CN113809304B - Preparation method and application of plasma-based tin dioxide/carbon nanotube composite material - Google Patents
Preparation method and application of plasma-based tin dioxide/carbon nanotube composite material Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a tin dioxide/carbon nano tube composite material based on plasma, wherein micron-sized high-purity tin metal powder, a carbon nano tube and deionized water are uniformly mixed according to a certain proportion to be in a semi-fluid state and are pressed into a cylinder shape to be used as a cathode; the method comprises the following steps of adopting a refractory conductive material as a positive electrode, keeping a certain distance from the positive electrode, switching on a power supply to generate direct current arc plasma, realizing uniform loading of tin dioxide nanoparticles on the surface of a carbon nanotube while dispersing the carbon nanotube to obtain a tin dioxide/carbon nanotube composite material, and drying the tin dioxide/carbon nanotube composite material to be used as a negative electrode of a lithium ion battery; compared with a chemical method, the preparation method has the advantages of simplicity, rapidness, green and the like, and the carbon nano tube conductive network structure not only provides enough space for the volume expansion of tin dioxide, but also is beneficial to electron transfer; the method is expected to realize industrialization, and provides a new idea for preparation of other nano composite materials.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method and application of a plasma-based stannic oxide/carbon nano tube composite material.
Background
The information in this background section is disclosed only to enhance an understanding of the general background of the disclosure and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The lithium ion battery is an ideal energy storage device, and is widely applied to energy storage of electric vehicles, power grids and electronic devices due to the advantages of high energy density, long cycle life, low cost and the like. At present, as a commercial lithium ion battery cathode material, graphite cannot meet increasing energy storage requirements due to the defects of low theoretical specific capacitance, limited cycle rate and the like, so that the search for a new high-performance alternative cathode material becomes urgent.
Tin dioxide is widely applied to lithium battery electrode materials due to the fact that tin dioxide has high theoretical specific capacity (781 mAh/g). However, in the application process, the problems that the irreversible capacity is large for the first time, a large volume effect (volume expansion of 250-300%) exists during lithium intercalation, agglomeration is easy to occur in the circulation process and the like exist, so that the tin dioxide is often compounded with other materials to improve the dispersibility of tin dioxide particles, inhibit the agglomeration of the particles and improve the circulation stability of electrode materials. The carbon nano tube has the advantages of large specific surface area, good conductivity, strong chemical stability and the like, and becomes a carrier material widely applied at present.
However, in the prior art, a complicated chemical method is mostly adopted for preparing the carbon nanotube/tin dioxide composite material, and in the prior art, purified and modified carbon nanotubes and a tin tetrachloride solution are mixed and subjected to ultrasonic treatment, concentrated ammonia water is added dropwise into the obtained solution, the pH =9 is adjusted, the solution is stirred for 3 hours, then the solution is subjected to suction filtration, washing and drying, and the obtained filter residue is calcined for 1 hour at 600 ℃ to obtain the carbon nanotube/tin dioxide composite electrode. For a chemical preparation method, on one hand, the use of chemical reagents causes that impurities are easily introduced in the preparation process, adverse effects are generated on the performance, and environmental pollution is caused; on the other hand, the complexity of the preparation process is not beneficial to large-scale production, so that the development of a simple and clean tin dioxide/carbon nanotube preparation method is of great significance.
Disclosure of Invention
The invention aims to provide a preparation method and application of a tin dioxide/carbon nano tube composite material based on plasma, which solve the problems of complex process for preparing the tin dioxide/carbon nano tube composite material by a chemical method, difficulty in removing impurities caused by the use of various chemical reagents and the like in the background technology.
According to the preparation method of the tin dioxide/carbon nano tube composite material based on the plasma, on one hand, the contact area of the tin dioxide and the carbon nano tube can be increased on the basis of ensuring the dispersion uniformity of the carbon nano tube, and the combination of the tin dioxide and the carbon nano tube is promoted; on the other hand, the tin dioxide/carbon nano tube composite material coated with different tin dioxide contents can be obtained by adjusting the mass ratio of the carbon nano tube to the tin source, so that the requirements of the lithium battery electrode material on the performances such as electrochemistry and the like are met.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of a tin dioxide/carbon nano tube composite material based on plasma comprises the following steps:
s1: uniformly mixing tin metal powder, carbon nano tubes and deionized water to a semi-fluid state;
s2: pressing the semifluid mixture prepared by S1 into a cylindrical solid;
s3: taking the cylindrical solid material prepared in the step S2 as a negative electrode, taking a refractory conductive material as a positive electrode, and respectively and correspondingly connecting the negative electrode and the positive electrode with a power supply;
s4: switching on a power supply, generating direct current arc plasma between the cathode and the anode to form carbon nano tube dispersed mist, and simultaneously gasifying and oxidizing the tin metal powder to obtain tin dioxide nano particles which are uniformly loaded on the surface of the carbon nano tube to form a tin dioxide/carbon nano tube composite material;
s5: and (5) collecting the tin dioxide/carbon nano tube composite material prepared in the step (S4), and carrying out ultrasonic treatment, filtration and drying.
