CN108075135B - Preparation method of vanadium-doped carbon titanium sulfide battery negative electrode material, obtained material and application thereof - Google Patents
Preparation method of vanadium-doped carbon titanium sulfide battery negative electrode material, obtained material and application thereof Download PDFInfo
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- CN108075135B CN108075135B CN201711439760.2A CN201711439760A CN108075135B CN 108075135 B CN108075135 B CN 108075135B CN 201711439760 A CN201711439760 A CN 201711439760A CN 108075135 B CN108075135 B CN 108075135B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a vanadium-doped carbon titanium sulfide battery cathode material, which comprises the following steps: (1) weighing vanadium powder, titanium powder, sulfur powder and carbon powder, and performing ball milling to obtain initial raw materials; (2) carrying out high-temperature self-propagating reaction on the initial raw materials to prepare a solid block sample; (3) performing ball milling treatment on the solid block sample to obtain a powdery small particle sample; (4) and (3) carrying out ultrasonic treatment, centrifugation and drying on the powdery small particle sample to obtain the vanadium-doped carbon titanium sulfide battery cathode material. The invention also discloses the vanadium-doped carbon titanium sulfide battery cathode material prepared by the preparation method and application of the vanadium-doped carbon titanium sulfide battery cathode material in preparing a lithium ion battery. Compared with the prior art, the preparation process is simple, rapid and pollution-free, and the prepared vanadium-carbon-doped titanium sulfide negative electrode material has high specific capacity, good conductivity, electrochemical activity and cycling stability, and is particularly suitable for manufacturing the negative electrode of the lithium ion battery.
Description
Technical Field
The invention relates to a preparation method of a vanadium-doped carbon titanium sulfide battery cathode material, and an obtained material and application thereof, and belongs to the technical field of lithium ion battery cathode materials.
Background
Rechargeable Lithium Ion Batteries (LIBs) are the most widely used electrical energy storage devices because of their advantages of high voltage, high energy density (light weight), low self-discharge rate, long cycle life, etc. The lithium ion battery has wide application range from the lithium ion battery to the micro equipment to transportation, fixed storage and the like, and the lithium ion battery has wide application range and wide performance requirement range, including high power, high energy density, long cycle life and wider working temperature range. Alternative materials are being investigated to meet these requirements.
Ti2SC is the substance with the lowest c/a ratio in S-containing MAX phases. It is therefore reasonable to consider this compound as having particular properties. Due to strong Ti-S hybridization, Ti2SC has high bulk modulus and hardness, and also has the characteristics of high electrical conductivity, high thermal conductivity, high stability, corrosion resistance and the like. Thus Ti2SC is expected to become a novel lithium ion battery cathode material, Xu and the like report that the lithium ion battery cathode material has better lithium storage capacity and about initial reversible capacity under the current density of 4CIs 80mAh g-1After 1000 cycles, the total weight of the product can be increased to 180mAh g-1(ACS Energy Letters, 2016, 1: 1094). However, pure Ti2SC has a very limited lithium storage capacity because it has a compact interlayer structure and is difficult to intercalate lithium ions.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of a vanadium-doped carbon titanium sulfide battery cathode material, which is simple and convenient to operate and low in cost.
The invention also aims to provide the vanadium-doped carbon titanium sulfide battery cathode material prepared by the preparation method, which has low cost and excellent performance.
The invention finally aims to provide the application of the vanadium-doped carbon titanium sulfide battery cathode material in preparing the lithium ion battery, which has high specific capacity and high charging and discharging speed. The cycle life is long.
The technical scheme is as follows: the invention relates to a preparation method of a vanadium-doped carbon titanium sulfide battery cathode material, which comprises the following steps:
(1) weighing vanadium powder, titanium powder, sulfur powder and carbon powder, and performing ball milling to obtain initial raw materials;
(2) carrying out high-temperature self-propagating reaction on the initial raw materials to prepare a solid block sample;
(3) performing ball milling treatment on the solid block sample to obtain a powdery small particle sample;
(4) and (3) carrying out ultrasonic treatment, centrifugation and drying on the powdery small particle sample to obtain the vanadium-doped carbon titanium sulfide battery cathode material.
The molar ratio of the vanadium powder, the titanium powder, the sulfur powder and the carbon powder is (0.05-0.6): (1.4-2.2): (0.8-1.2), preferably V: Ti: S: C (0.1-0.5): (1.5-2.0): 1, more preferably V: Ti: S: C (0.1: 1.9: 1), V: Ti: S: C (0.2: 1.8: 1) and V: Ti: S: C (0.5: 1.5: 1).
And (2) during ball milling in the step (1), the rotating speed is 300-400r/min, the ball milling time is 3-4 hours, and the ball milling is carried out under the condition of inert gas.
And (3) the self-propagating reaction in the step (2) is carried out by adopting a self-propagating synthesis device under the conditions of vacuum and inert gas.
