CN112349896A - Flexible hollow carbon nanofiber/tin disulfide composite electrode and preparation method thereof - Google Patents
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Abstract
The invention belongs to the field of negative electrode materials of sodium ion batteries in new energy materials, and discloses a flexible hollow carbon nanofiber/tin disulfide composite electrode and a preparation method thereof. The preparation process comprises the following steps: carrying out coaxial electrostatic spinning, curing and carbonizing on polyacrylonitrile and polymethyl methacrylate spinning stock solution to obtain hollow carbon fibers; the hollow carbon fiber is subjected to hydrothermal reaction and calcination to obtain the flexible hollow carbon nanofiber/tin disulfide composite electrode material. The tin disulfide nanosheets prepared in the invention grow on the inner and outer surfaces of the hollow carbon nanofiber, so that the loading capacity of tin disulfide can be increased, the transmission distance of de-intercalated ions in the material in the charging and discharging process can be reduced, and the storage capacity can be improved, thereby improving the cycle performance and the rate capability of the battery. The stable three-dimensional structure and the internal hollow structure of the whole electrode material can effectively buffer the volume change of the tin disulfide in the electrochemical reaction process, so that the pulverization of the structure of the electrode material is relieved, and the high conductivity of the hollow carbon nanofiber can effectively improve the conductivity of the composite material. And the material has flexibility, and the whole preparation process can greatly simplify the preparation process of the battery electrode material.
Description
Technical Field
The invention belongs to the field of negative electrode materials of sodium ion batteries in new energy materials, and particularly relates to a flexible hollow carbon nanofiber/tin disulfide composite electrode and a preparation method thereof.
Background
In the modern society, the storage and conversion of energy have become important problems restricting the sustainable development of the world economy. Lithium ion batteries have conquered the portable electronic market by having the advantages of high operating voltage, high capacity, small self-discharge, long cycle life, etc. However, with the real arrival of the era of electric vehicles and smart grids, the global lithium resource will not be enough to meet the huge demand of the future lithium ion battery market. Therefore, it is very critical to develop other cheap related energy storage technologies that can replace lithium ion batteries. Sodium ion batteries have a similar charge and discharge mechanism as lithium ion batteries, and sodium resources are far more abundant than lithium, so sodium ion batteries are an ideal substitute for lithium ion batteries.
The electrode material is a key problem in the sodium ion battery technology, and as for the negative electrode material, the novel sodium ion battery negative electrode material mainly comprises the following components: carbon-based materials, metal or alloy materials, titanate materials, organic materials, metal sulfide materials, etc., which have a high theoretical specific capacity and a special two-dimensional layered structure due to their multi-electron electrochemical reaction mechanism, are rapidly becoming hot spots of research. In addition, with the development of flexible electronic books, flexible mobile phones and wearable electronic watches, and some portable medical electronic devices, the demand for flexible batteries is increasing. Therefore, the research and development of the high-capacity foldable flexible sodium-ion battery cathode material has important practical significance.
Tin disulfide with high theoretical specific capacity is a sodium ion battery negative electrode material which is widely researched, however, the tin disulfide-based negative electrode material can generate great volume expansion in the circulating process, and the electrode material is pulverized and falls off. In addition, tin disulfide as a sodium ion battery negative electrode material also faces the problem of its inherent poor conductivity. The problem can be effectively solved by constructing nano-scale tin disulfide and compounding the nano-scale tin disulfide with a carbon material with better conductivity.
The chinese patent application No. 201810170239.1 discloses a carbon-coated composite material having a hollow core-shell structure, wherein an outer coating layer is a hollow carbon shell, a nano-sheet is disposed in the hollow carbon shell, and a space gap is reserved between the nano-sheet and the hollow carbon shell. Because the space is reserved between the nano sheet and the hollow carbon shell, the volume change caused by ion deintercalation can be effectively buffered, and the battery cycle performance of the material can be effectively improved. However, the composite material is not flexible, and the electrode preparation process needs to add a binder and a conductive agent to coat the composite material on a metal current collector, which cannot meet the requirements of the current flexible devices.
