CN110459754B - High-performance lithium ion battery C3N4Preparation method of/carbon composite negative electrode material - Google Patents
High-performance lithium ion battery C3N4Preparation method of/carbon composite negative electrode material Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
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- 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
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a high-performance lithium ion battery C3N4The preparation method of the/carbon composite negative electrode material comprises the steps of placing a precursor containing C and N elements and a liquid carbon source into a reactor, sealing the reactor under the atmosphere of argon, carrying out heat preservation reaction at 400-600 ℃ for 1-4 hours, cooling the mixture, washing and drying to obtain the product, wherein the preparation method is carried out in a sealed reaction environment, and the prepared C is prepared3N4The material has high yield, and simultaneously, the material is added with a liquid carbon source so as to be in C3N4In-situ carbonization and compounding into C in the synthesis process3N4the/C structure improves the conductivity of the material, thereby having excellent electrochemical performance. The invention is suitable for preparing the lithium ion battery C3N4A/carbon composite negative electrode material.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium ion battery cathode materials, and relates to a high-performance lithium ion battery C3N4A preparation method of a/carbon composite negative electrode material.
Background
The lithium ion battery has the advantages of long cycle life, high energy density, rapid charge and discharge and the like, is widely applied to emerging fields of mobile electronic equipment such as electric vehicles, hybrid electric vehicles, smart grids and the like, but the energy density of the lithium ion battery still needs to be further improved. The current commercial lithium ion battery cathode material is mainly a graphite material, the theoretical capacity of the lithium ion battery cathode material is only 372mAh/g, and the improvement of the overall energy density of the battery is severely restricted. Therefore, developing a new replaceable anode material with high discharge capacity and safety and economy is one of the hot spots in the research field of battery materials at present.
Since the carbon nanotubes were discovered in the 80 s of the last century, the research of carbon materials has been turned over worldwide, and new carbon materials with different structures and morphologies, such as graphene and C, were synthesized in succession3N4And the like. C3N4The compound has the characteristics of good chemical stability, low cost, simple preparation and the like, and is researched by the majority of scientific research personnel. However, pure C3N4The structure of the material is relatively complete, the active sites are less, and the C is synthesized at present3N4The method is mainly that the precursor containing carbon and nitrogen elements such as melamine or urea is carbonized and polymerized at high temperature to prepare the C3N4There are problems of excessively low yield (yield less than 10%) and poor conductivity, thus limiting C to a great extent3N4The application field in electrochemistry. Therefore, development of C having high conductivity, simple synthesis, low cost and high electrochemical performance3N4The synthesis method has important significance.
Disclosure of Invention
The invention aims to provide a high-performance lithium ion battery C3N4The preparation method of the/carbon composite negative electrode material has the advantages of simplicity, easy process control and short period, and the C with high yield and high specific capacity is prepared by adopting a closed reaction method without adding any catalyst in the reaction process3N4A carbon negative electrode material.
