CN111755672B - Molybdenum disulfide coated molybdenum dioxide negative electrode material and preparation method and application thereof - Google Patents
Molybdenum disulfide coated molybdenum dioxide negative electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a molybdenum disulfide-coated molybdenum dioxide negative electrode material; belongs to the technical field of preparation of lithium ion battery cathode materials. The method comprises the step of roasting the superfine molybdenum precursor in sulfur dioxide atmosphere to obtain the molybdenum dioxide material with the surface layer uniformly wrapped with the molybdenum disulfide nano layer in one step. The material is used as a lithium ion battery cathode, and not only has high specific capacity, but also has good cycling stability and rate capability. The synthesis method is simple and effective, and the prepared material has excellent performance and wide application prospect.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery cathode materials, and particularly relates to a molybdenum disulfide coated molybdenum dioxide cathode material, and preparation and application thereof.
Background
Lithium ion batteries are widely used in electric vehicles and portable electronic devices, including mobile phones, notebook computers, video cameras, and the like. Due to the low theoretical specific capacity (372mAh/g) of the commercial graphite negative electrode, the increasing requirements of human beings are difficult to meet, and the high specific capacity negative electrode material becomes a hot point of research. Among a plurality of novel anode materials, molybdenum dioxide has wide sources and higher theoretical specific capacity (838mAh/g), and is considered as an ideal substitute of a graphite anode material. However, the direct use of molybdenum dioxide as the negative electrode of the lithium ion battery has the problems of poor cycle stability, poor rate performance and the like. In order to solve the problem, a plurality of researches propose that the structural stability of the material is improved by constructing the material combining molybdenum dioxide with nano carbon, molybdenum carbide, molybdenum disulfide and the like. Among them, molybdenum disulfide is also an excellent lithium storage material, and the theoretical specific capacity of the molybdenum disulfide reaches 670 mAh/g. Therefore, the molybdenum dioxide-molybdenum disulfide heterostructure is constructed, and the electrochemical performance of the material can be further optimized by utilizing the synergistic effect of the molybdenum dioxide and the molybdenum disulfide heterostructure.
The molybdenum dioxide-molybdenum disulfide composite material can be prepared by a one-pot method (Liu H2/MoS2/Heteroatom-Doped Carbon Hybrid Materials for High-Performance Lithium-Ion Storage[J]Chemelecrochem, 2016,3(6): 922-932). Firstly, carrying out hydro-thermal treatment on an organic vulcanizing agent, an organic solvent and a molybdenum raw material under the conditions of high temperature and high pressure to obtain a uniformly dispersed molybdenum-sulfur composite precursor, and then roasting and reducing to obtain MoO2And MoS2A composite material. The method is fine in operation, and the prepared product is good in uniformity, but has the problems of complex working procedures, low efficiency, difficulty in equipment expansion and the like.
In addition, sulfur powder sulfiding roasting is also a common practice (Xu Z, Wang H, Li Z, et al2Distribution Enabling Improved Lithium Ion Battery Performance[J].The Journal of Physical Chemistry C,2014,118(32):18387-18396；Xu Z,Wang T,Kong L,et al.MoO2@MoS2Nanoarchitectures for High-Loading Advanced Lithium-Ion Battery Anodes[J].Particle&Particle Systems Characterization,2017,34(3): 1600223). High-temperature sulfur steam pair MoO generation by adopting sulfur3(CN106410150A) or MoO2(CN105514403A) sulfurizing and reducing to obtain MoS etched on the surface2MoO of a layer2A material. However, this type of process has inherent disadvantages in itself: good air permeability in the molybdenum trioxide or molybdenum dioxide material layerThere will be excess sulfur vapor passing through, resulting in overcuring; and less sulfur vapor passes through the part with poor air permeability of the material layer, resulting in MoS2And is rarely produced. Therefore, when the molybdenum disulfide-coated molybdenum dioxide material is prepared by directly adding sulfur powder, the degree of sulfuration etching is difficult to control, the sulfuration uniformity of the synthesized material is poor, and finally, the electrical properties of the obtained material, such as specific capacity and long-term cycle performance, are poor.