Preferably, the tin metal powder is micron-sized high-purity tin metal powder; the mass ratio of the micron-sized high-purity tin metal powder to the carbon nano tubes to the deionized water is (8).
Preferably, the refractory conductive material is one of iron, copper, aluminum, tungsten and graphite.
Preferably, the refractory conductive material is tungsten or graphite.
Preferably, in step S3, the distance between the two electrodes of the negative electrode and the positive electrode is 2-5mm, and the power supply parameters are as follows: the voltage is 8000-10000V, the power is 50W, and the frequency is 0.1-10 HZ.
Preferably, in the step S5, the ultrasonic time of the tin dioxide/carbon nanotube composite material is 0.5h, the drying temperature is 60-150 ℃, and the drying time is 1-2h.
An application of a plasma-based tin dioxide/carbon nanotube composite material, in particular to an application of the plasma-based tin dioxide/carbon nanotube composite material in a lithium battery cathode material.
The invention has the beneficial effects that:
1. compared with a chemical method, the preparation method of the tin dioxide/carbon nano tube composite material based on the plasma has the advantages of no use of any chemical reagent, simple preparation, rapidness, green and the like, and can realize uniform loading of tin dioxide nano particles on the surface of the carbon nano tube while the carbon nano tube is dispersed. The carbon nano tube conductive network structure not only can provide enough space for the volume expansion of the tin dioxide, but also is beneficial to realizing the electron transfer between the electrode and the tin dioxide in the lithium ion intercalation/deintercalation process. The method is expected to realize industrialization, and provides a new idea for preparation of other nano composite materials.
2. According to the invention, the cylindrical solid material is used as a negative electrode, a power supply is switched on, direct current arc plasma is generated between the negative electrode and a positive electrode, carbon nano tube dispersion mist is formed, and tin metal powder is gasified and oxidized; the carbon nano tube and the tin metal powder are mixed and pressed into a cylindrical solid material and simultaneously used as a negative electrode, the dispersion of the carbon nano tube and the gasification and oxidation of the tin metal powder have a synergistic effect, namely the formation of the dispersion mist of the carbon nano tube hinders the collision and aggregation among tin metal steam, and effectively inhibits the particle agglomeration caused by the collision among the tin steam, and the tin dioxide particles formed by adopting the preparation method disclosed by the invention are all in a nanometer level; simultaneously, the tin vapor and the carbon nano tube dispersion mist are better combined, and the dispersibility of the tin dioxide on the surface of the carbon nano tube is improved; the combination of the tin dioxide and the carbon nano tube is attributed to the condensation and oxidation of tin vapor on the surface of the carbon nano tube, and the tin dioxide still stably exists on the surface of the carbon nano tube after ultrasonic treatment, thereby showing good combination strength.
Drawings
FIG. 1 is a graphical representation of a tin dioxide/carbon nanotube composite material prepared in accordance with the present invention;
wherein: (a) Is SnO 2 Scanning Electron Micrographs (SEM) of/CNTs; (b) And (c) SnO at different magnifications 2 Transmission Electron Microscopy (TEM) of/CNTs; (d) Is SnO 2 High Resolution Transmission Electron Microscopy (HRTEM) of/CNTs;
FIG. 2 shows SnO prepared by the present invention 2 X-ray diffraction (XRD) patterns of/CNTs and commercially available tin dioxide;
FIG. 3 shows SnO prepared by the present invention 2 The specific surface area and the pore size distribution of the/CNTs composite material;
wherein: (e) Is SnO 2 Nitrogen adsorption/desorption isotherms of the/CNTs composite; (f) SnO obtained for Barrett-Joyner-Halenda process 2 The pore size distribution of the/CNTs composite material;
FIG. 4 shows SnO prepared by the invention 2 CNTs and commercially available SnO 2 100mAg as negative electrode material of lithium ion battery -1 Cycling stability at current density.