The technical scheme of the invention is as follows:
high-performance lithium ion battery C3N4The preparation method of the/carbon composite cathode material is sequentially carried out according to the following steps,
(1) placing a precursor containing C and N elements and a liquid carbon source into a reactor, wherein the total volume of the two raw materials is less than 80% of the volume of the reactor, replacing the air in the reactor with argon, and sealing the reactor;
after the reactor is closed, the liquid carbon source changes from liquid phase to gas phase to solid phase in the heating processAnd finally in situ in solid phase carbon particles3N4In the in situ reaction, not only C is changed3N4The structure of the catalyst also changes the appearance of the catalyst, and the product has excellent electrochemical performance;
(2) heating the reactor to 400-600 ℃, preserving the heat for 1-4 h, and taking out the mixture after the reactor is naturally cooled to room temperature;
in the step, the precursor is carbonized and polymerized in a high-temperature environment, meanwhile, a liquid carbon source is firstly changed into a gas-phase carbon source, then the gas-phase carbon source is carbonized into a solid-phase carbon source under the high-temperature condition, and in the process that the liquid carbon source is changed from a liquid phase into the gas-phase carbon source and is finally carbonized into a solid phase, carbon atoms participate in the carbonization and polymerization of the precursor and the crystal growth process in situ and influence the structure and the appearance of the final material; in the invention, the reaction temperature and time not only influence the success or failure of carbonization polymerization and crystal growth of the precursor in a high-temperature environment, but also influence the phase change speed of the carbon source and the process and participation sites of in-situ participation reaction, the precursor and the carbon source are subjected to heat preservation for 1-4 h at 400-600 ℃, the final product becomes the nano carbon, and the addition of the carbon source in the process not only changes the C of the precursor and the carbon source3N4The original shape of the product also changes the structure of the product, the synthesized material has good crystallinity, and the product structure is mainly wound together in a circular structure, so that the generated C3N4The active sites are increased, and the active sites are one of the key factors for the excellent electrochemical performance of the cathode material;
(3) washing the mixture with distilled water and absolute ethyl alcohol respectively for 3-5 times in sequence, filtering, and drying the obtained powder in a drying oven to obtain the high-performance lithium ion battery C3N4A/carbon composite negative electrode material.
In step (1), the precursor containing two elements, namely C and N, is one of melamine, urea or thiourea.
As another limitation of the present invention, in the step (1), the liquid carbon source is N-methylpyrrolidone or acetonitrile.
As a third limitation of the present invention, in the step (2), the temperature increase rate is 1 to 5 DEG/min.
As a fourth limitation of the present invention, in the step (1), the total volume of the precursor containing two elements of C and N and the liquid carbon source is 30-60% of the volume of the reactor.
The invention also has a limitation that in the step (3), the drying temperature is 80-110 ℃, and the drying time is 8-12 h.
The step of the invention is integrated, the precursor containing carbon and nitrogen and the liquid carbon source are added into the reactor, and the synthesized C is obtained through closed reaction3N4The carbon yield is greatly improved, the yield of the cathode material is improved to more than 60 percent from the prior 10 percent, and carbon source is added in the synthesis reaction process to generate C3N4The carbon is carbonized into nano carbon in the process, and the C is obviously improved3N4The material has excellent electrochemical performance.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the raw materials are cheap and easy to obtain, the reaction condition is mild, the preparation method is simple, the process is easy to control, the repeatability is high, and the period is short;
2. to obtain C3N4The material is synthesized in a closed reactor, so that the yield is improved by more than 6 times compared with that of the conventional synthesis;
3. due to the addition of a liquid carbon source, so that the carbon source is in C3N4In-situ carbonization and compounding into C in the synthesis process3N4Structure of/C, morphology and structure in comparison with C3N4The material has good conductivity, excellent electrochemical performance and good rate performance, has specific capacity of 721mAh/g at 0.1 ℃, and is more than twice of the theoretical capacity of commercial graphite (372 mAh/g); meanwhile, the material has high mass specific capacity and good cycling stability;
4. low production cost, large-scale production and industrialized popularization.
The present invention will be described in further detail with reference to specific embodiments.
Drawings
FIG. 1 shows a graph of C obtained in example 1 of the present invention3N4Transmission electron microscope pictures of/C materials;
FIG. 2 shows C obtained in example 1 of the present invention3N4XRD pictures of/C materials;
FIG. 3 shows C obtained in example 2 of the present invention3N4Electron energy loss spectrum of/C material;
FIG. 4 shows C obtained in example 3 of the present invention3N4the/C material is used as a multiplying power diagram of the lithium ion battery cathode material under different current densities;
FIG. 5 shows C obtained in example 3 of the present invention3N4Cycling performance plot of the/C material at a current density of 0.2C.
Detailed Description
In the following examples, commercially available reagents were used unless otherwise specified, and the preparation methods and the test methods were conventional unless otherwise specified.
