CN109830657B - MoS2/MoO2Preparation method of three-dimensional carbon lithium ion battery cathode material - Google Patents
MoS2/MoO2Preparation method of three-dimensional carbon lithium ion battery cathode material Download PDFInfo
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Abstract
The invention discloses a MoS2/MoO2A preparation method of a three-dimensional carbon lithium ion battery cathode material. The fruit residue carbon and ammonium molybdate are used as precursors, and the ammonium molybdate is decomposed into MoO under the high-temperature condition3Further carrying out oxidation reduction reaction with S powder to obtain MoO2In-situ synthesis method is adopted to make MoS2Nanosheet and MoO2Growing on the three-dimensional pomace carbon to form MoS with three-dimensional carbon support2/MoO2A composite material. The method can effectively disperse the three-dimensional carbon nano material, effectively regulate and control the structure of the composite nano material and ensure the tight combination of the components. The obtained product has high volume capacity of the lithium ion battery and good cycle performance. And the preparation process is simple and easy to control, the period is short, the energy consumption is low, the repeatability of the product is high, the yield is high, and the large-scale production is facilitated.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a MoS2/MoO2A preparation method of a three-dimensional carbon lithium ion battery cathode material.
Background
With the wide attention of people to clean energy and renewable resources, lithium ion batteries have been widely used as working power sources (mobile phones, notebook computers, digital cameras, etc.) of various electronic products and power batteries of mobile equipment(electric vehicles, submarines, missile launching, etc.). Compared with the conventional secondary battery, the lithium ion battery has the advantages of high energy, high operating voltage, high safety, small environmental pollution and the like, and is considered as the most promising chemical power source. At present, the negative electrode material of the secondary battery is mainly a carbon-based material, but the theoretical capacity of the material is only 372mAh g-1And the current requirements of people for small volume and large capacity are difficult to meet. In addition, the carbon-based material is easy to fall off during the charging and discharging process, and has a safety problem, so that the search for a new lithium ion battery anode material capable of replacing the carbon-based material becomes a hot spot of the current research.
Much research work has been done to find alternative materials for the negative electrode having high capacity, among which transition metal oxides and sulfides such as Co3O4、SnO2And MoS2And the like, show higher capacity when used as a negative electrode material of a lithium ion battery, and attract extensive attention. ([1]Wang T,Li H,Shi S.2D Film of Carbon NanofibersElastically Astricted MnO Microparticles:A Flexible Binder-Free Anode forHighly Reversible Lithium Ion Storage.Small, 2017.[2]Xu J,Zhang J,Zhang W,etal.Interlayer Nanoarchitectonics of Two-Dimensional Transition-MetalDichalcogenides Nanosheets for Energy Storage and ConversionApplications.Advanced Energy Materials,1700571,2017.[3]Zhanwei Xu,HuanleiWang,Zhi Li,Alireza Kohandehghan,Jia Ding,Jian Chen,Kai Cui,David Mitlin:Sulfur refines MoO2distribution enabling improved lithium ion batteryperformance.The Journal of Physical Chemistry C 118,18387-18396,2014.)