Disclosure of Invention
In order to solve the technical problems of difficult control of the sulfurization etching degree, poor sulfurization uniformity, non-ideal electrical properties of the material and the like in the existing preparation method, the first aim of the invention is to provide a preparation method of a molybdenum disulfide coated molybdenum dioxide cathode material, aiming at preparing the cathode material with excellent electrical properties through a brand new preparation mechanism.
The second purpose of the invention is to provide the molybdenum disulfide-coated molybdenum dioxide negative electrode material prepared by the preparation method.
The third purpose of the invention is to provide the application of the molybdenum disulfide coated molybdenum dioxide negative electrode material prepared by the preparation method.
A preparation method of a molybdenum disulfide coated molybdenum dioxide anode material (the molybdenum disulfide coated molybdenum dioxide anode material or the anode material for short) comprises the step of roasting metal molybdenum powder at the temperature of 600-750 ℃ in an atmosphere containing sulfur dioxide to prepare the molybdenum disulfide coated molybdenum dioxide anode material.
The invention provides a brand new mechanism for constructing a molybdenum disulfide-coated molybdenum dioxide negative electrode material in situ by one step; namely, the molybdenum oxidation and the vulcanization are carried out synchronously through the reaction of the metal molybdenum powder and the sulfur dioxide innovatively, so that the molybdenum disulfide is formed on the surface of the molybdenum dioxide in one step and in situ.
The total reaction formula of the brand new preparation mechanism is as follows: 3Mo +2SO2(g)＝MoS2+2MoO2. The invention adopts a brand new preparation mechanism, and can effectively overcome the problems of difficult control of etching degree and uneven vulcanization existing in the existing preparation methodTo give a title. The material prepared by the brand-new preparation mechanism has better electrical properties, such as higher initial specific capacity and long-term cycling stability.
The research of the invention also finds that under the innovative preparation mechanism, the shape and the particle size of the metal molybdenum precursor in the preparation process, the temperature in the roasting process, the temperature rise mechanism and other parameters are further controlled, so that the advantages of the innovative preparation mechanism can be more exerted, and the specific capacity and the rate capability of the prepared cathode material are improved.
The method has no special requirement on the shape of the metal molybdenum precursor, but the performance of the molybdenum disulfide coated molybdenum dioxide cathode material synthesized by taking the nano metal molybdenum as the precursor is better.
Preferably, the method comprises the following steps: the metal molybdenum precursor has at least one dimension less than 100 nm.
Preferably, the method comprises the following steps: the metal molybdenum powder is obtained by the following method: calcination of MoO under inert atmosphere3Obtaining 0.01-0.05g/L molybdenum oxide vapor, introducing the molybdenum oxide vapor into a roasting chamber at 1100-1300 ℃, and then blowing H according to 0.002-0.02g/L2Mixing and reacting for 3-8 seconds, leading out the gas-solid mixture, cooling and separating a solid product to obtain the molybdenum powder.
The nanometer molybdenum prepared by the specific method has good crystal growth due to high-temperature roasting treatment at the temperature of more than or equal to 1100 ℃, and the prepared molybdenum powder has certain surface inertia, so that the phenomena of particle expansion and agglomeration are greatly relieved when the molybdenum powder is roasted in the subsequent sulfur dioxide atmosphere.
The research of the invention also finds that the control of the temperature rise mechanism of the roasted metal molybdenum precursor is beneficial to further improving the electrical property of the prepared cathode material.
Preferably, the temperature is raised from room temperature to 450-500 ℃, and then raised to the roasting temperature at a heating rate of 2-5 ℃/min. The heating rate of heating from room temperature to 450-500 ℃ is 2-20 ℃/min. The research finds thatUnder the heating mechanism, the material has small granularity expansion and MoO2Surface MoS formation2The thickness is uniform, so that the performance of the prepared material can be further improved.
The inventor researches and discovers that the electrical property of the prepared cathode material can be improved by controlling the roasting temperature in a required range under the innovative preparation mechanism of the invention, and researches and discovers that the temperature higher than the range can cause the material to remarkably expand in granularity, agglomerate in particles and remarkably reduce the specific surface area.
Preferably, the calcination temperature is 650-700 ℃.
Preferably, the calcination time is 30 to 120 min.
Preferably, the sulfur dioxide-containing atmosphere is pure sulfur dioxide gas or mixed gas of sulfur dioxide and protective atmosphere; further preferred is a mixed gas of sulfur dioxide and a protective atmosphere. And under the preferable mixed atmosphere, the prepared negative electrode material has better consistency.