And (3) during ball milling, the rotating speed is 300-400r/min, the ball milling time is 3-4 hours, and the ball milling is carried out under the condition of inert gas.
And (4) performing ultrasonic treatment on the powdery small particle sample and the alcohol according to the proportion of 1g sample per 30ml of absolute ethyl alcohol in the ultrasonic treatment.
The centrifugation condition of the step (4) is 400-600 r/min, and the drying temperature is 55-65 ℃.
The invention also provides the vanadium-doped carbon titanium sulfide battery cathode material prepared by the preparation method and application of the vanadium-doped carbon titanium sulfide battery cathode material in preparing a lithium ion battery.
The technical effects are as follows: compared with the prior art, the preparation process is simple, rapid and pollution-free, and the prepared vanadium-carbon-doped titanium sulfide negative electrode material has high specific capacity, good conductivity, electrochemical activity and cycling stability, and is particularly suitable for manufacturing the negative electrode of the lithium ion battery.
Drawings
FIG. 1: SEM picture of the vanadium-doped carbon titanium sulfide cathode material prepared by the invention.
Detailed Description
The technical solution of the present invention is further illustrated below with reference to specific examples.
Example 1
64.91g of Ti powder with the granularity of 400 meshes, 22.89g of S powder with the granularity of 400 meshes, 8.57g of C powder with the granularity of 400 meshes and 3.64g of V powder with the granularity of 400 meshes are weighed. Mixing uniformly, placing in a vacuum ball milling tank, introducing argon, taking a hard alloy ball as a grinding ball, and ball milling for 3 hours at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain activated powder. Placing the activated powder in a graphite crucible, placing a tungsten wire coil on the surface of the graphite crucible, placing the graphite crucible in a self-propagating high-temperature synthesis device chamber, vacuumizing and filling argon, electrifying the tungsten wire coil to ignite the ball-milling activated powder for self-propagating reaction, and obtaining a blocky product. Putting the block-shaped product into a ball milling tank, taking a hard alloy ball as a milling ball, ball milling for 3h at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain (V,Ti)2SC powder. Mixing the powder small particle sample and alcohol according to the proportion of 1g sample per 30ml absolute ethyl alcohol, ball milling the (V, Ti)2The SC powder and alcohol are put into an ultrasonic cleaning machine for ultrasonic treatment for 24 h. And centrifuging at 500 rpm for 20 minutes after the ultrasonic treatment is finished, then performing suction filtration on the centrifuged upper suspension, and drying in a vacuum drying oven at 60 ℃ for 4 hours to obtain the battery cathode material. And (3) putting the prepared battery negative electrode material, acetylene black and PVDF into a grinding tank for grinding for 45min according to the mass ratio of 8: 1. And (3) until the mixture becomes a viscous liquid, smearing the viscous liquid on a copper sheet, putting the copper sheet into a vacuum drying oven, carrying out vacuum drying for 12 hours at the temperature of 100 ℃, taking out the copper sheet, and putting the copper sheet into a glove box to assemble the lithium battery. The performance of the battery is tested, and after the battery is charged and discharged for 100 times in a constant 400mA/g mode, the specific discharge capacity is 260.3 mAh/g. After 1000 cycles of charge and discharge at a constant 400mA/g, the battery capacity was 899.2 mAh/g.
Example 2
61.36g of Ti powder with the granularity of 400 meshes, 22.84g of S powder with the granularity of 400 meshes, 8.55g of C powder with the granularity of 400 meshes and 7.26g of V powder with the granularity of 400 meshes are weighed. Mixing uniformly, placing in a vacuum ball milling tank, introducing argon, taking a hard alloy ball as a grinding ball, and ball milling for 3 hours at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain activated powder. Placing the activated powder in a graphite crucible, placing a tungsten wire coil on the surface of the graphite crucible, placing the graphite crucible in a self-propagating high-temperature synthesis device chamber, vacuumizing and filling argon, electrifying the tungsten wire coil to ignite the ball-milling activated powder for self-propagating reaction, and obtaining a blocky product. Placing the block-shaped product into a ball milling tank, taking a hard alloy ball as a milling ball, ball milling for 3h at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain (V, Ti)2SC powder. Mixing the powder small particle sample and alcohol according to the proportion of 1g sample per 30ml absolute ethyl alcohol, ball milling the (V, Ti)2And putting the SC powder and alcohol into an ultrasonic cleaning machine for ultrasonic treatment for 24 h. Centrifuging at the speed of 400 rpm for 20 minutes after the ultrasonic treatment is finished, then performing suction filtration on the centrifuged upper suspension, and drying in a vacuum drying oven at the temperature of 55 ℃ for 4 hours to obtain the battery cathode material. Putting the prepared battery cathode material, acetylene black and PVDF into a grinding tank according to the mass ratio of 8: 1Grinding for 45 min. And (3) until the mixture becomes a viscous liquid, smearing the viscous liquid on a copper sheet, putting the copper sheet into a vacuum drying oven, carrying out vacuum drying for 12 hours at the temperature of 100 ℃, taking out the copper sheet, and putting the copper sheet into a glove box to assemble the lithium battery. The performance of the battery is tested, and after the battery is subjected to constant charge and discharge cycles of 400mA/g for 100 times, the specific discharge capacity of the battery is 285.5 mAh/g. After 1000 cycles of charge and discharge at a constant 400mA/g, the battery capacity was 980.2 mAh/g.
