CN111900371A - Titanium nitride/sulfur composite material for lithium-sulfur battery anode and preparation method thereof - Google Patents
Titanium nitride/sulfur composite material for lithium-sulfur battery anode and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a titanium nitride/sulfur composite material for a lithium-sulfur battery anode and a preparation method thereof. The method mainly comprises the surface treatment of titanium foil, TiO2Preparing a long nanotube array, crystallizing and roasting, preparing a TiN nanotube array, carrying sulfur and the like. The specific surface area of the material is improved by preparing TiN with the nanotube array arrangement morphology, and meanwhile, the TiN material has good flexibility, and the special tubular arrangement morphology of the TiN material is beneficial to loading sulfur and inhibiting volume expansion. The high conductivity of TiN can further improve the electrochemical performance, and the assembled battery has high specific capacity, high multiplying power and ultra-long cycle performance.
Description
Technical Field
The invention belongs to the field of lithium-sulfur battery anode materials, and particularly relates to a titanium nitride/sulfur composite material for a lithium-sulfur battery anode and a preparation method thereof.
Background
With the rapid development of electric vehicles and large-scale energy storage devices, the demand for rechargeable batteries with high energy density and long cycle life is increasingly urgent. Sulfur has high theoretical specific capacity (1675mA h g-1) High natural abundance, low slip ratio and environmental friendlinessAnd the like, and is considered as a candidate material of the next generation energy storage device. Compared with a commercial lithium ion battery, the lithium-sulfur battery has more excellent performance, and the theoretical energy density is 2600 Wh/kg. However, the lithium sulfur battery still has some problems that hinder the application and development thereof, such as insulation of sulfur, volume expansion during the cycle, shuttle effect of soluble polysulfide, dendritic growth of lithium negative electrode, and rapid consumption of electrolyte. To solve the above problems, the most common method is to support sulfur on a material with good conductivity as a cathode of a lithium sulfur battery, including a porous carbon/sulfur composite material, a metal-based compound, a graphene-based material, a carbon nanotube, and the like. However, carbon-based materials tend to be less adsorptive of polysulfides, limiting the shuttling effect of polysulfides for only a short period of time. Research shows that the transition metal nitride has strong adsorption effect on the LiPS, has excellent conductivity, is an ideal carrier for sulfur, and can effectively inhibit shuttle effect of sulfide in the charge-discharge process.
Disclosure of Invention
The invention provides a titanium nitride/sulfur composite material for a lithium-sulfur battery anode and a preparation method thereof, aiming at overcoming the defects of poor sulfur conductivity and volume expansion and shuttle effect in the charging and discharging processes of a lithium-sulfur battery. The specific surface area of the material is improved by preparing TiN with the nanotube array arrangement morphology, and meanwhile, the TiN material has good flexibility, and the special tubular arrangement morphology of the TiN material is beneficial to loading sulfur and inhibiting volume expansion. In addition, TiN has good conductivity, and makes up for the defect of poor conductivity of sulfur.
The technical scheme of the invention is as follows: a preparation method of a titanium nitride/sulfur composite material for a positive electrode of a lithium-sulfur battery comprises the following steps:
(1) surface treatment of titanium foil
Carrying out ultrasonic treatment on a pure titanium foil with the thickness of 0.1mm in a mixed solution of acetone and ethanol for 2 hours, placing the pure titanium foil in a concentrated nitric acid solution for chemical polishing, then washing the pure titanium foil with deionized water, and finally drying the pure titanium foil under the protection of nitrogen;
(2)TiO2preparation of long nanotube arrays
Oxidizing titanium foil in aqueous solution containing 2mg/mL ammonium fluoride and 8mg/mL ethylene glycol for 2h at constant potential of 60V to obtain TiO2A long nanotube array;
(3) crystallization roasting
TiO prepared in the step (2)2Roasting the long nanotube array in air at 450-600 ℃ for 2h to realize phase change from an amorphous state to an anatase type;
(4) preparation of TiN nanotube array
TiO phase-changed in the step (3)2The long nanotube array is subjected to gradient temperature rise to 600-800 ℃ in an ammonia atmosphere, heat preservation is carried out for 3 hours, and then cooling is carried out to room temperature, so as to obtain a TiN nanotube array;
(5) carrying sulfur
Mixing the prepared TiN nanotube array and pure sulfur powder in a ratio of 1:3, fully grinding, and placing the obtained ground mixture in a reaction kettle for hydrothermal reaction to obtain the titanium nitride/sulfur composite material.