FIG. 5 shows SnO prepared by the invention 2 CNTs and commercially available SnO 2 The electrochemical impedance spectrum of the lithium ion battery cathode material in the frequency range of 0.01Hz-100 KHz;
Detailed Description
In order to clearly illustrate the technical features of the present solution, the following explains the present solution by way of specific embodiments and with reference to the accompanying drawings.
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
Examples
1. Preparation of stannic oxide/carbon nano tube composite material
A preparation method of a tin dioxide/carbon nano tube composite material based on plasma comprises the following steps:
s1: uniformly mixing micron-sized high-purity tin metal powder, a carbon nano tube and deionized water according to a mass ratio of 8;
s2: pressing the semifluid mixture prepared by S1 into a cylindrical solid;
s3: taking the cylindrical solid material prepared in the step S2 as a negative electrode, taking a metal tungsten wire conductive material as a positive electrode, and correspondingly connecting the negative electrode and the positive electrode with a power supply respectively; the distance between the two electrodes of the negative electrode and the positive electrode is 2-5mm; the power supply parameters are as follows: voltage 8000V, power 50W, frequency 5HZ;
s4: switching on a power supply, generating direct current arc plasma between the cathode and the anode to form carbon nano tube dispersed fog, and simultaneously gasifying and oxidizing the tin metal powder to obtain tin dioxide nano particles which are uniformly loaded on the surface of the carbon nano tube to form a tin dioxide/carbon nano tube composite material;
s5: and (4) collecting the tin dioxide/carbon nano tube composite material prepared in the step (S4), carrying out ultrasonic treatment for 0.5h, and drying for 2h at 100 ℃.
2. Application of plasma-based stannic oxide/carbon nanotube composite material
The invention discloses an application of a plasma-based tin dioxide/carbon nanotube composite material, which is applied to a lithium battery cathode material.
Electrochemical performance test
The electrochemical performance was performed under the following conditions: mixing the prepared stannic oxide/carbon nanotube composite material serving as a negative electrode active substance with conductive carbon black and polyvinylidene fluoride, wherein the weight ratio of the stannic oxide/carbon nanotube composite material to the conductive carbon black to the polyvinylidene fluoride is (8). Assembling 2032 button cell in glove box by using pure lithium sheet as counter electrode, wherein the diaphragm is polypropylene/polyethylene microporous film, and the electrolyte is LiPF of 1.15M 6 The battery is assembled and then subjected to charge and discharge tests on a blue test system, and the voltage window is 0.01V-3V. Electrochemical impedance spectroscopy testing was performed using an electrochemical workstation (CHI 660D) at a frequency range of 0.01Hz-100 KHz.
FIG. 1 shows a tin dioxide/carbon nanotube composite material (SnO) prepared by the present invention 2 CNTs), apparent carbon nanotube tubular structure can be seen from fig. 1, and SnO 2 The tin dioxide/carbon nano tube composite material based on the plasma has good dispersibility.
FIG. 2 shows SnO prepared by the present invention 2 CNTs and commercially available tin dioxide (SnO) 2 ) By comparing with the standard value card (JCPDS 41-1445), it can be seen that the main diffraction peak is SnO 2 The tetragonal rutile phase is well matched, which shows that the tin metal powder forms SnO under the action of direct current arc plasma 2 And (3) nanoparticles.
FIG. 3 shows SnO prepared by the present invention 2 The specific surface area and the pore size distribution of the/CNTs composite material show that SnO is shown 2 The specific surface area of the/CNTs composite material is 181.92m 2 g -1 Pore size distribution was analyzed by Barrett-Joyner-Halenda (BJH) method and the pore volume was 0.89mL g -1 The average pore diameter is 16.76nm, and the large specific surface area and pore volume are favorable for relieving strain generated in the electrochemical cycle process, relieving volume expansion of tin dioxide and improving cycle stability.
FIG. 4 shows SnO prepared by the present invention 2 CNTs and commercially available SnO 2 100mAg as negative electrode material of lithium ion battery -1 The cycling stability at current density, although commercially available SnO, can be seen from the figure 2 Shows a higher initial discharge capacity, but after 60 cycles the capacity drops rapidly to 200mAh g -1 Below, the cycling stability is poor, while the SnO prepared by the present application 2 the/CNTsshowed high cycling stability at 100mA g -1 The lower circulation still has 472mAh g after 200 circles -1 The capacity of (c).
