CN115411244A - Nitrogen-doped porous hard carbon negative electrode material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a preparation method of a biomass-derived nitrogen-doped porous hard carbon negative electrode material, which is mainly applied to the field of negative electrode materials of lithium ion batteries. The specific preparation method comprises the following steps: 1) Cutting silkworm cocoon into half pieces, and soaking in potassium chloride solution for 24-36 hr; 2) Carrying out hydrothermal treatment at 140-160 ℃ for 4-6h; 3) Vacuum drying silkworm cocoon at 60 deg.C for 6-8 hr; 4) Placing the prepared silkworm cocoons in a tube furnace, calcining for 3-5h at 700-1100 ℃ in an argon atmosphere; 5) Taking out the product, washing with deionized water for 3 times, soaking in deionized water for 24-36 hr, filtering, and vacuum drying at 60 deg.C; 6) Pulverizing, adding 3-5% asphalt, and mixing for 30min; 7) And (3) putting the mixture into a tube furnace, calcining for 2-4h at 800-1200 ℃ in an argon atmosphere to obtain the final product. The method has the advantages of simple preparation process, easily obtained raw materials, green and environment-friendly reaction reagents, porous microstructure of the final product, large specific surface, rich nitrogen, uniform distribution and the like. The lithium ion battery cathode material has good rate charging performance when being applied to lithium ion battery cathode materials.
Description
Technical Field
The invention relates to a preparation method and application of a nitrogen-doped porous hard carbon negative electrode material, belonging to the field of negative electrode materials of lithium ion batteries.
Background
The proposal of the double-carbon strategy shows a new trend of practicing green, environment-friendly and low-carbon development in China. Demands in the fields of new energy automobiles, energy storage power stations and digital tools are rapidly outbreaked, and the well-drawn lithium ion batteries are concerned by the market, and meanwhile, more severe requirements such as long service life, quick charging, safety and the like are also provided for the lithium ion batteries. Most of the current mainstream commercial lithium ion battery cathode materials are graphite carbon materials, but the defects of poor rate capability and the like cannot meet the market demand, so that modification design needs to be carried out from the graphite materials.
The graphite carbon material has the advantages of excellent conductivity, mature production system, abundant raw material sources and the like. Since the first commercial lithium ion battery using graphite as the negative electrode material was successfully developed by sony corporation, the graphite carbon material has also been occupying a major share of the negative electrode material market. Generally, graphitic carbon materials can be classified into graphite, soft carbon, hard carbon, and the like. The hard carbon precursor is mainly derived from natural products and artificial polymers, and the biomass material belongs to common natural products, such as herbaceous plants, woody plants and biomass wastes.
Hard carbon refers to polymeric pyrolytic carbon that is difficult to graphitize, including randomly oriented short-range ordered few-layered graphitic lamellar domains, nanopores, and amorphous carbon domains. However, hard carbon has problems of low first efficiency, poor charge rate performance, and the like.
The porous structure has developed pores and larger specific surface area, and internal defects can provide abundant lithium storage sites and increase reactive sites in the charging and discharging process. Meanwhile, the abundant pore distribution can effectively shorten the diffusion distance of lithium ions in the carbon cathode material, greatly accelerate ion transfer, improve the integral rate capability and prolong the cycle life. The introduction of the heteroatom can also improve the electrical property of the material, for example, the doping of nitrogen element often forms pyridine nitrogen, pyrrole nitrogen and graphite nitrogen structures and large pi bond electron distribution, which are all helpful for improving the conductivity of the material.