The gradient temperature rise process in the step (4) comprises the following stages: ∙ min at 5 DEG C-1The heating rate of (2) is increased from room temperature to 300 ℃; at 2 ℃ for ∙ min-1The heating rate of (2) is from 300 ℃ to 700 ℃; at 1 ℃ for ∙ min-1The rate of temperature rise of (2) is from 700 ℃ to 800 ℃.
The gradient temperature rise process in the step (4) comprises the following stages: ∙ min at 5 DEG C-1The temperature rising rate of (2) is increased from room temperature to 200 ℃; at 2 ℃ for ∙ min-1The heating rate of (2) is from 200 ℃ to 500 ℃; at 1 ℃ for ∙ min-1The rate of temperature rise of (2) is from 500 ℃ to 600 ℃.
The temperature of the hydrothermal reaction in the step (5) is 155 ℃, and the heat preservation time is 12 h.
The titanium nitride/sulfur composite material for the positive electrode of the lithium-sulfur battery is prepared by the method.
The invention has the beneficial effects that: the TiN in nanotube array shape prepared by the method has the advantages that one end of the hollow tubes is sealed, the other end of the hollow tubes is open, and the hollow tubes are spaced, so that the TiN has high specific surface area and high sulfur fixation effect. Meanwhile, the synthesized TiN has high conductivity, so that the problem of poor conductivity of sulfur elementary substances in the lithium-sulfur battery is solved. In addition, TiN as a transition metal nitride has higher chemical stability, can generate a large number of LiPS loading sites in the charging and discharging process of the lithium-sulfur battery, has strong adsorption capacity on the LiPS, can generate strong interaction with the LiPS, and limits polysulfide near the surface of an electrode, thereby more effectively inhibiting the shuttle effect. The high conductivity of TiN can further improve the electrochemical performance, and the assembled battery has high specific capacity, high multiplying power and ultra-long cycle performance.
The TiN prepared by the method is expected to promote the practicability of the lithium-sulfur battery with excellent specific capacity and cycle performance due to the unique structural design and the simple preparation process. In consideration of the stability of the ultra-long cycle, the lithium-sulfur battery has great application potential in the aspects of electric automobiles, portable electronic products, implantable sensors, medical equipment and the like.
Drawings
FIG. 1 is a graph showing the cycle performance of the TiN/S composite material obtained in examples 1-3 for the first 50 cycles of a lithium sulfur battery at a rate of 0.2 c.
FIG. 2 is a first turn of charge and discharge curves of the TiN/S composite material obtained in examples 1-3 for a lithium sulfur battery at a rate of 0.2 c.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
(1) Carrying out ultrasonic treatment on a pure titanium (Ti) foil with the thickness of 0.1mm in a mixed solution of acetone and ethanol for 2h, then carrying out chemical polishing in a concentrated nitric acid solution, then washing with deionized water, and finally drying the titanium foil under the protection of nitrogen.
(2) Oxidizing titanium foil in aqueous solution containing 2mg/mL ammonium fluoride and 8mg/mL ethylene glycol for 2h at constant potential of 60V to obtain TiO2An array of long nanotubes.
(3) Prepared TiO2The long nanotube array is roasted for 2h at 450 ℃ in the air, and the phase change from the amorphous state to the anatase type is realized.
(4) Converting the phase-changed TiO into2Heating the long nanotube array in ammonia gas to 800 ℃, preserving the heat for 3h, and then cooling to room temperature to obtain the TiN nanotube array. The temperature rise rate is divided into the following stages: the temperature rising rate from room temperature to 300 ℃ is 5 ℃ ∙ min-1The temperature rise rate from 300 to 700 ℃ is 2 ℃ ∙ min-1The temperature rise rate from 700 to 800 ℃ is ∙ min at 1 DEG C-1。
(5) Mixing the prepared TiN nanotube array and pure sulfur powder in a ratio of 1:3, fully grinding, placing the obtained ground mixture in a reaction kettle, and preserving heat for 12 hours at 155 ℃ to carry out hydrothermal reaction, thus obtaining the titanium nitride/sulfur composite material.
The TiN/S composite material prepared in example 1 was mixed with Ketjen black and polyvinylidene fluoride (PVDF) at a ratio of 8:1:1, and then ground for 30 minutes. Then dissolving the powder in a proper amount of NMP solution, grinding for 30 minutes to fully dissolve TiN/S powder in the NMP solution, and finally coating the fully ground slurry on an aluminum foil with a scraper, wherein the thickness of the fully ground slurry is 15 mm.