Disclosure of Invention
The invention aims to solve the technical problems of low strength, small load capacity, poor self-supporting effect, poor flexibility, use of a binder and the like of the conventional composite electrode, and provides a flexible hollow carbon nanofiber/tin disulfide composite electrode and a preparation method thereof, wherein the hollow carbon nanofiber is used as a substrate material for loading tin disulfide, and the expanded interlayer spacing of the tin disulfide is beneficial to the embedding and the separation of sodium ions on the electrode material and is beneficial to the acceleration of the conduction of the sodium ions and electrons; the tin disulfide of hollow structure internal load can increase unit load, alleviates the volume expansion that tin disulfide takes place in the electrochemical reaction process. The flexible hollow carbon nanofiber/tin disulfide composite electrode material prepared by the invention has high specific capacity and good rate capability.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a flexible hollow carbon nanofiber/tin disulfide composite electrode is prepared by the following preparation method:
(1) taking a polymethyl methacrylate solution as an inner layer spinning solution; using polyacrylonitrile solution as outer spinning solution;
(2) carrying out coaxial electrostatic spinning, curing and carbonization on the inner layer spinning solution and the outer layer spinning solution to obtain hollow carbon nanofibers;
(3) immersing the hollow carbon nanofiber into a hydrothermal reaction solution, carrying out ultrasonic treatment for 30-90min, and reacting for 3-9h at the temperature of 100-150 ℃ to obtain a precursor of the hollow carbon nanofiber/tin disulfide composite material; the hydrothermal reaction liquid is obtained by dissolving tin tetrachloride pentahydrate and thioacetamide in absolute ethyl alcohol and magnetically stirring for 30-40min, wherein the molar ratio of the tin tetrachloride pentahydrate to the thioacetamide is (1-3) to 5;
(4) and heating the precursor of the hollow carbon nanofiber/tin disulfide composite material to 200-400 ℃ at a speed of 1-4 ℃/min, calcining, and keeping the temperature for 60-180min to obtain the flexible hollow carbon nanofiber/tin disulfide composite electrode.
Further, the specific steps for preparing the spinning solution in the step (1) are as follows:
dissolving polyacrylonitrile in N, N-dimethylformamide, and continuously stirring to obtain an outer-layer spinning solution with solid content of 10-15%; dissolving polymethyl methacrylate in N, N-dimethylformamide, and continuously stirring to obtain an outer-layer spinning solution with solid content of 10-15%.
Further, the electrostatic spinning process in the step (2) is to spin the spinning solution under the conditions that the spinning voltage is 10KV-20KV and the spinning distance is 10-20cm, so as to obtain the primary spinning fiber.
Further, the solidification process in the step (2) is to heat the spun fiber obtained by electrostatic spinning to 150-300 ℃ at 4-6 ℃/min in the air atmosphere, and solidify for 1-3h at constant temperature to obtain the solidified fiber.
Further, the carbonization process in the step (2) is to heat up to 700-.
A preparation method of the flexible hollow carbon nanofiber/tin disulfide composite electrode comprises the following steps:
(1) taking a polymethyl methacrylate solution as an inner layer spinning solution; using polyacrylonitrile solution as outer spinning solution;
(2) carrying out coaxial electrostatic spinning, curing and carbonization on the inner layer spinning solution and the outer layer spinning solution to obtain hollow carbon nanofibers;
(3) immersing the hollow carbon nanofiber into a hydrothermal reaction solution, carrying out ultrasonic treatment for 30-90min, and reacting for 3-9h at the temperature of 100-150 ℃ to obtain a precursor of the hollow carbon nanofiber/tin disulfide composite material; the hydrothermal reaction liquid is obtained by dissolving tin tetrachloride pentahydrate and thioacetamide in absolute ethyl alcohol and magnetically stirring for 30-40min, wherein the molar ratio of the tin tetrachloride pentahydrate to the thioacetamide is (1-3) to 5;
(4) and heating the precursor of the hollow carbon nanofiber/tin disulfide composite material to 200-400 ℃ at a speed of 1-4 ℃/min, calcining, and keeping the temperature for 60-180min to obtain the flexible hollow carbon nanofiber/tin disulfide composite electrode.