The biomass carbon material is naturally rich in various heteroatoms such as elements of nitrogen, sulfur and the like, a porous structure can be obtained after pore-forming treatment and pyrolysis carbonization, and the introduction of the structures and the heteroatoms not only increases the contact area with electrolyte and provides more lithium storage sites, but also can improve the conductivity and rate capability of the material. Meanwhile, the larger specific surface area can generate more solid electrolyte interface films in the first charging and activating process, consume more lithium sources and reduce the overall first efficiency. Therefore, proper pore-forming treatment and pyrolysis carbonization need to be selected, the porous structure of the material is reasonably regulated and controlled, and the number, size and distribution of micropores, mesopores and macropores are optimized. The method comprises the steps of selecting KCl as a pore forming agent, using silk as a carbon source and a nitrogen source, soaking the silk in a KCl solution to enable the pore forming agent to be uniformly distributed on the surface of the silk, and carrying out pyrolysis carbonization and asphalt coating to obtain the nitrogen-doped porous carbon material. These can greatly accelerate ion transfer and improve the overall rate capability.
Disclosure of Invention
Based on the background, the invention provides a preparation method and application of a nitrogen-doped porous hard carbon negative electrode material. The method is characterized in that silk is used as a raw material, and by means of the natural nitrogen-containing characteristic of the silk, the nitrogen-doped porous carbon material can be obtained after the silk is soaked in a KCl solution and pyrolyzed and carbonized. The specific surface area and pore distribution of the porous carbon material are further regulated and controlled by adjusting the concentration of the KCl solution and the pyrolysis carbonization temperature, and finally the nitrogen-doped porous hard carbon negative electrode material is obtained. In this design model, the introduction of porous structure and heteroatom had both increased with electrolyte area of contact, provided more lithium storage sites, and abundant pore distribution can effectively shorten the diffusion distance of lithium ion in carbon negative electrode material, greatly accelerated the ion transfer, promoted the electric conductivity and the multiplying power performance of material, was favorable to satisfying the demand of current market to the aspect of filling soon.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention also provides a nitrogen-doped porous hard carbon cathode material, the microstructure of which is a honeycomb-shaped and porous structure, the pore diameter is distributed between 2 nm and 10nm, the pore diameter is uniformly distributed on the surface of the material, and the specific surface area is 5m to 15 m 2 The nitrogen content is 4-15 percent.
A preparation method of a nitrogen-doped porous hard carbon negative electrode material comprises the following specific steps:
1) Removing silkworm pupa from silkworm cocoon, cleaning with deionized water, and cutting half to half for use;
2) Heating 300g of deionized water to 60-80 ℃, adding 100-200g of KCl, stirring to prepare a KCl solution at 80 ℃, soaking the stand horse in the prepared silkworm cocoon, stopping heating the KCl solution, cooling to room temperature, and keeping the soaking time for 24-36h;
3) Carrying out hydrothermal treatment at 140-160 ℃ for 4-6h;
4) Taking out the silkworm cocoon, standing in a fume hood for 30-45min, and drying in a vacuum drying oven at 60 deg.C;
5) Placing the dried silkworm cocoons in a tube furnace, calcining for 3-5h at 700-1100 ℃ in an argon atmosphere;
6) Obtaining the product in the step 5), washing the product for 3 times by using deionized water, then soaking the product for 24 to 36 hours by using the deionized water, filtering the product, and drying the product in vacuum at 60 ℃;
7) Grinding and crushing the product obtained in the step 6) to obtain a final product.
Preferably, the preparation method of the nitrogen-doped porous hard carbon negative electrode material comprises the following steps
1) The silkworm cocoon in the step 1) is one of a mulberry silkworm cocoon, an oak silkworm cocoon and a castor silkworm cocoon;
2) The solution in the step 2) is KCl, naCl or KNO 3 The preparation temperature of the KCl solution is 60-80 ℃, and the heating is stopped after the silkworm cocoons are added;
3) The hydrothermal treatment temperature in the step 3) is 140-160 ℃, and the time is 4-6h;
4) Standing the fume hood in the step 4) for 30-45min, and performing vacuum drying at the temperature of 50-60 ℃ under the vacuum degree of-80-95 kPa;
5) In the step 5), the carbonization equipment is one of a tubular carbonization furnace, a box-type carbonization furnace, a roller kiln and a pushed slab kiln, the protective atmosphere is one of argon and helium, the calcination temperature is 700-1000 ℃, and the calcination time is 3-5h;
6) Washing the product in the step 6) for 3 times by using deionized water, soaking for 24-36h, filtering, and carrying out vacuum drying at the temperature of 50-60 ℃ and under the vacuum degree of-80-95 kPa;
7) In the step 7), the crushing equipment is one of a mechanical mill, an air flow mill or a ball mill, and the proportion of asphalt is 3-5%;
8) In the step 8), the carbonization equipment is one of a tubular carbonization furnace, a box-type carbonization furnace, a roller kiln and a pushed slab kiln, the protective atmosphere is one of argon and helium, the calcination temperature is 800-1200 ℃, and the calcination time is 2-4h.
