CN113903912A - Preparation method of carbon-loaded titanium carbide material, product obtained by preparation method and application of product - Google Patents
Preparation method of carbon-loaded titanium carbide material, product obtained by preparation method and application of product Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon-loaded titanium carbide material, which comprises the following steps: (a) adding glucose and sodium chloride into water, stirring and standing for more than thirty minutes, adding titanium fluoride, continuously stirring, drying, and calcining in a protective atmosphere to obtain a carbon-supported titanium carbide precursor; (b) and adding water into the carbon-supported titanium carbide precursor, carrying out suction filtration, drying, and calcining the dried powder under a protective atmosphere to obtain the carbon-supported titanium carbide material. The invention also discloses the carbon-loaded titanium carbide material prepared by the preparation method. The invention also discloses an application of the carbon-loaded titanium carbide material in a lithium ion battery cathode. The preparation method is simple and efficient; when the prepared carbon-loaded titanium carbide material is applied to a lithium ion battery cathode material, the prepared carbon-loaded titanium carbide material has excellent cycle stability and high rate capability, and the surface roughness of the material is 10Ag‑1Has 225mAhg after charging and discharging for 10000 times under high current density‑1The specific capacity of (A).
Description
Technical Field
The invention relates to a preparation method of a composite material, an obtained product and application thereof, in particular to a preparation method of a carbon-loaded titanium carbide material, and the obtained product and application thereof.
Background
In recent thirty years, the development of electronic devices including smart phones, notebook computers and electric vehicles has greatly promoted the rapid development of batteries. Various rechargeable batteries such as lithium ion batteries, sodium ion batteries, lithium sulfur batteries and sodium sulfur batteries are emerging, wherein the lithium ion batteries are the most widely commercialized and applied batteries due to their long cycle life, high energy density and portable characteristics. In recent years, carbon-based materials have been rapidly developed. Researchers have demonstrated that the mixing of graphite with Carbon Nanotubes (CNTs) can reduce the charge transfer resistance of the negative electrode by nearly 2 times compared to commercial graphite, thereby enhancing the effect of rapid charging in lithium ion batteries. Simulation studies have shown that the diffusion barrier for lithium ions is related to the degree of lithiation of graphite, and that the higher the degree of lithiation of graphite, the larger the diffusion barrier for lithium ions, resulting in an increase in overpotential.
At present, transition metal carbide is concerned about chemical energy storage in point due to its advantages of high melting point, high hardness, good chemical stability, good conductivity and the like. In addition, WC, TiC, TaC, etc. have sp electronic properties and catalytic performance similar to those of noble metals, so that substitution of Pt, Au and Pd with transition metal carbides can significantly reduce the cost of the catalyst. TiC, as a transition metal compound, has good conductivity (1.5X 10)4Scm-1) And the density is low, and the like, so that when the modified lithium ion battery cathode material is used for modifying the lithium ion battery cathode material, the electron mobility of the material can be improved. The volume change during lithium intercalation/deintercalation is suppressed. There are research groups which use carbon dioxide in the air as a carbon source to prepare TiC @ C-TiO by a method of TiC oxidation in the air2The core-shell composite negative electrode has a structural design limitation, and the content of carbon source carbon dioxide is difficult to control, so that the content of the carbon source carbon dioxide is 1Ag-1Has a current density of only 254mAhg-1Specific discharge capacity of (2).
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention aims to provide a simple and efficient preparation method of the carbon-supported titanium carbide material, and the invention also aims to provide the carbon-supported titanium carbide material with good conductivity, high multiplying power and long cycle life.
The technical scheme is as follows: the preparation method of the carbon-supported titanium carbide material comprises the following steps:
(a) adding glucose and sodium chloride into water, stirring and standing for more than thirty minutes to uniformly mix the materials, adding titanium fluoride, continuously stirring, drying, and calcining in a protective atmosphere to obtain a carbon-supported titanium carbide precursor;
(b) and adding water into the carbon-supported titanium carbide precursor, carrying out suction filtration, drying, and calcining the dried powder under a protective atmosphere to obtain the carbon-supported titanium carbide material.