The invention has the beneficial effects that:
the invention provides a flexible hollow carbon nanofiber/tin disulfide composite electrode and a preparation method thereof, which have good sodium storage performance and excellent electrochemical performance when used as a sodium ion battery. The tin disulfide nanosheet grows in the inside and the external surface of the hollow carbon nanofiber, so that the capacity of tin disulfide can be increased, the transmission distance of de-embedded ions in the material in the charging and discharging process is reduced, and the storage capacity is improved, so that the cycle performance and the rate capability of the battery are improved. The stable three-dimensional structure and the internal hollow structure of the whole electrode material can effectively buffer the volume change of the tin disulfide in the electrochemical reaction process, so that the pulverization of the structure of the electrode material is relieved, and the high conductivity of the hollow carbon nanofiber can effectively improve the conductivity of the composite material. And the material has flexibility, the whole preparation process can greatly simplify the preparation process of the battery electrode material, and the preparation method has large-scale and industrialized prospects.
Drawings
Fig. 1 is a scanning electron microscope image of the flexible hollow carbon nanofiber/tin disulfide composite electrode prepared in example 1.
Fig. 2 is an optical photograph of the flexible hollow carbon nanofiber/tin disulfide composite electrode prepared in example 1.
Detailed Description
The present invention is further described in detail below by way of specific examples, which will enable one skilled in the art to more fully understand the present invention, but which are not intended to limit the invention in any way.
Example 1
Weighing 1.95g of polyacrylonitrile, dissolving in 17.55g N, N-dimethylformamide at 60 ℃ to prepare 10 wt% of N, N-dimethylformamide solution of polyacrylonitrile; 1.95g of polymethyl methacrylate was weighed and dissolved in 11.05g N, N-dimethylformamide at 60 ℃ to prepare a 15 wt% solution of polymethyl methacrylate in N, N-dimethylformamide. And stirring uniformly to obtain the spinning solution.
Carrying out coaxial electrostatic spinning, wherein the spinning parameters are as follows: the spinning voltage interval is 20KV, and the spinning distance is 10 cm. And (3) heating the obtained spun fiber to 150 ℃ at the heating rate of 4 ℃/min in the air atmosphere, and keeping the temperature for 2h for curing. And (3) placing the cured fiber in a large-cavity atmosphere furnace, heating to 700 ℃ at a speed of 4 ℃/min under the protection of argon, keeping the temperature for 30min, heating to 1100 ℃ at a speed of 4 ℃/min, and keeping the temperature for 30min, thereby obtaining the hollow carbon nanofiber. 0.6312g of tin tetrachloride pentahydrate and 0.2254g of thioacetamide (the molar ratio of the tin tetrachloride pentahydrate to the thioacetamide is 3: 5) are dissolved in 60mL of absolute ethanol, and the mixture is magnetically stirred for 30min to prepare a hydrothermal reaction solution. And (3) putting the hollow carbon nanofibers into the hydrothermal reaction solution, and performing ultrasonic treatment for 30 min. And transferring the hollow carbon nanofiber and the hydrothermal reaction solution into a liner of a reaction kettle, and reacting for 9 hours at 100 ℃ to obtain a precursor of the hollow carbon nanofiber/tin disulfide composite material. And (3) calcining the precursor in a tubular atmosphere furnace, heating to 200 ℃ at a speed of 4 ℃/min under the protection of argon, and keeping the temperature for 180min, thereby obtaining the flexible hollow carbon nanofiber/tin disulfide composite material.
Electrochemical tests show that the charge-discharge rate of the material is 0.05A g when the charge-discharge voltage range is 0.01-3V-1Under the condition, the reversible capacity reaches 365mAh g-1。
Example 2
Weighing 1.95g of polyacrylonitrile, dissolving in 15.78g N, N-dimethylformamide at 60 ℃ to prepare an N, N-dimethylformamide solution of 11 wt% of polyacrylonitrile; 1.95g of polymethyl methacrylate was weighed and dissolved in 13.05g N, N-dimethylformamide at 60 ℃ to prepare a 13 wt% solution of polymethyl methacrylate in N, N-dimethylformamide. And stirring uniformly to obtain the spinning solution.
