CN109119636B - Titanium vanadium nitrogen nanofiber current collector and preparation method thereof - Google Patents
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Abstract
The invention discloses a titanium vanadium nitrogen nanofiber current collector and a preparation method and application thereof. The titanium vanadium nitrogen nanofiber current collector is prepared by the following steps: s1, preparing a precursor solution; s2, spinning the precursor solution in the step S1 by using an electrostatic spinning device to obtain precursor nano fibers; s3, nitriding the precursor nanofiber at the temperature of 600-800 ℃ to obtain the titanium-vanadium-nitrogen nanofiber current collector. The titanium vanadium nitrogen nanofiber current collector disclosed by the invention combines the characteristics of titanium nitride, vanadium nitride and a self-supporting nano structure, and does not contain nonpolar carbon; the advantages of titanium nitride, vanadium nitride, non-polar carbon and a self-supporting nano structure are cooperatively exerted, compared with the single use of titanium nitride or vanadium nitride, the lithium-sulfur battery electrode has better conductivity and lower shuttle effect, has more outstanding improvement effect on the performance of the lithium-sulfur battery, and has great significance for improving the performance of the lithium-sulfur battery.
Description
Technical Field
The invention belongs to the technical field of preparation of current collectors of electric storage materials, and particularly relates to a titanium-vanadium-nitrogen nanofiber current collector and a preparation method thereof.
Background
With the continuous consumption of non-renewable petroleum fuels and the strong demand of new generations of human beings for advanced energy, people are continuously prompted to explore new rechargeable energy storage equipment. Lithium sulfur batteries are considered to be an excellent next generation energy source choice due to low cost, abundant reserves, environmental friendliness and their high theoretical capacity. However, the performance of the catalyst is affected by the low conductivity of sulfur and the shuttling effect of polysulfide, and thus the catalyst is difficult to satisfy the actual wide application. Therefore, a material is sought, the conductivity of the material is improved, the polysulfide shuttling effect of the material is inhibited, and the material has great significance for improving the performance of the lithium-sulfur battery.
Carbon-based materials are of high interest because of their electrical conductivity, but nonpolar carbon is not conducive to adsorptive conversion of polar lithium polysulfides. Research shows that the metal nitride has excellent performance, such as high conductivity and improved sulfur utilization rate; chemical resistance ensures electrode integrity during battery cycling, etc. Wherein, vanadium nitride has catalytic performance similar to noble metal, promotes redox kinetics and has high adsorbability to lithium polysulfide, and inhibits shuttle effect of the lithium polysulfide; titanium nitride is higher than vanadium nitride conductivity, can further promote electric conductivity, and titanium nitride can provide more adsorption sites in addition to this reinforcing vanadium nitride is to the excellent of lithium polysulfide high adsorptivity, and promotes vanadium nitride further to exert its catalytic action.
Titanium nitride or vanadium nitride has certain improvement effect on the conductivity or shuttle effect of the lithium-sulfur battery positive electrode, but still has a larger improvement space, and the improvement space is to further improve the conductivity of the lithium-sulfur battery electrode and reduce the shuttle effect.
Disclosure of Invention
The invention aims to provide a titanium vanadium nitrogen nanofiber current collector. The invention combines the characteristics of titanium nitride, vanadium nitride and self-supporting nano structures to prepare the titanium vanadium nitrogen nanofiber current collector, and the titanium vanadium nitrogen nanofiber current collector does not contain nonpolar carbon. Meanwhile, titanium nitride and vanadium nitride are adopted to prepare the titanium-vanadium-nitrogen nanofiber current collector, and the titanium-vanadium-nitrogen nanofiber current collector and the vanadium nitride have a synergistic effect, so that compared with the case of singly using the titanium nitride or the vanadium nitride, the lithium-sulfur battery electrode has the advantages of better conductivity, lower shuttle effect and more prominent improvement effect on the performance of the lithium-sulfur battery.
Another object of the present invention is to provide the application of the titanium vanadium nitrogen nanofiber current collector.
The above object of the present invention is achieved by the following scheme:
a titanium vanadium nitrogen nanofiber current collector is prepared by the following steps:
s1, preparing a precursor solution: the solute in the solution comprises a titanium-containing compound, a vanadium-containing compound and polyvinylpyrrolidone; the solvent is organic alcohol;
s2, spinning the precursor solution obtained in the step S1 by using an electrostatic spinning device to obtain precursor nano fibers;
s3, nitriding the precursor nanofiber at the temperature of 600-800 ℃ to obtain the titanium vanadium nitrogen nanofiber current collector;
wherein the molar ratio of the titanium element to the vanadium element in the precursor solution is 1-5: 1.
