CN109950509B - MoO (MoO)2/MoS2Composite electrode material and preparation method thereof - Google Patents
MoO (MoO)2/MoS2Composite electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a MoO2/MoS2A composite electrode material and a preparation method thereof. The preparation method comprises the following steps: s1, mixing ammonium molybdate powder and oxalic acid powder, calcining the uniformly mixed solid powder, and cooling to obtain MoO3A precursor; s2, mixing the MoO3Uniformly mixing the precursor and sulfur powder, then placing the uniformly mixed solid powder into a closed reaction kettle, reacting for 0.5-100h at 170-230 ℃, and cooling after the reaction is finished; wherein, the MoO3The weight ratio of the precursor to the sulfur powder is 1: 0.5-5; s3, heating the reaction product cooled in the step S2 to 500-2/MoO2A composite material. The method is simple to operate, safe and reliable, is beneficial to industrial production, and the content of each component in the composite material is controllable.
Description
Technical Field
The invention belongs to the field of batteries, and particularly relates to a MoO2/MoS2A composite electrode material and a preparation method thereof.
Background
With the rapid development of various electric vehicles, the demand for high-capacity and high-energy electrode materials for batteries has increased dramatically. Molybdenum dioxide (MoO)2) Due to high specific capacity (880mAh g)-1) Low cost, low toxicity, natural and rich, and has attracted wide attention in the fields of lithium ion batteries and SCs. However, MoO2The severe volume change in the charge and discharge process causes the poor cycle stability and high rate performance, and the practical application of the material is influenced. Literature reports MoO prepared by a two-step process2/Au/MnO2The composite structure showed excellent electrochemical performance (X.Zhang, Y.Xu, Y.Ma, M.Yang, Y.Qi, A hierarchical MoO)2/Au/MnO2A chemostructure with enhanced electrochemical performance for application as supercapacitors, Eur.J.Inorg.chem.2015(2015) 3764-3768). The composite material exhibits superior electrochemical performance compared to a single compound. Thus, MoO2With other electrical activityThe compounding of materials to improve their properties has become a research hotspot. Among these Mo-based compounds, MoS2Since higher ionic conductivity (above oxides) and higher theoretical capacity (above graphite) are better choices.
At present, MoO2/MoS2There are three main methods for the synthesis of composite materials. One is the conventional hydrothermal process. The hydrothermal method mainly uses molybdenum salt or molybdenum oxide as a molybdenum source, the molybdenum source and various sulfur sources are dissolved in water or an organic solvent, some auxiliary reagents are added, certain acidity and alkalinity are controlled, and the target product is synthesized by reaction in a sealed container at about 200 ℃. The method has simple and controllable process and uniform product appearance, and is the MoO synthesized at present2/MoS2The main method of the composite material, but the solvent consumption is large, the wastewater treatment cost is high, and the large-scale production of the composite material is limited.
The second is an in situ growth method. CN106410150A discloses MoO3The precursor and the S powder are mixed according to the weight ratio of 0.5: (1.0-5.0), uniformly grinding, heating from room temperature to 400-600 ℃ under an inert condition, carrying out heat preservation reaction for 0.5-2 h, then continuously heating to 600-800 ℃, carrying out heat preservation reaction for 0.5-2 h, cooling to room temperature, washing and drying a reaction product, and thus obtaining the MoO with the core-shell structure2-MoS2The negative electrode material of the sodium ion battery. CN105514403B and CN103367713A disclose similar methods, MoO3And (3) blending the precursor and S powder, and then calcining at high temperature. The method is simple and feasible, and is suitable for small-batch production. However, the composition of the composite material of the synthesis product is greatly affected by the gas flow rate, the calcination temperature and the precursor ratio. The flow rate is high, and the temperature is high, so that a large amount of sulfur is evaporated and lost. In order to increase the content of molybdenum sulfide in the compound, the dosage of S powder, S powder and MoO needs to be increased3The mass ratio of the precursor is as high as 5:0.5, namely the molar ratio is as high as 40:1, if the large-scale production is carried out, a large amount of excess sulfur vapor is subjected to cold deposition in a tubular furnace, so that a gas passage is easily blocked, and the safety problem is caused.