Example 1 a high Performance lithium ion Battery C3N4Preparation method of/carbon composite negative electrode material
This embodiment is a high performance lithium ion battery C3N4The preparation method of the/carbon composite negative electrode material is sequentially carried out according to the following steps:
(11) weighing 1kg of melamine-containing medicine with analytical purity and 1L of NMP (N-methylpyrrolidone), placing the melamine-containing medicine and the NMP into a reactor, enabling the total filling volume of the two raw materials to be 30% of the volume of the reactor (the volume of an inner cavity of the reactor), replacing the air in the reactor with argon, and then sealing the reactor;
(12) the reactor was heated to 500 ℃ at a heating rate of 1 ℃/min and the holding time was 4 hours. Then, after the reactor is naturally cooled to the room temperature, taking out the mixture;
(13) washing the above mixture with anhydrous ethanol and distilled water separately for 3 times, filtering, and standing the obtained powderVacuum drying at 80 deg.C for 12h in an air drying oven to obtain C with high quality and specific capacity3N4the/C composite negative electrode material.
FIG. 1 shows a graph of C obtained in example 1 of the present invention3N4Transmission electron microscopy of the/C material, it can be seen that the synthesized material is mainly intertwined with each other in a circular structure. FIG. 2 shows C obtained in example 1 of the present invention3N4XRD picture of/C material, it can be seen that the synthesized material has better crystallinity, corresponding to g-C3N4And PDF cards of carbon materials.
The preparation method is simple, the process is easy to control, and the material has good rate capability, higher specific capacity and good cycling stability.
Example 2A high Performance lithium ion Battery C3N4Preparation method of/carbon composite negative electrode material
(21) Weighing 2.2kg of urea-containing medicine with analytical purity and 2L of acetonitrile, placing the urea-containing medicine and the acetonitrile into a reactor, enabling the total filling volume of the two raw materials to be 60% of the volume of the reactor (the volume of an inner cavity of the reactor), replacing air in the reactor with argon, and then sealing the reactor;
(22) the reactor was heated to 400 ℃ at a rate of 5 ℃/min and the hold time was 3 hours. Then, after the reactor is naturally cooled to the room temperature, taking out the mixture;
(23) washing the above mixture with anhydrous ethanol and distilled water separately and centrifugally for 5 times, vacuum drying the obtained powder in vacuum drying oven at 110 deg.C for 8 hr to obtain C with high quality and specific capacity3N4the/C composite negative electrode material.
C made in this example3N4the/C material is mainly intertwined with each other in a circular structure and has better crystallinity, FIG. 3 shows the C obtained3N4The electron energy loss spectrum of/C, as can be seen from the figure, the synthesized material mainly comprises three elements of carbon, nitrogen and oxygen, wherein the oxygen appears due to the oxygen adsorbed on the surface of the sample in the test.
The preparation method is simple, the process is easy to control, and the material has good rate capability, higher specific capacity and good cycling stability.
Embodiment 3 a high-performance lithium ion battery C3N4Preparation method of/carbon composite negative electrode material
(31) Weighing 1.6kg of thiourea-containing medicine with analytical purity and 1.5L of NMP, placing the medicine and the NMP in a reactor, enabling the total filling volume of the two raw materials to be 50% of the volume of the reactor (the volume of an inner cavity of the reactor), replacing air in the reactor with argon, and then sealing the reactor;
(32) the reactor was heated to 600 ℃ at a rate of 3 ℃/min and the hold time was 1 hour. Then, after the reactor is naturally cooled to room temperature, taking out the mixture;
(33) centrifuging and washing the above mixture with anhydrous ethanol and distilled water for 4 times, respectively, vacuum drying the obtained powder in a vacuum drying oven at 100 deg.C for 10 hr to obtain C with high quality and specific capacity3N4the/C composite negative electrode material.