The molar ratio of the titanium element to the vanadium element in the titanium-vanadium-nitrogen nanofiber current collector is 1-5: 1. The vanadium nitride has catalytic performance similar to that of noble metal, promotes redox kinetics and high adsorbability to lithium polysulfide, and inhibits shuttle effect of the lithium polysulfide; compared with vanadium nitride, titanium nitride has higher conductivity, can further improve the conductivity, and can provide more adsorption sites, thereby enhancing the superiority of vanadium nitride in high adsorption of lithium polysulfide and promoting vanadium nitride to further exert the catalytic action of vanadium nitride; according to the invention, titanium nitride and vanadium nitride are combined to prepare the titanium-vanadium-nitrogen nanofiber current collector, the advantages of the titanium nitride and the vanadium nitride are utilized, and the titanium nitride and the vanadium nitride play a synergistic role, so that compared with the single use of the titanium nitride or the vanadium nitride, the lithium-sulfur battery electrode has better conductivity and lower shuttle effect, and has a more prominent improvement effect on the performance of the lithium-sulfur battery.
When the content of titanium nitride is too small, the conductivity of the current collector is too poor, and when the content of titanium nitride is too large, the performance of vanadium nitride catalysis and other performances is inhibited, so that the synergistic effect of the titanium nitride and the vanadium nitride is not good.
Since the nonpolar carbon is not beneficial to the adsorption and conversion of the polar lithium polysulfide, the invention adopts the electrostatic spinning technology and combines the high-temperature nitriding treatment technology to remove the nonpolar carbon in the fiber spinning, thereby reducing the adverse effect caused by that the nonpolar carbon can only weakly physically adsorb the lithium polysulfide; and the obtained nano-fiber has a self-supporting structure, so that when the nano-fiber is used for preparing a lithium-sulfur battery, the use of a binder and an additive is avoided, and the transportation of ions and electrons in an electrolyte is facilitated. The titanium vanadium nitrogen nanofiber current collector synergistically exerts the advantages of titanium nitride, vanadium nitride, non-polar carbon and a self-supporting nano structure, and has great significance in improving the performance of the lithium-sulfur battery.
Preferably, the molar ratio of the titanium element to the vanadium element in the precursor solution is 4: 1.
preferably, the nitriding temperature in step S3 is 800 ℃ and the nitriding time is 2h to 8 h.
Preferably, the titanium-containing compound is Ti (OC)2H5)4，TiO2，Ti4O7，TiCl3，TiCl4Or TiH4(ii) a The vanadium-containing compound is VO (OC)2H5)3，V(OC2H5)3，NH4VO3，Na3VO4，VCl2Or V2O5。
Preferably, the titanium-containing compound is Ti (OC)2H5)4(i.e., tetrabutyl titanate); the vanadium-containing compound is V (OC)2H5)3(i.e., vanadium acetylacetonate).
Preferably, the mass volume concentration of the polyvinylpyrrolidone and the solvent in the precursor solution is 0.083-0.167 g/mL.
Preferably, the mass volume concentration of the polyvinylpyrrolidone and the solvent in the precursor solution is 0.15 g/mL.
Preferably, the conditions of the electrospinning apparatus are: the voltage is 15-25 kV, the receiving distance is 15-20 cm, and the propelling speed is 0.01-0.05 mL/min.
The application of the titanium vanadium nitrogen nanofiber current collector in the preparation of the lithium-sulfur battery electrode is also within the protection scope of the invention.
Compared with the prior art, the invention has the following beneficial effects:
the invention combines the characteristics of titanium nitride, vanadium nitride and self-supporting nano structure to prepare the titanium vanadium nitrogen nanofiber current collector, and does not contain nonpolar carbon; the titanium vanadium nitrogen nanofiber current collector is processed by adopting an electrostatic spinning technology and a high-temperature nitriding technology, so that nonpolar carbon does not exist in the titanium vanadium nitrogen nanofiber current collector and the titanium vanadium nitrogen nanofiber current collector has a self-supporting structural characteristic. The titanium vanadium nitrogen nanofiber current collector synergistically exerts the advantages of titanium nitride, vanadium nitride, non-polar carbon and a self-supporting nano structure, and compared with the independent use of the titanium nitride or the vanadium nitride, the lithium sulfur battery electrode has the advantages of better conductivity and lower shuttle effect, has a more prominent improvement effect on the performance of the lithium sulfur battery, and has great significance in improving the performance of the lithium sulfur battery.