The third method is a vapor deposition method. CN109207957A discloses S and MoO in solid state3Putting sulfur powder in a low-temperature region of a tube furnace to be evaporated into steam as a precursor, and putting molybdenum dioxide in the tube furnaceEvaporating into vapor in a high-temperature area, making the two vapors meet under the drive of carrier gas, and synthesizing MoS on a target substrate after chemical vapor reaction2/MoO2Wherein the concentration of S steam in the tubular furnace temperature zone can be adjusted through the magnitude of the carrier gas flow. The method utilizes gas phase reaction, the reaction is more thorough, and the method is more favorable for preparing pure phase MoS2Obtaining pure MoS by this method is disclosed in CN106757361A2. However, this method requires a higher reaction temperature, up to 800 ℃ or higher, sulfur vapor is much more excessive, and S and MoO3The mass ratio of the powder is as high as 100:3, and the method also has the safety problem caused by sulfur vapor blocking the instrument. Instead of sulfur powder, the method of introducing hydrogen sulfide gas (1.Dingbin Xiao, Jinying Zhuang, Xin Li, Dan Zhuao, Hongyang Huang, Jianliang Huang, Daxian Cao, Zhuhui Li, and Chunning Niu, ACS Nano 2016,10, 9509-9515.2. Prabhat Kumar, Megha Singh, Rabindar K. Sharma, G.B. Reddy, Materials Chemistry and Physics 178(2016)6e11) is not suitable for popularization because of its strong toxicity.
Disclosure of Invention
The invention aims to provide an improved MoO (MoO) aiming at the problems of complex process, poor controllability and safety of composite material content and the like in the prior art2/MoS2The preparation method of the composite electrode material is simple to operate, safe and reliable, is beneficial to industrial production, and has controllable content of each component in the composite material.
In order to achieve the above object, a first aspect of the present invention provides a MoO2/MoS2The preparation method of the composite electrode material comprises the following steps:
s1, mixing ammonium molybdate powder and oxalic acid powder, calcining the uniformly mixed solid powder, and cooling to obtain MoO3A precursor;
s2, mixing the MoO3Uniformly mixing the precursor and sulfur powder, then placing the uniformly mixed solid powder into a closed reaction kettle, reacting for 0.5-100h at 170-230 ℃, and cooling after the reaction is finished; wherein, the MoO3The weight ratio of the precursor to the sulfur powder is 1: 0.5-5;
s3, heating the reaction product cooled in the step S2 to 500-2/MoO2A composite material.
The technical key points of the invention are as follows: using a sealed hydrothermal reaction kettle as a reactor to react MoO3The precursor is mixed with sulfur powder to change the sulfur powder into sulfur vapor at certain temperature, and the vapor generates certain pressure in a sealed container to promote the sulfurization reaction of oxide.
By controlling the sulfur powder and the MoO3The proportion between the precursors, the temperature and the time of the vulcanization reaction to realize the MoO2/MoS2The controllability of the composition of the composite material can obtain the required composite material. MoO prepared by the method2/MoS2The lithium ion battery cathode material has higher specific discharge capacity and better cycling stability.
Further, in step S1, the calcining conditions include: the temperature is 450 ℃ and 550 ℃ and the time is 1-4 hours.
According to the present invention, in step S1, the amounts of ammonium molybdate and oxalic acid may be determined as required, and preferably, the molar ratio of ammonium molybdate to oxalic acid is 1: 2-4.
According to the present invention, in step S2, the reaction time is preferably 1 to 60 hours, and more preferably 4 to 48 hours.
Further, in step S2, the MoO3The weight ratio of the precursor to the sulfur powder is 1: 1-3.
By further controlling the sulfur powder and the MoO3The proportion of the precursors, the temperature and the time of the vulcanization reaction can obtain MoO with more excellent performance2/MoS2A composite electrode material.
According to the present invention, in step S2, the closed reaction kettle may be a conventional hydrothermal reaction kettle, such as a hydrothermal reaction kettle with a teflon liner.
According to the present invention, in step S3, the temperature is preferably increased at a relatively slow rate, and particularly preferably at a rate of 3 to 8 ℃/min.
In the present invention, the cooling is preferably performed in a natural cooling manner in all of the three steps, and, specifically,
in step S1, calcining, and naturally cooling to room temperature to obtain MoO3A precursor;
in step S2, after the reaction is finished, the reaction product is naturally cooled to room temperature;
and in the step S3, after heat preservation, cooling to room temperature along with the furnace.
According to the present invention, the method of uniformly mixing the solid powder in steps S1 and S2 may employ various methods that are conventional in the art, such as a milling method.
According to a specific embodiment of the present invention, the preparation method comprises the steps of:
first, the precursor MoO3The synthesis of (2): weighing a certain amount of ammonium molybdate tetrahydrate and oxalic acid, grinding the ammonium molybdate tetrahydrate and the oxalic acid into powder by using a mortar respectively, and then mixing and grinding the ammonium molybdate tetrahydrate and the oxalic acid together to fully mix the two solid powders. Then placing the uniformly mixed solid powder in a crucible, calcining for 2 hours in a muffle furnace at 500 ℃, naturally cooling to room temperature, and taking out to obtain MoO3And (3) precursor.