MoS2With a unique layered structure, the atoms between the S-Mo-S sheets are strongly covalent bonded, while the S-Mo-S layers are bonded by van der Waals forces, which is Li+Provides space and access. The lithium ion battery cathode active material is used as a lithium ion battery cathode active material, and the theoretical capacity is 670mAh g-1. However, due to the sheet-like MoS2When used as a negative electrode material of a lithium ion battery, the lithium ion battery shows poor stability due to superposition of charge and discharge, poor conductivity and the like ([4 ]]Yongji Gong,Shubin Yang,Liang Zhan, Lulu Ma, Robert Vajtai, Pulickel M.Ajayan: A bottom-up pro rod to build 3D architecture from biosheets for super organic materials 24,125-130,2014.). In order to solve the problem, a great deal of research is carried out on inhibiting the collapse of the structure of the molybdenum disulfide during the charge and discharge processes by changing the two-dimensional layered structure of the molybdenum disulfide, and improving the electrochemical performance of the molybdenum disulfide material. For example, the structure of molybdenum disulfide is regulated and controlled by a hydrothermal method, and ultrathin, bent and porous molybdenum disulfide is prepared. ([5]J.-W.Jiang,Z. Qi,H.S.Park,T.Rabczuk,Elastic bending modulus of single-layermolybdenum disulfide(MoS2):finite thickness effect,Nanotechnology,24,435705,2013.[6]J. Kibsgaard,Z.Chen,B.N.Reinecke,T.F.Jaramillo,Engineering thesurface structure of MoS2to preferentially expose active edge sites forelectrocatalysis,Nature Materials,11,963,2012.[7]H.Liu,F.Zhang,W.Li,X.Zhang,C.S.Lee,W.Wang,Y. Tang,Porous tremella-like MoS2Polyurethane composites with enhanced performance for lithium-ion batteries and electronics Acta 167,132-138, 2015) furthermore, the introduction of carbon additives such as carbon nanotubes, graphene with large specific surface area and high conductivity has been investigated and generally used to improve the cycle performance of these materials ([8 ]]Yang Zhao,Ying Huang,XuSun,Haijian Huang,Ke Wang,Meng Zong,Qiufen Wang:Hollow Zn2SnO4boxes wrappedwith flexible graphene as anode materials for lithium batteriesElectrochimica Acta 120,128–132,2014.)。
Disclosure of Invention
The invention aims to provide a MoS2/MoO2Preparation method of three-dimensional carbon lithium ion battery cathode material, the method has simple and easily controlled preparation process, short reaction period, low energy consumption, high repeatability and high yield, and MoS prepared by the method2/MoO2The three-dimensional carbon material used for the lithium ion battery cathode material has the characteristics of high discharge specific capacity, good cycle stability and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) dissolving 0.1-1 g of KOH in 50ml of deionized water, and then adding 0.5-1.5 g of apple pomace into the deionized water to mix to obtain a solution A;
2) putting the solution A into a high-temperature and high-pressure sterilizer, placing the sterilizer in an oven, preserving heat at 180-210 ℃ for 18-26 h, cooling to room temperature, taking out a product, and evaporating the obtained solution to dryness at 100-115 ℃ to remove water to obtain a product B;
3) putting the product B into a magnetic boat, and putting the magnetic boat into a tube furnace from room temperature for 5-10 ℃ min-1Heating to 500-700 ℃ at a heating rate, calcining for 2-3 h, cooling to room temperature along with the furnace, cleaning with deionized water and ethanol, and drying to obtain a product C;
4) mixing the raw materials in a ratio of 1: (0.1-10) taking the product C and ammonium molybdate according to the mass ratio, and uniformly mixing and grinding to obtain a preform D;
5) according to the following steps of 1: (0.5-10) taking the prefabricated body D and S powder according to the mass ratio, uniformly grinding, placing in a porcelain boat, and carrying out 5-10 ℃ min under the argon condition-1The temperature rising rate is increased from room temperature to 600-750 ℃, and the reaction is carried out for 0.5-2 h under the condition of heat preservation, so as to obtain a product E;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
The reaction vessel in the step 1) is a stainless steel reaction inner kettle.
And 5) when the temperature is raised to 150 ℃, closing the argon flow.