The protective atmosphere is nitrogen or argon.
The invention also provides a molybdenum disulfide-coated molybdenum dioxide cathode material prepared by the preparation method, which comprises molybdenum dioxide and a molybdenum disulfide layer coated on the surface of the molybdenum dioxide in situ; the molybdenum disulfide layer is 2H phase molybdenum disulfide with the thickness of 0.6-10 nm; the molybdenum dioxide is monoclinic phase molybdenum dioxide.
The material has the microscopic characteristic of the innovative preparation mechanism, and has better electrical properties compared with the material prepared by the existing preparation method.
The invention also provides application of the molybdenum disulfide coated molybdenum dioxide cathode material as a lithium ion battery cathode material.
Advantageous effects
1. The invention provides a brand new mechanism for constructing a molybdenum disulfide coating on the surface of molybdenum dioxide in one step and in situ.
2. Compared with other preparation methods, the method does not use elemental sulfur as a vulcanizing agent, but adopts sulfur dioxide to synchronously oxidize-vulcanize the ultrafine metal molybdenum powder, and because the vulcanizing agent is generated in the oxidation process of the metal molybdenum powder and is subjected to in-situ vulcanization reduction, and the generated vulcanizing agent cannot be excessive theoretically, the problems of over-vulcanization and nonuniform vulcanization in the existing method are avoided.
3. Researches show that the material prepared by the brand-new preparation mechanism has better specific capacity, rate capability and cycling stability.
Drawings
Fig. 1 is an X-ray diffraction pattern (XRD) of the metal molybdenum powder precursor prepared in example 1.
Fig. 2 is a Transmission Electron Micrograph (TEM) of the metal molybdenum powder precursor prepared in example 1.
Fig. 3 is an X-ray diffraction pattern (XRD) of the molybdenum disulfide coated molybdenum dioxide material prepared in example 1.
Fig. 4 is a Transmission Electron Micrograph (TEM) of the molybdenum disulfide coated molybdenum dioxide material prepared in example 1.
Fig. 5 is a High Resolution Transmission Electron Micrograph (HRTEM) of the molybdenum disulfide coated molybdenum dioxide material prepared in example 1.
Fig. 6 is a constant current charge and discharge performance diagram of the molybdenum disulfide-coated molybdenum dioxide material prepared in example 1 as a negative electrode of a lithium ion battery.
Fig. 7 is a graph of rate performance of the molybdenum disulfide-coated molybdenum dioxide material prepared in example 1 as a negative electrode of a lithium ion battery.
Fig. 8 is a Transmission Electron Micrograph (TEM) of the molybdenum disulfide coated molybdenum dioxide material prepared in example 2.
Fig. 9 is a Transmission Electron Micrograph (TEM) of the molybdenum disulfide-coated molybdenum dioxide material prepared in example 3 as a negative electrode of a lithium ion battery.
Fig. 10 is a constant current charge/discharge performance diagram of the molybdenum disulfide-coated molybdenum dioxide material prepared in example 3 as a negative electrode of a lithium ion battery.
Fig. 11 is a constant current charge and discharge performance diagram of the molybdenum disulfide-coated molybdenum dioxide material prepared in comparative example 1 as a negative electrode of a lithium ion battery.
Detailed Description
The invention is further illustrated and described below with reference to examples, without the scope of the claims being limited by the examples below.
Example 1:
calcination of MoO under inert atmosphere30.03g/L of molybdenum trioxide vapor was obtained, which was introduced into a roasting chamber at 1150 ℃ and further charged with H at 0.01g/L2Mixing and reacting for 7 seconds, leading out the gas-solid mixture, cooling and separating a solid product to obtain the molybdenum powder. Loading the prepared molybdenum powder precursor into a quartz boat, placing the quartz boat in a heating zone of a tube furnace, and introducing 33% SO2And the air flow of 67 percent Ar is heated to 500 ℃ at the speed of 20 ℃/min (first heating rate), then heated to 700 ℃ (roasting temperature) at the speed of 5 ℃/min (second heating rate), heated for 60min at constant temperature, stopped heating, naturally cooled to room temperature along with the furnace and then taken out.