Drawings
Fig. 1 is a graph comparing the constant current charge and discharge performance of the lithium sulfur battery using the ti-v-n nanofiber current collector and the conventional aluminum foil current collector in example 1.
Fig. 2 is a graph comparing the rate performance of a lithium sulfur battery using a titanium vanadium nitrogen nanofiber current collector and a conventional aluminum foil current collector in example 1.
Fig. 3 is a graph comparing the conductivity performance of the lithium sulfur battery using the titanium vanadium nitrogen nanofiber current collector and the conventional aluminum foil current collector in example 1.
Fig. 4 is a graph comparing the rate performance of a lithium sulfur battery using a ti-v-n nanofiber current collector and a simple ti-nitride current collector, a simple v-nitride current collector in example 1.
Detailed Description
The present invention is further described in detail below with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention. The test methods used in the following examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are, unless otherwise specified, commercially available reagents and materials.
Example 1
A titanium vanadium nitrogen nanofiber current collector is prepared by the following steps:
(1) preparing a precursor solution: solute in the precursor solution is 3mL of tetrabutyl titanate, 0.75g of vanadium acetylacetonate and 1.8g of polyvinylpyrrolidone, and the solvent is 12mL of absolute ethyl alcohol;
(2) preparing the precursor solution in the step (1) into nano fibers by using a uniaxial spinning technology, wherein the voltage is 17.5kV, the acceptance distance is 20cm, and the propelling speed is 0.03 mL/min;
(3) calcining and nitriding the nano-fibers in the step (2) at 800 ℃ to obtain a self-supporting carbon-free titanium vanadium nitrogen nano-fiber current collector.
Example 2
The preparation process of the titanium vanadium nitrogen nanofiber current collector is the same as that in example 1, except that the amount of vanadium acetylacetonate in the step (1) is 0.6 g.
Example 3
The preparation process of the titanium vanadium nitrogen nanofiber current collector is the same as that in example 1, except that the amount of vanadium acetylacetonate in the step (1) is 1.0 g.
Example 4
The preparation process of the titanium vanadium nitrogen nanofiber current collector is the same as that in example 1, except that the amount of vanadium acetylacetonate in the step (1) is 0.5 g.
Example 5
The preparation process of the titanium vanadium nitrogen nanofiber current collector is the same as that in example 1, except that the amount of vanadium acetylacetonate in the step (1) is 1.5 g.
Example 6
The preparation process of the titanium vanadium nitrogen nanofiber current collector is the same as that in example 1, except that the amount of vanadium acetylacetonate in the step (1) is 3.0 g.
Comparative example 1
A conventional general aluminum foil current collector was used as comparative example 1.
Comparative example 2
The preparation process of the titanium-doped nitrogen nanofiber current collector is the same as that in example 1, except that only tetrabutyl titanate is added into the precursor solution in the step (1), and vanadium acetylacetonate is not added.
Comparative example 3
The preparation process of the titanium-doped nitrogen nanofiber current collector is the same as that in example 1, except that only vanadium acetylacetonate is added to the precursor solution in the step (1), and tetrabutyl titanate is not added.
Application examples
The current collectors obtained in example 1 and comparative examples 1 to 3 were applied to lithium sulfur batteries for performance testing.
All current collectors were cut into disks 12mm in diameter and the test cell model was 2016 type coin cell. The test results are shown in FIGS. 1 to 3.
Fig. 1 is a graph comparing the long cycle performance of a lithium sulfur battery using a titanium vanadium nitrogen nanofiber current collector in example 1 and a lithium sulfur battery using a conventional aluminum foil current collector in comparative example 1. As shown in the figure, the lithium-sulfur battery using the titanium-vanadium-nitrogen nanofiber current collector is more excellent in long cycle performance, and the charge and discharge capacity under the 0.2C condition is much higher than that of the lithium-sulfur battery using the conventional aluminum foil current collector.
Fig. 2 is a graph comparing the rate performance of a lithium sulfur battery using a titanium vanadium nitrogen nanofiber current collector in example 1 and a lithium sulfur battery using a conventional aluminum foil current collector in comparative example 1. As shown, the lithium sulfur battery using the titanium vanadium nitrogen nanofiber current collector also performed more excellent in rate ring performance, from 0.1A g-1To 1.5A g-1And back to 0.1A g-1The charge and discharge capacity is much higher than that of the lithium-sulfur battery using the traditional aluminum foil current collector.
Fig. 3 is a graph comparing the conductivity performance of the lithium sulfur battery using the titanium vanadium nitrogen nanofiber current collector of example 1 and the lithium sulfur battery using the conventional aluminum foil current collector of comparative example 1. As shown in the figure, it is obvious that the conductivity is better when the titanium vanadium nitrogen nanofiber current collector is used.