The invention selects MoO2Can play the role of a conductive material and can partially or even completely replace the carbon nano material. The electrode material with high volume specific capacity is expected to be obtained. But if MoO is used alone2As MoS2Of conductive material and substrate, MoO2The material is an active material, and volume expansion is caused by charge and discharge, so that the structure of the whole material is collapsed. Therefore, the three-dimensional porous marc carbon material is selected as the nano support material. The pomace has rich fiber porous structure, the main components of the pomace comprise pectin, hemicellulose, lignin and the like, the pomace is a precursor prepared by excellent biochar, and the organic plastid with larger radius can effectively increase the interlayer spacing of the materialRapid transport of ions provides conditions. The waste fruit residues generated by a fruit juice factory are recycled to prepare the high-performance carbon nano material, so that the additional value of resources can be improved, the production cost of the battery is reduced, considerable economic benefits are obtained, and the environmental pollution can be reduced.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a MoS2/MoO2The preparation method of the three-dimensional carbon lithium ion battery cathode material is used for synthesizing the porous three-dimensional pomace carbon nanomaterial by hydrothermal activation, carbonization in an inert atmosphere in a tube furnace and the like. Mixing the prepared carbon nano-particles with ammonium molybdate to obtain a preform, further mixing the preform with sulfur powder, and decomposing the ammonium molybdate to generate MoO under the condition of argon atmosphere in a tube furnace3. S powder and MoO exist in a reaction environment in a gaseous state in the process of sublimation of S powder in the reaction process3Fully contact to realize MoO3Is completely reduced into MoO2Newly synthesized MoO2Further is partially vulcanized by S powder to finally form carbon-supported MoS2/MoO2A composite material. The S powder has dual roles of a reducing agent and a vulcanizing agent;
MoO3+S＝MoO2+SO2
MoO2+S＝MoS2+SO2
MoO2the framework plays a role in structural support, and the flaky MoS is avoided2And the material conductivity is improved and the material cycling stability is also improved by superposition. The preparation process is simple and easy to control, the period is short, the energy consumption is low, the repeatability of the product is high, the yield is high, and the large-scale production is facilitated.
Drawings
FIG. 1 shows MoS prepared according to the present invention2/MoO2XRD pattern of three-dimensional carbon lithium ion battery cathode material, wherein x-ray incident angle is twice of abscissa, and intensity after diffraction is on ordinate.
FIG. 2 shows MoS prepared according to the present invention2/MoO2SEM photograph of three-dimensional carbon lithium ion battery cathode material;
FIG. 3 shows MoS prepared according to the present invention2/MoO2The cycle performance test chart of the three-dimensional carbon lithium ion battery negative electrode material comprises the cycle number of a horizontal coordinate and the mass specific capacity of a vertical coordinate.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
1) dissolving 0.4g of KOH in 50ml of deionized water, adding 0.5g of apple pomace in a stainless steel reaction inner kettle, and mixing to obtain a solution A;
2) putting the solution A into a high-temperature high-pressure sterilizer, placing the sterilizer in an oven, preserving the heat at 180 ℃ for 20 hours, cooling to room temperature, taking out the product, and evaporating the obtained solution at 100 ℃ to remove water to obtain a product B;
3) placing the product B in a magnetic boat, and placing in a tube furnace from room temperature for 5 deg.C min-1Heating to 500 ℃ at the heating rate, calcining for 3h, cooling to room temperature along with the furnace, cleaning with deionized water and ethanol, and drying to obtain a product C;
4) mixing the raw materials in a ratio of 1: 3, uniformly mixing and grinding the product C and ammonium molybdate to obtain a preform D;
5) according to the following steps of 1: 2, grinding the powder D and S uniformly, placing the powder in a porcelain boat, and carrying out argon gas treatment at 5 ℃ for min-1The temperature rising rate is increased from room temperature to 600 ℃, the reaction is carried out for 2 hours in a heat preservation way, and a product E is obtained, wherein when the temperature rises to 150 ℃, the argon flow is closed, so that the high-concentration S steam and the prefabricated body D are kept to fully react;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
Example 2:
1) dissolving 1g of KOH in 50ml of deionized water, adding 1.5g of apple pomace in a stainless steel reaction inner kettle, and mixing to obtain a solution A;
2) putting the solution A into a high-temperature and high-pressure sterilizer, placing the sterilizer in an oven, preserving heat at 210 ℃ for 18h, cooling to room temperature, taking out a product, and evaporating the obtained solution to dryness at 115 ℃ to remove water to obtain a product B;