Example 2
(1) Carrying out ultrasonic treatment on a pure titanium (Ti) foil with the thickness of 0.1mm in a mixed solution of acetone and ethanol for 2h, then carrying out chemical polishing in a concentrated nitric acid solution, then washing with deionized water, and finally drying the titanium foil under the protection of nitrogen.
(2) Oxidizing titanium foil in aqueous solution containing 2mg/mL ammonium fluoride and 8mg/mL ethylene glycol for 2h at constant potential of 60V to obtain TiO2An array of long nanotubes.
(3) Prepared TiO2The long nanotube array is roasted for 2h at 600 ℃ in the air, and the phase change from the amorphous state to the anatase type is realized.
(4) Converting the phase-changed TiO into2Heating the long nanotube array in ammonia gas to 800 ℃, preserving the heat for 3h, and then cooling to room temperature to obtain the TiN nanotube array. The temperature rise rate is divided into the following stages: the temperature rising rate from room temperature to 300 ℃ is 5 ℃ ∙ min-1The temperature rise rate from 300 to 700 ℃ is 2 ℃ ∙ min-1The temperature rise rate from 700 to 800 ℃ is ∙ min at 1 DEG C-1。
(5) Mixing the prepared TiN nanotube array and pure sulfur powder in a ratio of 1:3, fully grinding, placing the obtained ground mixture in a reaction kettle, and preserving heat for 12 hours at 155 ℃ to carry out hydrothermal reaction, thus obtaining the titanium nitride/sulfur composite material.
Example 3
(1) Carrying out ultrasonic treatment on a pure titanium (Ti) foil with the thickness of 0.1mm in a mixed solution of acetone and ethanol for 2h, then carrying out chemical polishing in a concentrated nitric acid solution, then washing with deionized water, and finally drying the titanium foil under the protection of nitrogen.
(2) Oxidizing titanium foil in aqueous solution containing 2mg/mL ammonium fluoride and 8mg/mL ethylene glycol for 2h at constant potential of 60V to obtain TiO2An array of long nanotubes.
(3) Prepared TiO2The long nanotube array is roasted for 2h at 450 ℃ in the air, and the phase change from the amorphous state to the anatase type is realized.
(4) Converting the phase-changed TiO into2Heating the long nanotube array in ammonia gas to 600 ℃, preserving heat for 3h, and then cooling to room temperature to obtain the TiN nanotube array. The temperature rise rate is divided into the following stages: the temperature rising rate from room temperature to 200 ℃ is 5 ℃ ∙ min-1The temperature rise rate from 200 to 500 ℃ is 2 ℃ ∙ min-1The temperature rise rate from 500 to 600 ℃ is 1 ℃ for ∙ min-1。
(5) Mixing the prepared TiN nanotube array and pure sulfur powder in a ratio of 1:3, fully grinding, placing the obtained ground mixture in a reaction kettle, and preserving heat for 12 hours at 155 ℃ to carry out hydrothermal reaction, thus obtaining the titanium nitride/sulfur composite material.
And (3) analyzing a test result:
the titanium nitride/sulfur composite material synthesized in the example 1 has good cycle performance as a positive electrode material of a lithium-sulfur battery, and as shown in fig. 1 and 2, the specific discharge capacity of the battery in the first circle can reach 1221mA h ∙ g at a rate of 0.2C-1After 50 cycles, 785mA h ∙ g can still be remained-1The specific discharge capacity of the battery is obviously superior to the electrochemical performance of the batteries of the examples 2 and 3. The experimental parameters illustrated under example 1 are optimal. Meanwhile, the battery of the embodiment 1 keeps certain stability in the circulation process, and the attenuation of each circleThe reduction rate is only 0.71%, which shows that after TiN is introduced as a sulfur carrier material, the cycle capacity of the lithium-sulfur battery is remarkably improved, and the influence of polysulfide shuttle effect and poor sulfur conductivity on the electrochemical performance of the battery is effectively inhibited.
