxygen-free atmosphere, and carrying out heat treatment to obtain the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material.
Preferably, the nitrogen-containing organic substance includes at least one of an amine compound, a heterocyclic compound, an amide compound, and a nitrile compound.
Preferably, the amine compound includes at least one of cyanamide, dicyandiamide, tryptophan, cystine, citrulline, lysine, threonine, leucine, isoleucine, valine, methionine, and phenylalanine.
Preferably, the heterocyclic compound comprises at least one of 2-methylimidazole, polyvinylpyrrolidone and melamine.
Preferably, the amide compound includes at least one of urea, malonyl urea, and thiourea.
Preferably, the nitrile compound includes at least one of terephthalonitrile and benzonitrile.
Preferably, the nickel salt includes at least one of nickel nitrate, nickelocene, nickel chloride, nickel acetate, nickel sulfate, nickel oxalate and nickel phosphate.
Preferably, the mass ratio of the nickel salt, the nitrogen-containing organic substance and the SBA-15 mesoporous molecular sieve is 1:1: 1-10: 1: 5.
Preferably, the oxygen-free atmosphere comprises N2、Ar、H2And H2-Ar mixed gasAny one of them.
Preferably, the time of the heat treatment is 1-6 h.
The invention can provide a synthetic method for synthesizing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material, and the optimized cathode material can be obtained by the synthetic method. The beneficial details are as follows:
1. according to the invention, nitrogen doping is introduced into the carbon material in a needle-like manner, so that the conductivity of the material can be improved, additional lithium ions can be added to be inserted into active sites, the capacity and the cycle stability of the material can be effectively improved, and experiments prove that the content of the material is 1A g-1Under the current density, the capacity is still maintained at 400mAh g after 1000 times of circulation-1Above, the coulombic efficiency is as high as 99%;
2. the synthesized negative electrode material has a unique three-dimensional nano structure, provides rich and rapid channels for ion and electron transmission, shortens the diffusion path of lithium ions, and effectively reduces the impedance and the polarization degree;
3. the synthesis method is simple and convenient, and is easy to realize large-scale production.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a transmission electron micrograph of an SBA-15 template of the present invention;
FIG. 2 is a scanning electron microscope image of the three-dimensional N-doped carbon tube-carbon tube cathode material obtained in example 1 of the present invention under different magnifications;
FIG. 3 is a transmission electron microscope image of the three-dimensional N-doped carbon tube-carbon tube cathode material obtained in example 2 of the present invention under different magnifications;
fig. 4 is a graph of electrochemical performance of the three-dimensional nitrogen-doped carbon tube-carbon tube negative electrode material obtained in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
1.45g of nickel nitrate, 0.2g of melamine and 1g of SBA-15 template were mixed by grinding, and N was added2In a tube furnace with atmosphere, the temperature is raised to 800 ℃ at the speed of 5 ℃/min and is preserved for 2 hours. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
As shown in FIG. 1, the SBA-15 template is a one-dimensional mesoporous nanorod. Fig. 2a, 2b and 2c show scanning electron micrographs of the synthesized three-dimensional nitrogen-doped carbon tube-carbon tube cathode material at different magnifications, which are three-dimensional nanostructures from which elongated carbon nanotubes are grown to form a conductive carbon network. The slender carbon nano tube is of a bamboo-shaped structure. FIGS. 3a, 3b, 3c and 3d show transmission electron micrographs at different magnifications of the synthesized three-dimensional nitrogen-doped carbon tube-carbon tube anode material, the diameter of the outer elongated carbon tube being about 20 nm. The nitrogen content of the negative electrode material was 5.2 wt%, which was 1A g-1The electrochemical performance under current density is shown in FIG. 4, the first discharge specific capacity is up to 578mAh g-1The capacity is still maintained at 421mAh g after 1600 times of circulation-1The coulombic efficiency is as high as 99%.
Example 2
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
1.5g of nickel acetate, 0.25g of dicyandiamide and 1g of SBA-15 template are ground and mixed, put into a tubular furnace with Ar atmosphere, heated to 700 ℃ at the speed of 5 ℃/min and kept for 4 hours. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
The nitrogen content of the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material is 4.8 wt%, which is 1A g-1The first discharge specific capacity under the current density is up to 562mAh g-1After 1000 times of circulation, the capacity is still maintained at 408mAh g-1The coulombic efficiency is as high as 99%.
Example 3
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
1g of nickelocene, 0.2g of melamine and 1g of SBA-15 template are mixed by grinding and placed in H2In a tube furnace with atmosphere, the temperature is raised to 600 ℃ at the speed of 2 ℃/min and is preserved for 6 hours. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
The nitrogen content of the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material is 4.4 wt%, which is 1A g-1The first discharge specific capacity under the current density is up to 582mAh g-1The capacity is still maintained to be 424mAh g after 1200 times of circulation-1The coulombic efficiency is as high as 99%.