3) placing the product B in a magnetic boat, and placing in a tube furnace from room temperature for 5 deg.C min-1Heating to 700 ℃ at a heating rate, calcining for 2h, cooling to room temperature along with the furnace, cleaning with deionized water and ethanol, and drying to obtain a product C;
4) mixing the raw materials in a ratio of 1: 4, uniformly mixing and grinding the product C and ammonium molybdate to obtain a preform D;
5) according to the following steps of 1: 3, grinding the powder D and S uniformly, placing the powder in a porcelain boat, and carrying out argon gas treatment at 10 ℃ for min-1The temperature rising rate is increased from room temperature to 700 ℃, the reaction is carried out for 2 hours under the condition of heat preservation, a product E is obtained, and when the temperature rises to 150 ℃, argon flow is closed, so that the high-concentration S steam and the prefabricated body D are kept to fully react;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
Example 3:
1) dissolving 0.5g of KOH in 50ml of deionized water, adding 1g of apple pomace in a stainless steel reaction inner kettle, and mixing to obtain a solution A;
2) putting the solution A into a high-temperature and high-pressure sterilizer, placing the sterilizer in an oven, preserving heat at 180 ℃ for 24 hours, cooling to room temperature, taking out a product, and evaporating the obtained solution to dryness at 115 ℃ to remove water to obtain a product B;
3) placing the product B in a magnetic boat, and placing in a tube furnace from room temperature at 10 deg.C for min-1Heating to 600 ℃ at a heating rate, calcining for 3h, cooling to room temperature along with the furnace, cleaning with deionized water and ethanol, and drying to obtain a product C;
4) mixing the raw materials in a ratio of 1: 5, uniformly mixing and grinding the product C and ammonium molybdate to obtain a preform D;
5) according to the following steps of 1: 2.5 taking the powder of the prefabricated body D and the powder of the prefabricated body S according to the mass ratio, grinding the powder evenly, placing the powder in a porcelain boat, and carrying out the treatment at the temperature of 10 ℃ for min under the condition of argon-1Is heated from room temperature to 600 ℃ for 2h to obtain a product E, wherein the argon flow is switched off when the temperature is raised to 150 ℃, so thatKeeping the high-concentration S steam to fully react with the preform D;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
As can be seen from FIG. 1, each diffraction peak in the XRD diffraction pattern of the composite material prepared by the invention can be matched with MoO2And MoS2The diffraction peaks of the standard card corresponded, indicating better crystallinity and higher purity.
From the micro-topography of FIG. 2, it can be seen that the particle size of the composite material prepared by the present invention is nano-scale, and MoS with uniform size is distributed on the surface of the particle2Nanosheets.
It can be seen from fig. 3 that the composite material prepared by the invention has excellent cycle stability and specific discharge capacity when being used for the lithium ion battery cathode electrode. At 100mA g-1The capacity is kept at 1000mAh g after 300 cycles under the current density of (1)-1The above.
Example 4:
1) dissolving 0.5g of KOH in 50ml of deionized water, adding 1g of apple pomace in a stainless steel reaction inner kettle, and mixing to obtain a solution A;
2) putting the solution A into a high-temperature high-pressure sterilizer, placing the sterilizer in an oven, preserving heat at 180 ℃ for 24 hours, cooling to room temperature, taking out a product, and evaporating the obtained solution to dryness at 105 ℃ to remove water to obtain a product B;
3) placing the product B in a magnetic boat, and placing in a tube furnace from room temperature at 10 deg.C for min-1Heating to 700 ℃ at a heating rate, calcining for 3h, cooling to room temperature along with the furnace, cleaning with deionized water and ethanol, and drying to obtain a product C;
4) mixing the raw materials in a ratio of 1: 2, uniformly mixing and grinding the product C and ammonium molybdate to obtain a preform D;
5) according to the following steps of 1: 5, grinding the powder D and S uniformly, placing the powder in a porcelain boat, and carrying out argon gas treatment at 10 ℃ for min-1The temperature rising rate is increased from room temperature to 750 ℃, and the reaction is carried out for 2 hours under the condition of heat preservation, thus obtaining a product E, wherein when the temperature rises to 150 DEG CClosing the argon flow so as to keep the high-concentration S steam and the preform D fully reacted;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
Example 5:
1) dissolving 0.1 g and 0.8g of KOH in 50ml of deionized water, adding 0.8g of apple pomace into a stainless steel reaction inner kettle, and mixing to obtain a solution A;