C made in this example3N4the/C material is mainly intertwined with each other in a circular structure and has better crystallinity, FIG. 4 shows C obtained in example 3 of the present invention3N4The multiplying power diagram of the/C material under different current densities when the material is used as the lithium ion battery cathode material can be seen from the diagram, the material has good multiplying power performance, has specific capacity of 721mAh/g under 0.1C, is more than twice of the theoretical capacity of commercial graphite (372 mAh/g), and has good application prospect. FIG. 5 shows C obtained in example 3 of the present invention3N4The cycle performance of the/C material at a current density of 0.2C is shown, and C can be seen from the graph3N4the/C has high specific capacity and good cycling stability when used as the negative electrode of the lithium ion battery.
The preparation method is simple, the process is easy to control, and the material has good rate capability, higher specific capacity and good cycling stability.
Example 4 comparative experiment
This embodiment is a C3N4The preparation method of the material comprises the following steps:
(41) weighing 2.2kg of melamine-containing medicine with analytical purity, placing the melamine-containing medicine into a reactor, and enabling the filling volume of the melamine-containing medicine to be 60% of the volume of the reactor (the volume of an inner cavity of the reactor);
(42) heating at a heating rate of 5 DEG/min under the protection of argon atmosphere, heating the reactor to 400 ℃, keeping the temperature for 3 hours, and then taking out the mixture after the reactor is naturally cooled to room temperature;
(43) centrifuging and washing the above mixture with anhydrous ethanol and distilled water for 5 times, vacuum drying the obtained powder in vacuum drying oven at 110 deg.C for 8 hr to obtain C3N4A material.
The following table shows C obtained in example 2 of the present invention3N4C-C composite obtained in this example3N4The material yield and the price are compared in a table, and as can be seen from the figure, the C obtained by adding the liquid carbon source for composite carbonization and carrying out closed reaction in the reactor in the technical scheme of the invention3N4The yield of the/C composite material is about 7 times higher than that of the composite material without adding a liquid carbon source and subjected to open reaction, and the price is about 7 times lower, so that the composite material has the advantages of low cost and high yield and is used for synthesizing the lithium ion battery cathode material.
Finally, it should be noted that: the above examples 1-3 are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (5)
1. High-performance lithium ion battery C3N4Carbon/carbon compositeThe preparation method of the cathode material is characterized by comprising the following steps: the steps are carried out in sequence according to the following steps,
(1) placing a precursor containing C and N elements and a liquid carbon source into a reactor, wherein the total volume of the two raw materials is less than 80% of the volume of the reactor, replacing the air in the reactor with argon, and sealing the reactor; the liquid carbon source is N-methyl pyrrolidone or acetonitrile;
(2) heating the reactor to 400-600 ℃, preserving the heat for 1-4 h, and taking out the mixture after the reactor is naturally cooled to room temperature;
(3) washing the mixture with distilled water and absolute ethyl alcohol respectively for 3-5 times in sequence, filtering, and drying the obtained powder in a drying oven to obtain the high-performance lithium ion battery C3N4A/carbon composite negative electrode material.
2. The high performance lithium ion battery C of claim 13N4The preparation method of the/carbon composite negative electrode material is characterized by comprising the following steps: in the step (1), the precursor containing two elements of C and N is one of melamine, urea or thiourea.
3. The high-performance lithium ion battery C according to claim 13N4The preparation method of the/carbon composite negative electrode material is characterized by comprising the following steps: in the step (2), the heating rate is 1-5 DEG/min.
4. The high-performance lithium ion battery C according to claim 13N4The preparation method of the/carbon composite negative electrode material is characterized by comprising the following steps: in the step (1), the total volume of the precursor containing the C and the N elements and the liquid carbon source is 30-60% of the total volume of the reactor.
5. The high-performance lithium ion battery C according to any one of claims 1 to 43N4The preparation method of the/carbon composite negative electrode material is characterized by comprising the following steps: in the step (3), the drying temperature is 80-110 ℃, and the drying time is 8～12h。
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| CN103745836A (en) * | 2013-12-29 | 2014-04-23 | 渤海大学 | A method for preparing a g-C3N4/carbon quantum dot composite electrode |
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