The method utilizes natural nitrogen-rich biological carbon material, namely silk, and regulates the specific surface area and pore distribution of the porous carbon material by adjusting the concentration of a KCl solution and the pyrolysis carbonization temperature, thereby finally obtaining the nitrogen-doped porous hard carbon cathode material. The porous structure and the introduction of the hetero atoms increase the contact area with the electrolyte and provide more lithium storage sites in the charging process, the diffusion distance of lithium ions in the carbon cathode material can be effectively shortened by rich pore distribution, the ion transfer is greatly accelerated, the conductivity and the rate capability of the material are improved, and the assembled lithium ion battery has excellent electrochemical performance finally.
Drawings
Fig. 1 is an SEM picture of the nitrogen-doped porous carbon material prepared in example one.
Fig. 2 is an XRD pattern of the nitrogen-doped porous carbon material prepared in example one.
Fig. 3 is a raman spectrum of the nitrogen-doped porous carbon material prepared in example one.
Fig. 4 is a charge and discharge curve diagram of the nitrogen-doped porous carbon material prepared in example one.
Fig. 5 is a graph comparing the rate capability of the nitrogen-doped porous carbon material prepared in example one and the nitrogen-doped porous carbon material prepared in example two and the nitrogen-doped carbon material prepared in comparative example one.
Detailed Description
The process provided by the present invention is further illustrated by the following examples, to which the invention is not limited.
Example one
Removing silkworm pupa from silkworm cocoon, cleaning with deionized water, and cutting half to half for use; heating 300g of deionized water to 60-80 ℃, adding 100-200g of KCl, stirring to obtain a KCl solution at 80 ℃, immersing the stand horse in the prepared silkworm cocoon, stopping heating the KCl solution, cooling to room temperature, and keeping the immersion time for 24 hours; carrying out hydrothermal treatment at 140 ℃ for 4h; taking out the silkworm cocoon, standing in a fume hood for 30-45min, and drying in a vacuum drying oven at 60 deg.C; placing the dried silkworm cocoons in a tube furnace, calcining for 4 hours at 900 ℃ in an argon atmosphere; obtaining a product, washing the product with deionized water for 3 times, then soaking the product in the deionized water for 24 hours, filtering the product, and drying the product in vacuum at 60 ℃; pulverizing, adding 3% asphalt, and mixing for 30min; placing the mixture in a tube furnace, calcining for 4h at 1100 ℃ under the argon atmosphere; and screening to obtain the nitrogen-doped porous carbon material.
The prepared composite material, carbon black, CMC and SBR are homogenized, coated and rolled according to the proportion of 96.
The SEM of the prepared nitrogen-doped porous carbon material is shown in figure 1, and the figure shows that honeycomb and porous structures with large specific surface area are successfully prepared. Fig. 2 is an XRD pattern of the nitrogen-doped porous carbon material, from which it can be known that a characteristic diffraction peak appears at 24.2 °, corresponding to the (002) crystal face of carbon, and according to the bragg formula, the interlayer spacing is 0.3675nm, which is favorable for rapid insertion and extraction of lithium ions. FIG. 3 is a Raman diagram of a nitrogen-doped porous carbon material at 1579cm -1 And 1340cm -1 Two obvious broad peaks are present, corresponding to the characteristic peaks of graphene: g peak and D peak.