Example 4
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
grinding and mixing 1.5g of nickel sulfate, 0.3g of polyvinylpyrrolidone and 1g of SBA-15 template, adding N2In a tube furnace with atmosphere, the temperature is raised to 900 ℃ at the rate of 10 ℃/min and is preserved for 2 hours. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
The nitrogen content of the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material is 5.6 wt%, which is 1A g-1The first discharge specific capacity under the current density is as high as 509mAh g-1Circulation ofThe capacity is still kept at 406mAh g after 1000 times-1The coulombic efficiency is as high as 99%.
Example 5
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
2g of nickel nitrate, 0.4g of urea and 1.5g of SBA-15 template are ground and mixed, put into a tubular furnace with Ar atmosphere, heated to 1000 ℃ at a speed of 10 ℃/min and kept for 1 hour. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
The nitrogen content of the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material is 5.4 wt%, which is 1A g-1The first discharge specific capacity under the current density is as high as 569mAh g-1After 1000 times of circulation, the capacity is still maintained at 414mAh g-1The coulombic efficiency is as high as 99%.
Example 6
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
grinding and mixing 1.25g of nickel nitrate, 0.3g of 2-methylimidazole and 1.5g of SBA-15 template, adding H2In a tube furnace with-Ar atmosphere, the temperature is raised to 800 ℃ at the speed of 2.5 ℃/min and the temperature is kept for 2 hours. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
The nitrogen content of the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material is 5.1 wt%, which is 1A g-1The first discharge specific capacity under the current density is up to 556mAh g-1After 1000 times of circulation, the capacity is still maintained at 402mAh g-1The coulombic efficiency is as high as 99%.
Example 7
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
grinding and mixing 1.5g of nickel chloride, 0.25g of tryptophan and 1.25g of SBA-15 template, adding H2In a tube furnace with-Ar atmosphere, the temperature is raised to 800 ℃ at the speed of 5 ℃/min and is preserved for 2 hours. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
The nitrogen content of the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material is 5.6 wt%, which is 1A g-1The first discharge specific capacity under the current density is as high as 512mAh g-1After 1000 times of circulation, the capacity is still maintained at 408mAh g-1The coulombic efficiency is as high as 99%.
Example 8
The embodiment provides a preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material, which comprises the following specific steps:
2g of nickel oxalate, 0.4g of lysine and 1g of SBA-15 template are ground and mixed, and put into H2In a tube furnace with atmosphere, the temperature is raised to 700 ℃ at the speed of 10 ℃/min and is preserved for 2 hours. And after the reaction is finished, cooling to room temperature, taking out, stirring for 12 hours at room temperature by adopting 10M HCl, and stirring for 12 hours at 80 ℃ by adopting 1M NaOH to remove Ni residues and an SBA-15 template, thus obtaining the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material.
The nitrogen content of the three-dimensional nitrogen-doped carbon tube-carbon tube cathode material is 5.9 wt%, which is 1A g-1The first discharge specific capacity under the current density is up to 523mAh g-1After 1000 times of circulation, the capacity is still maintained at 423mAh g-1The coulombic efficiency is as high as 99%.
In summary, the present invention is only a preferred embodiment, and not intended to limit the scope of the invention, and all equivalent changes and modifications in the shape, structure, characteristics and spirit of the present invention described in the claims should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material is characterized by comprising the following steps:
grinding and mixing nickel salt, a nitrogen-containing organic matter and an SBA-15 mesoporous molecular sieve, heating to 600-1000 ℃ at the speed of 1-20 ℃/min in an oxygen-free atmosphere, and carrying out heat treatment to obtain the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery cathode material.
2. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material according to claim 1, wherein the nitrogen-containing organic compound comprises at least one of an amine compound, a heterocyclic compound, an amide compound and a nitrile compound.
3. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material according to claim 2, wherein the amine compound comprises at least one of cyanamide, dicyandiamide, tryptophan, cystine, citrulline, lysine, threonine, leucine, isoleucine, valine, methionine, and phenylalanine.
4. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material according to claim 2, wherein the heterocyclic compound comprises at least one of 2-methylimidazole, polyvinylpyrrolidone and melamine.
5. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material according to claim 2, wherein the amide compound comprises at least one of urea, malonylurea and thiourea.
6. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material according to claim 2, wherein the nitrile compound comprises at least one of terephthalonitrile and benzonitrile.
7. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material of claim 1, wherein the nickel salt comprises at least one of nickel nitrate, nickelocene, nickel chloride, nickel acetate, nickel sulfate, nickel oxalate and nickel phosphate.
8. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material as claimed in claim 1, wherein the mass ratio of the nickel salt, the nitrogen-containing organic substance and the SBA-15 mesoporous molecular sieve is 1:1: 1-10: 1: 5.
9. The method of claim 1, wherein the oxygen-free atmosphere comprises N2、Ar、H2And H2Any one of Ar mixed gas.
10. The method for preparing the three-dimensional nitrogen-doped carbon tube-carbon tube lithium ion battery anode material of claim 1, wherein the time of the heat treatment is 1-6 h.
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