Example 3
50.80g of Ti powder with the granularity of 400 meshes, 22.69g of S powder with the granularity of 400 meshes, 8.50g of C powder with the granularity of 400 meshes and 18.02g of V powder with the granularity of 400 meshes are weighed. Mixing uniformly, placing in a vacuum ball milling tank, introducing argon, taking a hard alloy ball as a grinding ball, and ball milling for 3 hours at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain activated powder. Placing the activated powder in a graphite crucible, placing a tungsten wire coil on the surface of the graphite crucible, placing the graphite crucible in a self-propagating high-temperature synthesis device chamber, vacuumizing and filling argon, electrifying the tungsten wire coil to ignite the ball-milling activated powder for self-propagating reaction, and obtaining a blocky product. Placing the block-shaped product into a ball milling tank, taking a hard alloy ball as a milling ball, ball milling for 3h at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain (V, Ti)2SC powder. Mixing the powder small particle sample and alcohol according to the proportion of 1g sample per 30ml absolute ethyl alcohol, ball milling the (V, Ti)2And putting the SC powder and alcohol into an ultrasonic cleaning machine for ultrasonic treatment for 24 h. And centrifuging for 20 minutes at a speed of 600 rpm after the ultrasonic treatment is finished, then performing suction filtration on the centrifuged upper suspension, and drying for 4 hours in a vacuum drying oven at a temperature of 65 ℃ to obtain the battery cathode material. And (3) putting the prepared battery negative electrode material, acetylene black and PVDF into a grinding tank for grinding for 45min according to the mass ratio of 8: 1. And (3) until the mixture becomes a viscous liquid, smearing the viscous liquid on a copper sheet, putting the copper sheet into a vacuum drying oven, carrying out vacuum drying for 12 hours at the temperature of 100 ℃, taking out the copper sheet, and putting the copper sheet into a glove box to assemble the lithium battery. The performance of the battery is tested, and after the battery is charged and discharged for 100 times in a constant 400mA/g mode, the specific discharge capacity is 234.5 mAh/g. After 1000 cycles of charge and discharge at a constant 400mA/g, the battery capacity was 837.6 mAh/g.
Example 4
61.36g of the powder with the granularity of 400 meshes are weighedTi powder, 22.84g of S powder with the granularity of 400 meshes, 8.55g of C powder with the granularity of 400 meshes and 7.26g of V powder with the granularity of 400 meshes. Mixing uniformly, placing in a vacuum ball milling tank, introducing argon, taking a hard alloy ball as a grinding ball, and carrying out ball milling for 3h at the rotating speed of 300r/min according to the ball-material ratio of 10: 1 to obtain activated powder. Placing the activated powder in a graphite crucible, placing a tungsten wire coil on the surface of the graphite crucible, placing the graphite crucible in a self-propagating high-temperature synthesis device chamber, vacuumizing and filling argon, electrifying the tungsten wire coil to ignite the ball-milling activated powder for self-propagating reaction, and obtaining a blocky product. Placing the block-shaped product in a ball milling tank, taking a hard alloy ball as a milling ball, and ball milling for 3h at the rotating speed of 300r/min according to the ball-material ratio of 10: 1 to obtain (V, Ti)2SC powder. Mixing the powder small particle sample and alcohol according to the proportion of 1g sample per 30ml absolute ethyl alcohol, ball milling the (V, Ti)2And putting the SC powder and alcohol into an ultrasonic cleaning machine for ultrasonic treatment for 24 h. And centrifuging for 20 minutes at 450 rpm after the ultrasonic treatment is finished, then performing suction filtration on the centrifuged upper suspension, and drying for 4 hours in a vacuum drying oven at 58 ℃ to obtain the battery cathode material. And (3) putting the prepared battery negative electrode material, acetylene black and PVDF into a grinding tank for grinding for 45min according to the mass ratio of 8: 1. And (3) until the mixture becomes a viscous liquid, smearing the viscous liquid on a copper sheet, putting the copper sheet into a vacuum drying oven, carrying out vacuum drying for 12 hours at the temperature of 100 ℃, taking out the copper sheet, and putting the copper sheet into a glove box to assemble the lithium battery. The performance of the battery is tested, and after the battery is subjected to constant charge and discharge cycles of 400mA/g for 100 times, the specific discharge capacity of the battery is 269.4 mAh/g. After 1000 cycles of charge and discharge at a constant 400mA/g, the battery capacity was 960.2 mAh/g.