From the charge-discharge curve chart of fig. 4, we can see that the reversible discharge gram capacity of the prepared nitrogen-doped porous carbon material reaches 405.9mAh/g under the condition of 40 mA.
From the rate performance graph of fig. 5, we can see that the reversible discharge capacities of the prepared nitrogen-doped porous carbon material reach 407.2, 328.3, 268.8, 224.2, 200.6 and 168.1mAh/g under the conditions of 40, 80, 200, 400, 800 and 2000 mA/g.
Example two
Removing silkworm pupa from silkworm cocoon, cleaning with deionized water, and cutting half to half for use; heating 300g of deionized water to 60-80 ℃, adding 100-200g of KCl, stirring to obtain a KCl solution at 80 ℃, soaking immediately in the prepared silkworm cocoon, stopping heating the KCl solution, cooling to room temperature, and keeping the soaking time for 24 hours; carrying out hydrothermal treatment at 140 ℃ for 4h; taking out the silkworm cocoon, standing in a fume hood for 30-45min, and drying in a vacuum drying oven at 60 deg.C; placing the dried silkworm cocoons in a tube furnace, calcining for 4 hours at 700 ℃ in an argon atmosphere; obtaining a product, washing the product with deionized water for 3 times, then soaking the product in the deionized water for 24 hours, filtering the product, and drying the product in vacuum at the temperature of 60 ℃; pulverizing, adding 3% asphalt, and mixing for 30min; placing the mixture in a tube furnace, calcining for 4 hours at 1100 ℃ under the argon atmosphere; and screening to obtain the nitrogen-doped porous carbon material.
The prepared composite material, carbon black, CMC and SBR are homogenized, coated and rolled according to a ratio of 96.
From the rate performance diagram of fig. 5, it can be seen that the reversible discharge capacities of the prepared nitrogen-doped porous carbon material reach 324.1, 264.2, 200.8, 160.2, 145.2 and 130.8mAh/g under the conditions of 40, 80, 200, 400, 800 and 2000 mA/g.
Comparative example 1
Removing silkworm pupa from silkworm cocoon, cleaning with deionized water, and cutting into halves; carrying out hydrothermal treatment on the silkworm cocoons for 4 hours at 140 ℃; taking out the silkworm cocoon, standing in a fume hood for 30-45min, and drying in a vacuum drying oven at 60 deg.C; placing the dried silkworm cocoons in a tubular furnace, and calcining for 4 hours at 900 ℃ in an argon atmosphere; obtaining a product, washing the product with deionized water for 3 times, then soaking the product in the deionized water for 24 hours, filtering the product, and drying the product in vacuum at the temperature of 60 ℃; pulverizing, adding 3% asphalt, and mixing for 30min; placing the mixture in a tube furnace, calcining for 4 hours at 1100 ℃ under the argon atmosphere; obtaining the nitrogen-doped carbon material.
The prepared composite material, carbon black, CMC and SBR are homogenized, coated and rolled according to the proportion of 96.
From the rate performance diagram of fig. 5, it can be seen that the reversible discharge capacities of the prepared nitrogen-doped porous carbon material reach 270.3, 206.9, 162.4, 147.1, 132.3 and 117.3mAh/g under the conditions of 40, 80, 200, 400, 800 and 2000 mA/g.
It can be seen from the above examples and comparative examples that the nitrogen-doped porous carbon material prepared by the present invention has a large specific surface area and exhibits excellent rate capability owing to its honeycomb and porous structure.
Claims (10)
1. A nitrogen-doped porous hard carbon negative electrode material is characterized in that: the microstructure is cellular and porous, the pore diameter is distributed at 2-10nm, the pore diameter is uniformly distributed on the surface of the material, and the specific surface area is 5-15 m 2 G, nitrogen content 4-15%.