Fig. 4 is a graph comparing rate performance of lithium sulfur batteries using the titanium vanadium nitrogen nanofiber current collector of example 1 and the current collectors prepared in comparative example 2 and comparative example 3. As shown in the figure, titanium nitride has better conductivity, better multiplying power and higher charge-discharge capacity compared with vanadium nitride. Compared with the titanium nitride, the titanium vanadium nitride has higher charge-discharge capacity and better stability than the vanadium nitride. According to the effect obtained by detection, in the titanium vanadium nitrogen nanofiber current collector prepared by the invention, the titanium nitride and the vanadium nitride play a synergistic role.
In addition, the inventor also examines the influence of the ratio of titanium nitride to vanadium nitride in the titanium vanadium nitrogen nanofiber current collector on the current collector performance. Through multiple tests, the titanium nitride and the vanadium nitride in the titanium-vanadium-nitrogen nanofiber current collector have a good synergistic effect when the molar ratio of the titanium nitride to the vanadium nitride is within the range of 1-5: 1, and when the ratio of the titanium nitride to the vanadium nitride is 4:1, the synergistic effect of the titanium nitride to the vanadium nitride is optimal, and the performance of the prepared current collector is optimal. When the content of titanium nitride is too low, the conductivity of the current collector is too poor, and when the content of titanium nitride is too high, the performance of vanadium nitride catalysis and other performances can be inhibited, so that the synergistic effect of the titanium nitride and the vanadium nitride is not good, and the performance of the prepared current collector is poor.
It should be finally noted that the above examples are only intended to illustrate the technical solutions of the present invention, and not to limit the scope of the present invention, and that other variations and modifications based on the above description and thought may be made by those skilled in the art, and that all embodiments need not be exhaustive. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (2)
1. The titanium vanadium nitrogen nanofiber current collector is characterized by being prepared by the following steps:
s1, preparing a precursor solution: the solute in the solution comprises Ti (OC)2H 5)4，V(OC 2H 5)3And polyvinylpyrrolidone; the solvent is organic alcohol;
s2, spinning the precursor solution in the step S1 by using an electrostatic spinning device to obtain precursor nano fibers; the conditions of the electrospinning apparatus were: the voltage is 15-25 kV, the receiving distance is 15-20 cm, and the propelling speed is 0.01-0.05 mL/min;
s3, nitriding the precursor nanofiber at 800 ℃ for 2-8 h to obtain the titanium-vanadium-nitrogen nanofiber current collector;
wherein the molar ratio of the titanium element to the vanadium element in the precursor solution is 4: 1;
the mass volume concentration of the polyvinylpyrrolidone and the solvent in the precursor solution is 0.15 g/mL.
2. Use of the titanium vanadium nitrogen nanofiber current collector as claimed in claim 1 for the preparation of electrodes for lithium sulfur batteries.
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| CN102094261A (en) * | 2009-12-09 | 2011-06-15 | 中国科学院兰州化学物理研究所 | Method for preparing titanium nitride nano fibers |
| CN102255098A (en) * | 2010-05-20 | 2011-11-23 | 索尼公司 | Biofule cell |
| CN103140971A (en) * | 2010-06-25 | 2013-06-05 | 日本硅电子技术株式会社 | Electrode collector material and production method for same |
| CN104532404A (en) * | 2014-12-18 | 2015-04-22 | 长春理工大学 | Vanadium nitride (VN) nano-fiber and preparation method thereof |
| CN107256956A (en) * | 2017-06-28 | 2017-10-17 | 山东大学 | A kind of nitrogen-doped carbon cladding vanadium nitride electrode material and preparation method and application |
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| CN102094261A (en) * | 2009-12-09 | 2011-06-15 | 中国科学院兰州化学物理研究所 | Method for preparing titanium nitride nano fibers |
| CN102255098A (en) * | 2010-05-20 | 2011-11-23 | 索尼公司 | Biofule cell |
| CN103140971A (en) * | 2010-06-25 | 2013-06-05 | 日本硅电子技术株式会社 | Electrode collector material and production method for same |
| CN104532404A (en) * | 2014-12-18 | 2015-04-22 | 长春理工大学 | Vanadium nitride (VN) nano-fiber and preparation method thereof |
| CN107256956A (en) * | 2017-06-28 | 2017-10-17 | 山东大学 | A kind of nitrogen-doped carbon cladding vanadium nitride electrode material and preparation method and application |
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