Carrying out coaxial electrostatic spinning, wherein the spinning parameters are as follows: the spinning voltage interval is 15KV, and the spinning distance is 12 cm. And (3) heating the obtained spun fiber to 200 ℃ at the heating rate of 6 ℃/min in the air atmosphere, and keeping the temperature for 3 hours for curing. And (3) placing the cured fiber in a large-cavity atmosphere furnace, heating to 800 ℃ at the speed of 6 ℃/min under the protection of argon, keeping the temperature for 60min, heating to 1100 ℃ at the speed of 6 ℃/min, and keeping the temperature for 60min, thereby obtaining the hollow carbon nanofiber. 0.4208g of tin tetrachloride pentahydrate and 0.2254g of thioacetamide (the molar ratio of the tin tetrachloride pentahydrate to the thioacetamide is 2: 5) are dissolved in 60mL of absolute ethanol, and the mixture is magnetically stirred for 35min to prepare a hydrothermal reaction solution. And (3) putting the hollow carbon nanofibers into the hydrothermal reaction solution, and performing ultrasonic treatment for 60 min. And transferring the hollow carbon nanofiber and the hydrothermal reaction solution into a liner of a reaction kettle, and reacting for 6 hours at 120 ℃ to obtain a precursor of the hollow carbon nanofiber/tin disulfide composite material. And (3) calcining the precursor in a tubular atmosphere furnace, heating to 300 ℃ at a speed of 3 ℃/min under the protection of argon, and keeping the temperature for 120min, thereby obtaining the flexible hollow carbon nanofiber/tin disulfide composite material.
Electrochemical tests show that the charge-discharge rate of the material is 0.05A g when the charge-discharge voltage range is 0.01-3V-1Under the condition of (2), the reversible capacity reaches 402mAh g-1。
Example 3
Weighing 1.95g of polyacrylonitrile, dissolving in 14.3g N, N-dimethylformamide at 60 ℃ to prepare 12 wt% of N, N-dimethylformamide solution of polyacrylonitrile; 1.95g of polymethyl methacrylate was weighed and dissolved in 14.3g N, N-dimethylformamide at 60 ℃ to prepare a 12 wt% solution of polymethyl methacrylate in N, N-dimethylformamide. And stirring uniformly to obtain the spinning solution.
Carrying out coaxial electrostatic spinning, wherein the spinning parameters are as follows: the spinning voltage interval is 13KV, and the spinning distance is 15 cm. And (3) heating the obtained spun fiber to 250 ℃ at the heating rate of 5 ℃/min in the air atmosphere, and keeping the temperature for 1h for curing. And (3) placing the cured fiber in a large-cavity atmosphere furnace, heating to 800 ℃ at the speed of 5 ℃/min under the protection of argon, keeping the temperature for 60min, heating to 1000 ℃ at the speed of 5 ℃/min, and keeping the temperature for 60min, thereby obtaining the hollow carbon nanofiber. 0.2104g of tin tetrachloride pentahydrate and 0.2254g of thioacetamide (the molar ratio of the tin tetrachloride pentahydrate to the thioacetamide is 1: 5) are dissolved in 60mL of absolute ethanol, and the mixture is magnetically stirred for 30min to prepare a hydrothermal reaction solution. And (3) putting the hollow carbon nanofibers into the hydrothermal reaction solution, and performing ultrasonic treatment for 60 min. And transferring the hollow carbon nanofiber and the hydrothermal reaction solution into a liner of a reaction kettle, and reacting for 6 hours at 120 ℃ to obtain a precursor of the hollow carbon nanofiber/tin disulfide composite material. And (3) calcining the precursor in a tubular atmosphere furnace, heating to 350 ℃ at a speed of 2 ℃/min under the protection of argon, and keeping the temperature for 90min, thereby obtaining the flexible hollow carbon nanofiber/tin disulfide composite material.
Electrochemical tests show that the charge-discharge rate of the material is 0.05A g when the charge-discharge voltage range is 0.01-3V-1Under the condition of (1), the reversible capacity reaches 461mAh g-1。
Example 4
Weighing 1.95g of polyacrylonitrile, dissolving in 11.05g N, N-dimethylformamide at 60 ℃ to prepare a 15 wt% polyacrylonitrile N, N-dimethylformamide solution; 1.95g of polymethyl methacrylate was weighed and dissolved in 17.55g N, N-dimethylformamide at 60 ℃ to prepare a 10 wt% N, N-dimethylformamide solution of polymethyl methacrylate. And stirring uniformly to obtain the spinning solution.