2. A preparation method of a nitrogen-doped porous hard carbon negative electrode material is characterized by comprising the following steps:
(1) Removing silkworm pupa from silkworm cocoon, cleaning with deionized water, and cutting into halves for use;
(2) Heating 300g of deionized water to 60-80 ℃, adding 100-200g of KCl, stirring to prepare a KCl solution at 80 ℃, soaking the stand horse in the prepared silkworm cocoon, stopping heating the KCl solution, cooling to room temperature, and keeping the soaking time for 24-36h;
(3) Transferring the mixture into a high-pressure reaction kettle, and carrying out hydrothermal treatment at 140-160 ℃ for 4-6h;
(4) Taking out the silkworm cocoon, standing in a fume hood for 30-45min, and drying in a vacuum drying oven at 60 deg.C;
(5) Placing the dried silkworm cocoons in a tube furnace, calcining for 3-5h at 700-1100 ℃ in an argon atmosphere;
(6) Obtaining the product in the step 5), washing the product with deionized water for 3 times, then soaking the product in the deionized water for 24 to 36 hours, filtering the product and drying the product in vacuum at the temperature of 60 ℃;
(7) Grinding and crushing the product obtained in the step 6), adding 3-5% of asphalt, and mixing for 30min;
(8) And (3) putting the mixture into a tube furnace, calcining for 2-4h at 800-1200 ℃ in an argon atmosphere to obtain the final product.
3. The preparation method of the nitrogen-doped porous hard carbon anode material according to claim 2, characterized by comprising the following steps: the silkworm cocoon in the step 1) is one of a mulberry silkworm cocoon, an oak silkworm cocoon and a castor silkworm cocoon.
4. The method for preparing the nitrogen-doped porous hard carbon anode material according to claim 2, wherein the method comprises the following steps: the solution in the step 2) is KCl, naCl or KNO 3 The KCl solution is prepared at 60-80 deg.C, and heating is stopped after adding silkworm cocoon.
5. The method for preparing the nitrogen-doped porous hard carbon anode material according to claim 2, wherein the method comprises the following steps: the hydrothermal treatment temperature in the step 3) is 140-160 ℃, and the time is 4-6h.
6. The method for preparing the nitrogen-doped porous hard carbon anode material according to claim 2, wherein the method comprises the following steps: and step 4), standing for 30-45min in a fume hood, and performing vacuum drying at the temperature of 50-60 ℃ under the vacuum degree of-80-95 kPa.
7. The method for preparing the nitrogen-doped porous hard carbon anode material according to claim 2, wherein the method comprises the following steps: in the step 5), the carbonization equipment is one of a tubular carbonization furnace, a box-type carbonization furnace, a roller kiln and a pushed slab kiln, the protective atmosphere is one of argon and helium, the calcination temperature is 700-1100 ℃, and the calcination time is 3-5h.
8. The method for preparing the nitrogen-doped porous hard carbon anode material according to claim 2, wherein the method comprises the following steps: washing the product in the step 6) for 3 times by using deionized water, soaking for 24-36h, filtering, and carrying out vacuum drying at the temperature of 50-60 ℃ and under the vacuum degree of-80-95 kPa; in the step 7), the crushing equipment is one of a mechanical mill, an air flow mill or a ball mill, and the proportion of the asphalt is 3-5%.
9. The method for preparing the nitrogen-doped porous hard carbon anode material according to claim 2, wherein the method comprises the following steps: and 8) the carbonization equipment is one of a tubular carbonization furnace, a box-type carbonization furnace, a roller kiln and a pushed slab kiln, the protective atmosphere is one of argon and helium, the calcination temperature is 800-1200 ℃, and the calcination time is 2-4h.
10. The application of the nitrogen-doped porous hard carbon negative electrode material is characterized in that: the nitrogen-doped porous hard carbon negative electrode material of claim 1 is applied in a lithium ion battery.
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CN116632221B (en) * | 2023-07-24 | 2024-02-09 | 深圳海辰储能控制技术有限公司 | Negative electrode material, preparation method thereof, negative electrode plate, energy storage device and power utilization device |
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