Further, in the step (a), the drying temperature is 60-100 ℃, and the drying time is 15-25 h. The calcination temperature is 600-800 ℃, the heating rate is 4-5 ℃/min, and the heat preservation time is 2-4 hours. The calcination temperature is lower than 600 ℃, and the oxidation is incomplete; calcination temperatures above 800 ℃ can destroy the structure. The temperature rise rate is lower than 4 ℃/min, and the reaction is incomplete; the temperature rise rate is higher than 5 ℃/min, and the risk of frying the furnace exists. The mass ratio of glucose, sodium chloride and water is 2: 15: 10.
further, in the step (b), the number of times of suction filtration is 5-10. The calcination temperature is 1000-1200 ℃, the heating rate is 4-5 ℃/min, and the heat preservation time is 1-3 hours. The calcination temperature is lower than 1000 ℃, and carbonization is difficult to realize; calcination temperatures above 1200 ℃ can destroy the TiC structure. The temperature rise rate is lower than 4 ℃/min, and the reaction is incomplete; the temperature rise rate is higher than 5 ℃/min, and the risk of frying the furnace exists.
Further, the protective atmosphere is nitrogen, and occurrence of side reactions can be prevented.
The carbon-supported titanium carbide material prepared by the preparation method of the carbon-supported titanium carbide material has a layered structure of carbon and titanium carbide on the surface of the carbon.
Further, carbon is a porous carbon material having a three-dimensional layered structure. The titanium carbide has an average particle diameter of 5 to 20nm and excellent conductivity (1.5X 10)4Scm-1) And strength (hardness 9 to 10).
The carbon-loaded titanium carbide material is applied to the negative electrode of the lithium ion battery.
The preparation principle is as follows: glucose is used as a carbon source, and sodium chloride is dissolved in the suction filtration process to create a layered structure, and the two materials are low-cost, non-toxic and harmless materials, so that the method has a wide application prospect. Titanium carbide particles are loaded on the surface of layered carbon to form a hybrid functional material, the layered structure of the carbon material can provide space for shuttling lithium ions, the titanium carbide particles can provide more active sites, and the electronic conductivity of the material is improved. Moreover, because the titanium carbide has good strength and stability, the volume change of the electrode material in the process of intercalation and deintercalation of lithium ions is effectively inhibited when the titanium carbide is loaded on the surface of the layered carbon.
Has the advantages that: compared with the prior art, the invention has the following remarkable characteristics:
1. the preparation method is simple and efficient, the three-dimensional layered structure of the carbon material can be well created by the suction filtration method, and the titanium carbide nano-particles can be simply prepared by high-temperature sintering and firmly loaded on the surface of the three-dimensional layered carbon material;
2. when the prepared carbon-loaded titanium carbide material is applied to a lithium ion battery cathode material, the prepared carbon-loaded titanium carbide material has excellent cycle stability and high rate capability, and the surface roughness of the material is 10Ag-1Has 225mAhg after charging and discharging for 10000 times under high current density-1The excellent cycle performance of the material is far higher than that of the lithium ion battery cathode material on the market, the material has higher capacity and longer service life, and the lithium ion battery can have more excellent performance, so that the carbon material can be widely applied to the field of the lithium ion battery.
3. Glucose is used as a carbon source, and sodium chloride is dissolved in the suction filtration process to create a layered structure, and the two are both low-cost, non-toxic and harmless materials, so that the environment protection is facilitated.
Drawings
FIG. 1 is an X-ray diffraction pattern of the product obtained in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a product obtained in example 1 of the present invention, wherein a is 2500 times magnification and b is 5 ten thousand times magnification;
FIG. 3 is a transmission electron micrograph of products obtained in example 1, comparative example 2 and comparative example 3 of the present invention, wherein a is a magnification of 30 ten thousand and b is a magnification of 1200 ten thousand;
FIG. 4 is a graph showing rate performance of products obtained in example 1, comparative example 2 and comparative example 3 of the present invention on half-cells of lithium sheets;
FIG. 5 is a graph showing the cycle performance of the products obtained in example 1, comparative example 2 and comparative example 3 of the present invention in half-cells made of lithium sheets.