Claims (5)
1. A preparation method of a titanium nitride/sulfur composite material for a positive electrode of a lithium-sulfur battery comprises the following steps:
(1) surface treatment of titanium foil
Carrying out ultrasonic treatment on a pure titanium foil with the thickness of 0.1mm in a mixed solution of acetone and ethanol for 2 hours, placing the pure titanium foil in a concentrated nitric acid solution for chemical polishing, then washing the pure titanium foil with deionized water, and finally drying the pure titanium foil under the protection of nitrogen;
(2)TiO2preparation of long nanotube arrays
Oxidizing titanium foil in aqueous solution containing 2mg/mL ammonium fluoride and 8mg/mL ethylene glycol for 2h at constant potential of 60V to obtain TiO2A long nanotube array;
(3) crystallization roasting
TiO prepared in the step (2)2Roasting the long nanotube array in air at 450-600 ℃ for 2h to realize phase change from an amorphous state to an anatase type;
(4) preparation of TiN nanotube array
TiO phase-changed in the step (3)2The long nanotube array is subjected to gradient temperature rise to 600-800 ℃ in an ammonia atmosphere, heat preservation is carried out for 3 hours, and then cooling is carried out to room temperature, so as to obtain a TiN nanotube array;
(5) carrying sulfur
Mixing the prepared TiN nanotube array and pure sulfur powder in a ratio of 1:3, fully grinding, and placing the obtained ground mixture in a reaction kettle for hydrothermal reaction to obtain the titanium nitride/sulfur composite material.
2. The method according to claim 1, wherein the step (4) comprises the following steps: ∙ min at 5 DEG C-1The heating rate of (2) is increased from room temperature to 300 ℃; at 2 ℃ for ∙ min-1Temperature rising rate of from 300 DEG CTo 700 ℃; at 1 ℃ for ∙ min-1The rate of temperature rise of (2) is from 700 ℃ to 800 ℃.
3. The method according to claim 1, wherein the step (4) comprises the following steps: ∙ min at 5 DEG C-1The temperature rising rate of (2) is increased from room temperature to 200 ℃; at 2 ℃ for ∙ min-1The heating rate of (2) is from 200 ℃ to 500 ℃; at 1 ℃ for ∙ min-1The rate of temperature rise of (2) is from 500 ℃ to 600 ℃.
4. The method according to claim 1, wherein the hydrothermal reaction in step (5) is carried out at 155 ℃ for 12 hours.
5. The titanium nitride/sulfur composite material for a positive electrode of a lithium-sulfur battery, prepared according to any one of claims 1 to 4.
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Cited By (4)
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CN113511638A (en) * | 2021-06-30 | 2021-10-19 | 南京邮电大学 | Preparation method of TiN-S composite anode material by plasma chemical vapor codeposition |
CN113955726A (en) * | 2021-10-20 | 2022-01-21 | 安徽工程大学 | Titanium nitride micro-nano tube/sulfur composite material, preparation method thereof, lithium-sulfur battery anode and lithium-sulfur battery |
CN114079052A (en) * | 2021-11-16 | 2022-02-22 | 江西省科学院应用化学研究所 | Nanotube tungsten nitride/sulfur positive electrode material and preparation method thereof |
CN114464788A (en) * | 2022-01-14 | 2022-05-10 | 南京邮电大学 | Lithium-sulfur battery composite positive electrode material and preparation method and application thereof |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113511638A (en) * | 2021-06-30 | 2021-10-19 | 南京邮电大学 | Preparation method of TiN-S composite anode material by plasma chemical vapor codeposition |
CN113511638B (en) * | 2021-06-30 | 2022-12-06 | 南京邮电大学 | Preparation method of TiN-S composite anode material by plasma chemical vapor codeposition |
CN113955726A (en) * | 2021-10-20 | 2022-01-21 | 安徽工程大学 | Titanium nitride micro-nano tube/sulfur composite material, preparation method thereof, lithium-sulfur battery anode and lithium-sulfur battery |
CN113955726B (en) * | 2021-10-20 | 2022-12-09 | 安徽工程大学 | Titanium nitride micro-nano tube/sulfur composite material, preparation method thereof, lithium-sulfur battery anode and lithium-sulfur battery |
CN114079052A (en) * | 2021-11-16 | 2022-02-22 | 江西省科学院应用化学研究所 | Nanotube tungsten nitride/sulfur positive electrode material and preparation method thereof |
CN114079052B (en) * | 2021-11-16 | 2023-03-14 | 江西省科学院应用化学研究所 | Nanotube tungsten nitride/sulfur positive electrode material and preparation method thereof |
CN114464788A (en) * | 2022-01-14 | 2022-05-10 | 南京邮电大学 | Lithium-sulfur battery composite positive electrode material and preparation method and application thereof |
CN114464788B (en) * | 2022-01-14 | 2024-02-06 | 南京邮电大学 | Lithium-sulfur battery composite positive electrode material and preparation method and application thereof |
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