Second, MoO of different composition2/MoS2Synthesis of the composite material: weighing a certain amount of sulfur powder and the synthetic MoO3Grinding the mixture in a mortar to uniformly mix the two solid powders, transferring the mixed solid powder into a polytetrafluoroethylene inner village high-temperature reaction kettle, reacting for a period of time at 180-220 ℃ in a blast drying oven, and naturally cooling to room temperature after the reaction is finished to obtain MoO2/MoS2And (3) obtaining the product.
Thirdly, in order to improve the crystallinity of the product, the synthesized product is heated to 700-800 ℃ at the heating rate of 5 ℃/min and is kept for 2h in the tube furnace under the protection of argon, and then the temperature is reduced to room temperature to obtain MoS2/MoO2A composite material.
The second aspect of the present invention provides MoO prepared by the above preparation method2/MoS2A composite electrode material.
The invention has the beneficial technical effects that:
the method of the invention uses sulfur powder and MoO3Is a precursor and is sealed by a hydrothermal kettle for reaction to synthesize MoO2/MoS2A composite material. The method has simple process and safe operation, is suitable for industrial production, and has controllable material composition. The crystallinity of the product can be further improved by carrying out the heat-insulating treatment at a high temperature.
The composite material synthesized by the invention can be used as a lithium ion battery cathode material, and the electrochemical performance and MoS in the composite thereof2The content of (A) is related, the content is too low, the conductivity of the composite material is poor, and the discharge capacity is low; too high a content in MoO2The surface arrangement type is changed, so that the surface property of the composite material is changed, and therefore, by adopting the preparation method disclosed by the invention, the components of the composite material are regulated and controlled, the coordination effect among different components in the composite material is fully utilized, and the lithium ion battery cathode material with excellent performance can be obtained.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings.
FIG. 1 shows MoO's obtained in examples 1 to 4 of the present invention2-MoS2XRD pattern of the product.
FIGS. 2A-2D are MoO's prepared according to examples 1-4, respectively, of the present invention2-MoS2SEM image of the product.
FIG. 3 shows MoO obtained in examples 1 to 4 of the present invention2-MoS2Impedance plot of the product.
FIG. 4 shows MoO's obtained in examples 1-4 of the present invention2-MoS2And (3) an electrochemical cycle performance diagram of the product.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
Example 1
This example serves to illustrate the MoO of the invention2/MoS2The preparation method comprises the following steps:
(1) 0.01mol of ammonium molybdate tetrahydrate (1.7654g) and 0.03mol of oxalic acid (3.78g) were weighed using a scale and ground in a mortar to mix the two solid powders thoroughly. Then placing the mixed solid powder in a muffle furnace to be calcined for 2 hours at 500 ℃, then cooling to room temperature and taking out to obtain MoO3And (3) precursor.
(2) 0.5g of the MoO was weighed3Fully mixing the precursor and 1g of sulfur powder, then transferring the two powders into a 50mL polytetrafluoroethylene inner village high-temperature reaction kettle, reacting for 4 hours at 220 ℃ in a blast drying oven, then naturally cooling to room temperature, finally heating the obtained powder to 800 ℃ at the heating rate of 5 ℃/min in a tubular furnace under the protection of argon gas, keeping the temperature for 2 hours, cooling to room temperature along with the furnace to obtain MoS2/MoO2A composite material.
Example 2
This example serves to illustrate the MoO of the invention2/MoS2The preparation method comprises the following steps:
(1) the experimental procedure was exactly the same as in example 1, step (1).
(2) 0.5g of the MoO was weighed3Fully grinding the precursor and 0.8g of sulfur powder in a mortar, transferring the mixed solid powder into a 50mL polytetrafluoroethylene Namura high-temperature reaction kettle, sealing and reacting for 8 hours at 220 ℃ to obtain MoO2/MoS2Finally, raising the temperature to 750 ℃ at the temperature rise rate of 5 ℃/min in a tubular furnace under the argon protection environment, preserving the heat for 2h, and cooling to room temperature along with the furnace to obtain MoS2/MoO2A composite material.
Example 3
This example serves to illustrate the MoO of the invention2/MoS2The preparation method comprises the following steps:
(1) the experimental procedure was exactly the same as in example 1, step (1).
(2) 0.5g of the MoO was weighed3Fully mixing the precursor and 0.6g of sulfur powder in a mortar, then transferring the mixed solid powder into a polytetrafluoroethylene inner-village high-temperature reaction kettle, reacting for 24 hours at 200 ℃, naturally cooling to room temperature after the reaction is finished to obtain a primary product, finally heating the primary product to 700 ℃ at the heating rate of 5 ℃/min under the protection of argon in a tubular furnace, keeping the temperature for 2 hours, and turning to the room temperature along with the furnace to obtain MoS2/MoO2A composite material.