Detailed Description
Example 1
A preparation method of a carbon-supported titanium carbide material comprises the following steps:
(1) adding 2g of glucose and 15g of sodium chloride into 10ml of water, stirring and standing for 30 minutes, adding 0.2g of titanium fluoride, continuously and uniformly stirring, drying at 80 ℃ for 24 hours, calcining the dried powder at 750 ℃ in a nitrogen atmosphere, wherein the heating rate is 5 ℃/min, and the heat preservation time is 2 hours, so as to obtain a carbon-supported titanium carbide precursor;
(2) adding water into the carbon-loaded titanium carbide precursor, carrying out suction filtration for 7 times, drying at 80 ℃, calcining the dried powder at 1100 ℃ in a nitrogen atmosphere, wherein the heating rate is 5 ℃/min, and the heat preservation time is 2 hours, so as to obtain the carbon-loaded titanium carbide material.
FIG. 1 is an X-ray diffraction pattern of the product obtained in example 1. As can be seen from FIG. 1, the diffraction peaks of the prepared nanoparticles are completely consistent with the standard spectrum (PDF #32-1383) of titanium carbide, indicating that the prepared product is phase-pure titanium carbide.
As can be seen from the sem images of fig. 2a and 2b, the titanium carbide-carbon bulk is a three-dimensional lamellar structure.
The transmission electron microscope images in fig. 3a and 3b clearly show the structure of titanium carbide particles supported on the carbon layer, the average particle size of titanium carbide is 10nm, the lattice fringes can be clearly seen, the titanium carbide has good crystallinity, the measured lattice spacing is 0.25nm, and the measured lattice spacing corresponds to the (111) crystal plane.
The prepared carbon-loaded titanium carbide material is applied to a lithium ion battery cathode material, and is mixed with conductive carbon black and a binder (PVDF) according to the weight ratio of 7: 2: 1 weight ratio, and then performing electrochemical performance test on the half cell on the lithium sheet. FIG. 4 is a graph of rate performance for titanium carbide-carbon anodes at 0.1, 0.2, 0.5, 1, 2, 5, 10, 20Ag-1Has a specific discharge capacity of 432, 364, 318, 284, 248, 191, 144 and 99mAhg, respectively-1. When the current density returns to 0.1Ag again-1The specific discharge capacity can reach 387mAhg-1Good reversibility is shown.
Further, the cycle performance of the titanium carbide-carbon negative electrode is 10Ag as shown in FIG. 5-1Has excellent cycling stability under high current density and still has 225mAhg after 10000 cycles-1The specific discharge capacity and the capacity retention rate of (2) were 95.3%. Therefore, the TiC-C anode material obtained in the embodiment has excellent rate performance, long service life and good cycling stability.
Example 2
A preparation method of a carbon-supported titanium carbide material comprises the following steps:
(1) adding 2g of glucose and 15g of sodium chloride into 10ml of water, stirring and standing for 50 minutes, adding 0.2g of titanium fluoride, continuously and uniformly stirring, drying at 60 ℃ for 15 hours, calcining the dried powder at 600 ℃ in a nitrogen atmosphere, wherein the heating rate is 4 ℃/min, and the heat preservation time is 4 hours, so as to obtain a carbon-supported titanium carbide precursor;
(2) adding water into the carbon-loaded titanium carbide precursor, carrying out suction filtration for 5 times, drying at 80 ℃, calcining the dried powder at 1000 ℃ in a nitrogen atmosphere, wherein the heating rate is 4 ℃/min, and the heat preservation time is 1 hour, thus obtaining the carbon-loaded titanium carbide material.
In the obtained carbon-supported titanium carbide material, carbon is a porous carbon material with a three-dimensional layered structure, and titanium carbide with the average particle size of 5nm is arranged on the surface of the carbon.
Example 3
A preparation method of a carbon-supported titanium carbide material comprises the following steps:
(1) adding 2g of glucose and 15g of sodium chloride into 10ml of water, stirring and standing for 60 minutes, adding 0.2g of titanium fluoride, continuously and uniformly stirring, drying at 100 ℃ for 25 hours, calcining the dried powder at 800 ℃ in a nitrogen atmosphere, wherein the heating rate is 4.5 ℃/min, and the heat preservation time is 2-4 hours, so as to obtain a carbon-supported titanium carbide precursor;
(2) adding water into the carbon-loaded titanium carbide precursor, carrying out suction filtration for 10 times, drying at 80 ℃, calcining the dried powder at 1200 ℃ in a nitrogen atmosphere, wherein the heating rate is 4.5 ℃/min, and the heat preservation time is 3 hours, so as to obtain the carbon-loaded titanium carbide material.