FIG. 5 shows SnO prepared by the present invention 2 CNTs and commercially available SnO 2 As an Electrochemical Impedance Spectroscopy (EIS) of the lithium ion battery cathode material in the frequency range of 0.01Hz-100KHz, snO can be seen in the figure 2 The charge transfer resistance of the/CNTs is 119.8 omega, which is lower than that of the commercially available SnO 2 198.7 Ω, indicating that the introduction of the carbon nanotubes accelerates electron transport during the electrochemical reaction and has higher charge transfer efficiency. At the same time, at low frequencies, the slope of the line represents the ionic conductivity, snO, of the material 2 The impedance slope of the/CNTs is larger than that of the commercially available SnO 2 The slope of the impedance of (A), indicating SnO 2 /CNTs have excellent Li + The diffusion rate thus has better lithium storage characteristics and exhibits better electrochemical performance.
In summary, compared with a chemical method, the preparation method of the tin dioxide/carbon nanotube composite material based on the plasma has the advantages of simple preparation, rapidness, green and the like without using any chemical reagent, and uniform loading of the tin dioxide nanoparticles on the surface of the carbon nanotube is realized while the carbon nanotube is dispersed. The carbon nano tube conductive network structure not only can provide enough space for the volume expansion of the tin dioxide, but also is beneficial to realizing the electron transfer between the electrode and the tin dioxide in the lithium ion intercalation/deintercalation process; the invention prepares a high-performance tin dioxide/carbon nano tube composite material, and can be used as a good lithium battery cathode material.
The above embodiments are preferred embodiments of the present disclosure, but the present disclosure is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present disclosure should be construed as equivalents and are included in the scope of the present disclosure.
Claims (7)
1. A preparation method of a tin dioxide/carbon nano tube composite material based on plasma is characterized by comprising the following steps:
s1: uniformly mixing tin metal powder, carbon nano tubes and deionized water to a semi-fluid state; the tin metal powder is micron-sized high-purity tin metal powder; the mass ratio of the micron-sized high-purity tin metal powder to the carbon nano tube to the deionized water is 8;
s2: pressing the semifluid mixture prepared in the step S1 into a cylindrical solid;
s3: taking the cylindrical solid material prepared in the step S2 as a negative electrode, taking a refractory conductive material as a positive electrode, and respectively and correspondingly connecting the negative electrode and the positive electrode with a power supply;
s4: switching on a power supply, generating direct current arc plasma between the cathode and the anode to form carbon nano tube dispersed fog, gasifying and oxidizing tin metal powder to obtain tin dioxide nano particles, and uniformly loading the tin dioxide nano particles on the surface of the carbon nano tube to form a tin dioxide/carbon nano tube composite material;
s5: and (5) collecting the tin dioxide/carbon nano tube composite material prepared in the step (S4), and carrying out ultrasonic treatment, filtration and drying.
2. The method of claim 1, wherein the refractory conductive material is one of iron, copper, aluminum, tungsten, and graphite.
3. The method of claim 2, wherein the refractory conductive material is tungsten or graphite.
4. The method for preparing the tin dioxide/carbon nanotube composite material according to claim 1, wherein in the step S3, the distance between the two electrodes of the negative electrode and the positive electrode is 2 to 5mm, and the power supply parameters are as follows: the voltage is 8000 to 10000V, the power is 50W, and the frequency is 0.1HZ-10HZ.
5. The method of claim 1, wherein in step S5, the ultrasonic time of the tin dioxide/carbon nanotube composite is 0.5 h.
6. The method for preparing the tin dioxide/carbon nanotube composite material as claimed in claim 1, wherein in the step S5, the drying temperature of the tin dioxide/carbon nanotube composite material is 60 to 150 ℃ and the drying time is 1 to 2 hours.
7. The application of the plasma-based tin dioxide/carbon nanotube composite material is characterized in that the tin dioxide/carbon nanotube composite material is prepared by the preparation method according to any one of claims 1 to 6, and the plasma-based tin dioxide/carbon nanotube composite material is applied to a lithium battery cathode material.
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| CN102623669A (en) * | 2012-03-31 | 2012-08-01 | 大连理工大学 | Preparation method and application of carbon tin nanometer composite powder |
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| CN102623669A (en) * | 2012-03-31 | 2012-08-01 | 大连理工大学 | Preparation method and application of carbon tin nanometer composite powder |
| CN103482623A (en) * | 2013-09-05 | 2014-01-01 | 大连理工大学 | Method for preparing nano diamonds by using direct-current arc process |
| CN111203249A (en) * | 2019-09-18 | 2020-05-29 | 杭州电子科技大学 | Preparation method of graphene-coated transition metal carbide nanocapsules and application of nanocapsules in microwave catalysis field |
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