2) putting the solution A into a high-temperature high-pressure sterilizer, placing the sterilizer in an oven, preserving heat at 200 ℃ for 22h, cooling to room temperature, taking out a product, and evaporating the obtained solution at 110 ℃ to remove water to obtain a product B;
3) placing the product B in a magnetic boat, and placing in a tube furnace from room temperature at 8 deg.C for min-1The temperature is raised to 650 ℃ at the temperature raising rate, the mixture is calcined for 2.5h, the mixture is cooled to room temperature along with the furnace, and the product C is obtained after the mixture is cleaned by deionized water and ethanol and then dried;
4) mixing the raw materials in a ratio of 1: taking the product C and ammonium molybdate according to the mass ratio of 0.1, and uniformly mixing and grinding to obtain a preform D;
5) according to the following steps of 1: taking the powder D and S of the preform in a mass ratio of 0.5, grinding uniformly, placing in a porcelain boat, and carrying out argon gas treatment at 6 ℃ for min-1The temperature rising rate is increased from room temperature to 730 ℃, the reaction is carried out for 0.5h under the condition of heat preservation, and a product E is obtained, wherein when the temperature rises to 150 ℃, the argon flow is closed, so that the high-concentration S steam and the preform D are kept to fully react;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
Example 6:
1) dissolving 0.8g of KOH in 50ml of deionized water, adding 1.2g of apple pomace in a stainless steel reaction inner kettle, and mixing to obtain a solution A;
2) putting the solution A into a high-temperature and high-pressure sterilizer, placing the sterilizer in an oven, preserving heat at 190 ℃ for 26 hours, cooling to room temperature, taking out a product, and evaporating the obtained solution to dryness at 115 ℃ to remove water to obtain a product B;
3) placing the product B in a magnetic boat, and placing in a tube furnace from room temperature at 6 deg.C for min-1The temperature rising rate is increased to 550 ℃, the mixture is calcined for 2.5h, the mixture is cooled to room temperature along with the furnace, and the product C is obtained after the mixture is cleaned by deionized water and ethanol and then dried;
4) mixing the raw materials in a ratio of 1: 10, uniformly mixing and grinding the product C and ammonium molybdate to obtain a preform D;
5) according to the following steps of 1: 10, grinding the powder D and S uniformly, placing the powder in a porcelain boat, and carrying out argon gas treatment at 8 ℃ for min-1The temperature rising rate is increased from room temperature to 650 ℃, the reaction is carried out for 1h, and a product E is obtained, wherein when the temperature rises to 150 ℃, the argon flow is closed, so that the high-concentration S steam and the preform D are kept to fully react;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
Claims (2)
1. MoS2/MoO2The preparation method of the three-dimensional carbon lithium ion battery cathode material is characterized by comprising the following steps of:
1) dissolving 0.1-1 g of KOH in 50ml of deionized water, and then adding 0.5-1.5 g of apple pomace into the deionized water to mix to obtain a solution A;
2) putting the solution A into a high-temperature and high-pressure sterilizer, placing the sterilizer in an oven, preserving heat at 180-210 ℃ for 18-26 h, cooling to room temperature, taking out a product, and evaporating the obtained solution to dryness at 100-115 ℃ to remove water to obtain a product B;
3) putting the product B into a magnetic boat, and putting the magnetic boat into a tube furnace from room temperature for 5-10 ℃ min-1Heating to 500-700 ℃ at a heating rate, calcining for 2-3 h, cooling to room temperature along with the furnace, cleaning with deionized water and ethanol, and drying to obtain a product C;
4) mixing the raw materials in a ratio of 1: (0.1-10) taking the product C and ammonium molybdate according to the mass ratio, and uniformly mixing and grinding to obtain a preform D;
5) according to the following steps of 1: (0.5-10), uniformly grinding the prefabricated body D and the powder S, placing the ground prefabricated body D and the powder S in a porcelain boat, and placing the ground prefabricated body D and the powder S in 5 percent by mass under the argon condition～10℃min-1The temperature rising rate is increased from room temperature to 600-750 ℃, the reaction is carried out for 0.5-2 h in a heat preservation way, and when the temperature rises to 150 ℃, the argon flow is closed, so that a product E is obtained;
6) washing the product E with deionized water and ethanol for multiple times and vacuum drying at 70 ℃ to obtain MoS with three-dimensional carbon support2/MoO2A lithium ion battery cathode material.
2. The MoS of claim 12/MoO2The preparation method of the three-dimensional carbon lithium ion battery cathode material is characterized by comprising the following steps: the reaction vessel in the step 1) is a stainless steel reaction inner kettle.
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