In the obtained carbon-supported titanium carbide material, carbon is a porous carbon material with a three-dimensional layered structure, and titanium carbide with the average particle size of 20nm is arranged on the surface of the carbon.
Example 4
A preparation method of a carbon-supported titanium carbide material comprises the following steps:
(1) adding 2g of glucose and 15g of sodium chloride into 10ml of water, stirring and standing for 120 minutes, adding 0.2g of titanium fluoride, continuously and uniformly stirring, drying at 70 ℃ for 20 hours, calcining the dried powder at 700 ℃ in a nitrogen atmosphere, and keeping the temperature for 2.5 hours at the heating rate of 4 ℃/min to obtain a carbon-supported titanium carbide precursor;
(2) adding water into the carbon-supported titanium carbide precursor, carrying out suction filtration for 8 times, drying at 80 ℃, calcining the dried powder at 1050 ℃ in a nitrogen atmosphere, wherein the heating rate is 4 ℃/min, and the heat preservation time is 1.5 hours, thus obtaining the carbon-supported titanium carbide material.
In the obtained carbon-supported titanium carbide material, carbon is a porous carbon material with a three-dimensional layered structure, and titanium carbide with the average particle size of 15nm is arranged on the surface of the carbon.
Example 5
A preparation method of a carbon-supported titanium carbide material comprises the following steps:
(1) adding 2g of glucose and 15g of sodium chloride into 10ml of water, stirring and standing for 100 minutes, adding 0.2g of titanium fluoride, continuously and uniformly stirring, drying at 90 ℃ for 18 hours, calcining the dried powder at 650 ℃ in a nitrogen atmosphere, wherein the heating rate is 5 ℃/min, and the heat preservation time is 3.5 hours, so as to obtain a carbon-supported titanium carbide precursor;
(2) adding water into the carbon-supported titanium carbide precursor, carrying out suction filtration for 6 times, drying at 80 ℃, calcining the dried powder at 1150 ℃ in a nitrogen atmosphere, wherein the heating rate is 5 ℃/min, and the heat preservation time is 2.5 hours, so as to obtain the carbon-supported titanium carbide material.
In the obtained carbon-supported titanium carbide material, carbon is a porous carbon material with a three-dimensional layered structure, and titanium carbide with the average particle size of 8nm is arranged on the surface of the carbon.
Comparative example 1
This comparative example is identical to the rest of the preparation of example 1, except that: and (3) using acetic acid to replace glucose as a carbon source, using the obtained product as a lithium ion battery cathode material, and testing the rate capability and the cycle performance. As can be seen from FIGS. 4 and 5, the rate capability and cycle capability of the comparative example are inferior to those of example 1, at 10Ag-1Can only circulate 4000 circles under the current density of (1), and the specific capacity is also only 170mAhg-1。
Comparative example 2
This comparative example is identical to the rest of the preparation of example 1, except that: and (3) replacing sodium chloride with potassium chloride, and testing the rate capability and the cycle performance by using the obtained product as a lithium ion battery cathode material. As can be seen from FIGS. 4 and 5, the rate capability and cycle capability of the comparative example are inferior to those of example 1, at 10Ag-1Can only circulate 4300 circles under the current density of (1), and has the specific capacity of 230mAhg-1。
Comparative example 3
This comparative example is identical to the rest of the preparation of example 1, except that: and (3) using acetic acid to replace glucose as a carbon source, using potassium chloride to replace sodium chloride, using the obtained product as a lithium ion battery cathode material, and testing the rate capability and the cycle performance. As can be seen from FIGS. 4 and 5, the rate capability and cycle capability of the comparative example are inferior to those of examples 1, 1 and 2, at 10Ag-1Can only cycle 2200 circles under the current density of (1), and the specific capacity is also only 110mAhg-1。
Comparative example 4
Respectively with phenolic resin, Pluronic F127 andthe citric acid titanium complex is used as a carbon source, a template agent and a titanium source, and the TiO is synthesized by a general method2@ C and TiO2the/TiC @ C mesoporous composite membrane. 1.5g of F127, 2.5g of phenolic resin and 3.0g of titanium citrate solution were dissolved in 16ml of a water/ethanol mixture (1: 1). After stirring at room temperature for 30min, the solution was coated on a silicon wafer at a speed of 600rpm for 10s to form a thin film. Drying the film at 40 ℃ for 3-5 h, aging at 100 ℃ for 24h, and pyrolyzing at 700 ℃ and 900 ℃ respectively in nitrogen for 2h to obtain mesoporous TiO2@ C and TiO2a/TiC @ C composite film. The obtained product is used as the lithium ion battery cathode material to carry out the test of the cycle performance at 1.5Ag-1Current density of 200mAhg only after 5000 cycles-1And there is a significant capacity fade after cycle 2000. The three-dimensional porous layered structure of the cathode material prepared by the method can effectively inhibit the volume change in the lithium ion intercalation and deintercalation process, and effectively improves the cycle stability of the electrode material.