Example 4
This example serves to illustrate the MoO of the invention2/MoS2The preparation method comprises the following steps:
(1) the experimental procedure was exactly the same as in example 1, step (1).
(2) 0.5g of the MoO was weighed3Grinding the precursor and 0.5g of sulfur powder in a mortar to uniformly mix the two solid powders, transferring the mixed solid powder into a reaction kettle, reacting for 48 hours at 200 ℃, naturally cooling after the reaction is finished, heating the cooled solid powder to 700 ℃ under the protection of argon in a tubular furnace, preserving the heat for 2 hours, cooling to room temperature along with the furnace to obtain MoS2/MoO2A composite material.
Test example 1
FIG. 1 shows the synthesis of MoS at different sealing reaction times for examples 1-42/MoO2XRD pattern of composite material, as can be seen from FIG. 1, MoS synthesized by hydrothermal kettle sealing reaction for 4 hours2/MoO2In the composite material, MoO2The characteristic peaks all have higher intensity, and MoS2The characteristic peak of (a) is relatively weak; MoO in composite with extended sealing reaction time2The intensity of the characteristic peak gradually decreases, and MoS2The diffraction peak intensity gradually increases. From this, the MoS in the composite can be deduced2The content increases with the duration of the sealing reaction.
Test example 2
FIGS. 2A-D show the sequential synthesis of MoS for different seal reaction times of examples 1-42/MoO2Scanning electron microscope imageIt can be seen that the appearance of the synthesized sample is not greatly different. The main reason for the differences in composite properties is not due to morphology.
Test example 3
FIG. 3 shows the synthesis of MoS under different sealing time conditions of examples 1-42/MoO2The ac impedance profile of the composite. As can be seen from fig. 3, the radius of the sample is the smallest after 8 hours of the sealing reaction, indicating that the charge transfer resistance is the smallest, indicating that the sample has better electrochemical performance after 8 hours of the sealing reaction.
Test example 4
FIG. 4 shows the MoS synthesized for examples 1-4 at different seal reaction times2/MoO2Cycling performance curves of the composite at a current density of 100mA/g for 50 weeks. As can be seen from the discharge curve in FIG. 4, the discharge specific capacities of the samples after sealing reaction for 4h, 8h, 24h and 48h are 573.1mAh/g, 824.8mAh/g, 574.2mAh/g and 411mAh/g in sequence after 50-week circulation, and the charge-discharge cycle performance of the sample after sealing reaction for 8h is the best.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (7)
1. MoO (MoO)2/MoS2The preparation method of the composite electrode material is characterized by comprising the following steps of:
s1, mixing ammonium molybdate powder and oxalic acid powder, calcining the uniformly mixed solid powder, and cooling to obtain MoO3A precursor;
s2, mixing the MoO3Uniformly mixing the precursor and sulfur powder, then placing the uniformly mixed solid powder into a closed reaction kettle, reacting for 4-48h at 170-230 ℃, and cooling after the reaction is finished; wherein, the MoO3The weight ratio of the precursor to the sulfur powder is 1: 1-3; the closed reaction kettle is provided with a polytetrafluoroethylene liningThe hydrothermal reaction kettle;
s3, heating the reaction product cooled in the step S2 to 500-2/MoO2A composite material.
2. The MoO of claim 12/MoS2A method for producing a composite electrode material, wherein in step S1, the calcination conditions include: the temperature is 450 ℃ and 550 ℃ and the time is 1-4 hours.
3. The MoO of claim 12/MoS2The preparation method of the composite electrode material is characterized in that in step S1, the molar ratio of ammonium molybdate to oxalic acid is 1: 2-4.
4. The MoO of claim 12/MoS2The preparation method of the composite electrode material is characterized in that in step S3, the temperature rise rate is 3-8 ℃/min.
5. The MoO of claim 12/MoS2The preparation method of the composite electrode material is characterized in that,
in step S1, calcining, and naturally cooling to room temperature to obtain MoO3A precursor;
in step S2, after the reaction is finished, the reaction product is naturally cooled to room temperature;
and in the step S3, after heat preservation, cooling to room temperature along with the furnace.
6. The MoO of claim 12/MoS2The method for producing the composite electrode material is characterized in that in steps S1 and S2, the method for uniformly mixing the solid powder is a grinding method.
7. MoO produced by the production method according to any one of claims 1 to 62/MoS2A composite electrode material.
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Effective date of registration: 20221014 Address after: 230000 B-2704, wo Yuan Garden, 81 Ganquan Road, Shushan District, Hefei, Anhui. Patentee after: HEFEI LONGZHI ELECTROMECHANICAL TECHNOLOGY Co.,Ltd. Address before: 430023 No. 68 Xuefu South Road, Changqing Garden, Hankou, Wuhan, Hubei. Patentee before: WUHAN POLYTECHNIC University |