Carrying out coaxial electrostatic spinning, wherein the spinning parameters are as follows: the spinning voltage interval is 10KV, and the spinning distance is 20 cm. And (3) heating the obtained spun fiber to 300 ℃ at the heating rate of 5 ℃/min in the air atmosphere, and keeping the temperature for 2h for curing. And (3) placing the cured fiber in a large-cavity atmosphere furnace, heating to 900 ℃ at the speed of 5 ℃/min under the protection of argon, keeping the temperature for 90min, heating to 1000 ℃ at the speed of 5 ℃/min, and keeping the temperature for 90min, thereby obtaining the hollow carbon nanofiber. 0.4208g of tin tetrachloride pentahydrate and 0.2254g of thioacetamide (the molar ratio of the tin tetrachloride pentahydrate to the thioacetamide is 2: 5) are dissolved in 60mL of absolute ethanol, and the mixture is magnetically stirred for 40min to prepare a hydrothermal reaction solution. And (3) putting the hollow carbon nanofibers into the hydrothermal reaction solution, and performing ultrasonic treatment for 90 min. And transferring the hollow carbon nanofiber and the hydrothermal reaction solution into a liner of a reaction kettle, and reacting for 3 hours at 150 ℃ to obtain a precursor of the hollow carbon nanofiber/tin disulfide composite material. And (3) calcining the precursor in a tubular atmosphere furnace, heating to 400 ℃ at a speed of 1 ℃/min under the protection of argon, and keeping the temperature for 60min, thereby obtaining the flexible hollow carbon nanofiber/tin disulfide composite material.
Electrochemical tests show that the charge-discharge rate of the material is 0.05A g when the charge-discharge voltage range is 0.01-3V-1Under the condition, the reversible capacity reaches 410mAh g-1。
Therefore, the flexible hollow carbon nanofiber/tin disulfide composite electrode material synthesized by the method has excellent electrochemical performance, and meanwhile, the flexible hollow carbon nanofiber/tin disulfide composite electrode material has the characteristics of self-support and flexibility, so that the problems that the hollow carbon nanofiber/tin disulfide composite material is low in strength and small in load, and a binder and a conductive agent are used in the electrode manufacturing process are solved, and the flexible hollow carbon nanofiber/tin disulfide composite electrode material is a very potential electrode material.
Claims (1)
1. A flexible hollow carbon nanofiber/tin disulfide composite electrode is characterized by being prepared by the following preparation method:
(1) taking a polymethyl methacrylate solution as an inner-layer spinning solution and a polyacrylonitrile solution as an outer-layer spinning solution;
(2) carrying out coaxial electrostatic spinning, curing and carbonization on the inner layer spinning solution and the outer layer spinning solution to obtain hollow carbon nanofibers;
(3) immersing the hollow carbon nanofiber into a hydrothermal reaction solution, carrying out ultrasonic treatment for 30-90min, and reacting for 3-9h at the temperature of 100-150 ℃ to obtain a precursor of the hollow carbon nanofiber/tin disulfide composite material; the hydrothermal reaction liquid is obtained by dissolving tin tetrachloride pentahydrate and thioacetamide in absolute ethyl alcohol and magnetically stirring for 30-40min, wherein the molar ratio of the tin tetrachloride pentahydrate to the thioacetamide is (1-3) to 5;
(4) and heating the precursor of the hollow carbon nanofiber/tin disulfide composite material to 200-400 ℃ at a speed of 1-4 ℃/min, calcining, and keeping the temperature for 60-180min to obtain the flexible hollow carbon nanofiber/tin disulfide composite electrode.
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| CN113823783A (en) * | 2021-08-25 | 2021-12-21 | 福建师范大学 | Preparation method and application of few-layer tin sulfide-sulfur-doped polyacrylonitrile compound potassium ion battery negative electrode material |
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