Comparative example 5
TiC @ C-TiO is prepared by adopting TiC oxidation method in air2Core-shell nanoparticles. Specifically, 0.2g of TiC was used as a precursor, and oxidized at 350 ℃ for 60min in a tube furnace in an air atmosphere. The obtained product is used as the lithium ion battery cathode material to carry out the rate capability test at 0.1, 0.2, 0.5, 1, 2, 3, 5 and 10Ag-1Has a current density of 352, 310, 274, 253, 227, 213, 191 and 158mAhg, respectively-1Specific discharge capacity of (2). The titanium carbide nanoparticles are loaded on the three-dimensional porous layered carbon material, so that the conductivity of the material can be effectively improved, and the rate performance of the material can be improved.
In summary, it can be seen in combination with the data of comparative example 1, comparative example 2, comparative example 3, comparative example 4, comparative example 5 and example 1 that: under the specific proportion and method of the application, when sodium chloride and glucose are used as raw materials, the prepared carbon-supported titanium carbide material has excellent cycle stability and high rate performance when applied to a lithium ion battery cathode material.
Claims (10)
1. The preparation method of the carbon-supported titanium carbide material is characterized by comprising the following steps of:
(a) adding glucose and sodium chloride into water, stirring and standing for more than thirty minutes, adding titanium fluoride, continuously stirring, drying, and calcining in a protective atmosphere to obtain a carbon-supported titanium carbide precursor;
(b) and adding water into the carbon-supported titanium carbide precursor, carrying out suction filtration, drying, and calcining the dried powder under a protective atmosphere to obtain the carbon-supported titanium carbide material.
2. The method for preparing a carbon-supported titanium carbide material according to claim 1, wherein: in the step (a), the drying temperature is 60-100 ℃, and the drying time is 15-25 h.
3. The method for preparing a carbon-supported titanium carbide material according to claim 1, wherein: in the step (a), the calcining temperature is 600-800 ℃, the heating rate is 4-5 ℃/min, and the heat preservation time is 2-4 hours.
4. The method for preparing a carbon-supported titanium carbide material according to claim 1, wherein: in the step (b), the number of times of suction filtration is 5-10.
5. The method for preparing a carbon-supported titanium carbide material according to claim 1, wherein: in the step (b), the calcining temperature is 1000-1200 ℃, the heating rate is 4-5 ℃/min, and the heat preservation time is 1-3 hours.
6. The method for preparing a carbon-supported titanium carbide material according to claim 1, wherein: the protective atmosphere is nitrogen.
7. The carbon-supported titanium carbide material obtained by the method for producing a carbon-supported titanium carbide material according to any one of claims 1 to 6, characterized in that: the carbon is of a layered structure, and titanium carbide is arranged on the surface of the carbon.
8. The carbon-supported titanium carbide material according to claim 7, wherein: the carbon is a porous carbon material having a three-dimensional layered structure.
9. The carbon-supported titanium carbide material according to claim 7, wherein: the average particle size of the titanium carbide is 5-20 nm.
10. The use of the carbon-supported titanium carbide material according to claim 7 in a negative electrode of a lithium ion battery.
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