Comparative example: pure carbon titanium sulfide
68.48g of Ti powder with the granularity of 400 meshes, 22.94g of S powder with the granularity of 400 meshes and 9.00g of C powder with the granularity of 400 meshes are weighed. Mixing uniformly, placing in a vacuum ball milling tank, introducing argon, taking a hard alloy ball as a grinding ball, and ball milling for 3 hours at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain activated powder. Placing the activated powder in a graphite crucible, placing a tungsten wire coil on the surface of the graphite crucible, placing the graphite crucible in a self-propagating high-temperature synthesis device chamber, vacuumizing and filling argon, electrifying the tungsten wire coil to ignite the ball-milling activated powder for self-propagating reaction, and obtaining a blocky product.Placing the block-shaped product in a ball milling tank, taking a hard alloy ball as a milling ball, and carrying out ball milling for 3h at the rotating speed of 400r/min according to the ball-material ratio of 10: 1 to obtain Ti2SC powder. The sample and alcohol are mixed according to the proportion of 1g sample per 30ml absolute ethyl alcohol, and the Ti after ball milling is carried out2And putting the SC powder and alcohol into an ultrasonic cleaning machine for ultrasonic treatment for 24 h. And centrifuging at 500 rpm for 20 minutes after the ultrasonic treatment is finished, then performing suction filtration on the centrifuged upper suspension, and drying in a vacuum drying oven at 60 ℃ for 4 hours to obtain the battery cathode material. And (3) putting the prepared battery negative electrode material, acetylene black and PVDF into a grinding tank for grinding for 45min according to the mass ratio of 8: 1. And (3) until the mixture becomes a viscous liquid, smearing the viscous liquid on a copper sheet, putting the copper sheet into a vacuum drying oven, carrying out vacuum drying for 12 hours at the temperature of 100 ℃, taking out the copper sheet, and putting the copper sheet into a glove box to assemble the lithium battery. And (3) testing the performance of the battery, wherein after constant charge and discharge cycles of 400mA/g are carried out for 100 times, the specific discharge capacity is 119.0 mAh/g. After 1000 cycles of charge and discharge at a constant 400mA/g, the battery capacity was 493.7 mAh/g.
Claims (8)
1. A preparation method of a vanadium-doped carbon titanium sulfide battery cathode material is characterized by comprising the following steps:
(1) taking vanadium powder, titanium powder, sulfur powder and carbon powder, and performing ball milling to obtain initial raw materials;
(2) carrying out high-temperature self-propagating reaction on the initial raw materials to prepare a solid block sample;
(3) performing ball milling treatment on the solid block sample to obtain a powdery small particle sample;
(4) carrying out ultrasonic treatment, centrifugation and drying on the powdery small particle sample to obtain the vanadium-doped carbon titanium sulfide battery cathode material;
wherein the molar ratio of the vanadium powder, the titanium powder, the sulfur powder and the carbon powder is (0.05-0.6): (1.4-2.2): (0.8-1.2).
2. The preparation method of the vanadium-doped carbon titanium sulfide battery cathode material as claimed in claim 1, wherein the ball milling in the step (1) is performed at a rotation speed of 300-400r/min for 3-4 hours under an inert gas condition.
3. The method for preparing the vanadium-doped carbon titanium sulfide battery cathode material as claimed in claim 1, wherein the self-propagating reaction in the step (2) is carried out in a self-propagating synthesis device under vacuum and inert gas conditions.
4. The preparation method of the vanadium-doped carbon titanium sulfide battery cathode material as claimed in claim 1, wherein the ball milling in the step (3) is performed at a rotation speed of 300-400r/min for 3-4 hours under an inert gas condition.
5. The method for preparing the vanadium-doped carbon titanium sulfide battery cathode material as claimed in claim 1, wherein the ultrasonic treatment of the sample of the powdery small particles and the alcohol in the step (4) is carried out at a ratio of 1g sample per 30ml of absolute ethanol.
6. The method for preparing the vanadium-doped carbon titanium sulfide battery cathode material as claimed in claim 1, wherein the centrifugation in the step (4) is performed at 400-600 rpm and the drying temperature is 55-65 ℃.
7. The vanadium-doped carbon titanium sulfide battery cathode material prepared by the preparation method of any one of claims 1 to 6.
8. The use of the vanadium-doped carbon titanium sulfide battery negative electrode material of claim 7 for the preparation of lithium ion batteries.
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| "三元层状化合物Ti2SC的制备及应用研究";王雨晨;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20160615;第18-51页 * |
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