As can be seen from the XRD pattern shown in FIG. 1, the prepared precursor is pure phase metal molybdenum; as can be seen from the TEM image shown in FIG. 2, the synthesized molybdenum is in the shape of a bar, and at least one dimension of the synthesized molybdenum is 30-60 nm; the XRD pattern shown in FIG. 3 indicates that the synthesized material contains a large amount of molybdenum dioxide and a small amount of molybdenum disulfide; FIG. 4 shows a TEM image showing that the synthesized material particles have at least one dimension of 40-80 nm; the HRTEM of fig. 5 shows that the edges of the synthesized molybdenum dioxide particles are uniformly wrapped with a molybdenum disulfide layer of about 3 nm.
And preparing the molybdenum disulfide-coated molybdenum dioxide material into an electrode for electrochemical test. The constant-current discharge test result shown in fig. 6 shows that the discharge specific capacity of the negative electrode reaches 1068mAh/g after the negative electrode is cycled for 130 circles under the charge and discharge current of 200 mA/g; the rate performance test shown in fig. 7 shows that when the charging and discharging currents are respectively 0.5, 1 and 2A/g, the specific capacity of the negative electrode can still reach about 900, 800 and 700 mA/g. The tests show that the cathode material has high specific capacity, excellent rate capability and good cycling stability.
Example 2:
using the same metallic molybdenum precursor as in example 1, the temperature increase rate of 500 ℃ or higher was reduced to 2 ℃/min (second temperature increase rate), the baking temperature was reduced to 650 ℃, and the baking time was extended to 90 min. Because the heating rate is slowed down, the roasting temperature is reduced, the reaction rate is correspondingly slowed down, and the material can be slowly and uniformly synthesized by prolonging the roasting time.
As shown in FIG. 8, the molybdenum disulfide-coated molybdenum dioxide material prepared under the condition has at least one dimension of 30-60nm, and compared with example 1, the particle size is smaller, and the particle agglomeration phenomenon is reduced. The molybdenum disulfide-coated molybdenum dioxide material is made into an electrode for electrochemical test, and after the electrode is circulated for 130 circles under the charging and discharging current of 200mA/g, the specific capacity of the negative electrode is still stable above 1100mAh/g, and the excellent electrochemical lithium storage performance is shown.
Example 3:
a commercially available spherical metal molybdenum powder with a size of 50nm was used as a precursor to prepare a molybdenum disulfide-coated molybdenum dioxide material under the same synthesis conditions as in example 1. As shown in FIG. 9, the particle size after calcination reached more than 100nm, and the agglomeration was severe. When an electrode made of the material is used for electrochemical tests, as shown in fig. 10, after the electrode is circulated for 130 circles under the charging and discharging current of 200mA/g, the specific capacity of the negative electrode is maintained to be about 700mAh/g, and the specific capacity can still be about twice of that of a commercially available graphite negative electrode, but compared with a negative electrode material synthesized by using a metal molybdenum precursor prepared by the method, the performance of the negative electrode material is obviously reduced.
Comparative example 1:
by adopting the same metallic molybdenum precursor and temperature rising system as example 1, the roasting temperature is only raised to 800 ℃, and TEM observation of the finally obtained material shows that the particle size of the finally obtained material is obviously higher than that of examples 1 and 2, reaches 70-120nm, and the agglomeration is serious. When an electrode made of the material is used for electrochemical tests, as shown in figure 11, under the charging and discharging current of 200mA/g, the specific capacity can reach more than 750mAh/g after 30 circles, but the capacity is attenuated after 100 circles. Therefore, when the roasting temperature is higher than the required range, the prepared material can obviously slide down in the aspects of cycling stability and specific capacity performance.
Claims (9)
1. A preparation method of a molybdenum disulfide-coated molybdenum dioxide negative electrode material is characterized by comprising the following steps: roasting the metal molybdenum precursor in an atmosphere containing sulfur dioxide at the temperature of 600-750 ℃ to prepare the molybdenum disulfide-coated molybdenum dioxide anode material; the molybdenum disulfide-coated molybdenum dioxide cathode material comprises molybdenum dioxide and a molybdenum disulfide layer coated on the surface of the molybdenum dioxide in situ; the molybdenum disulfide layer is 2H phase molybdenum disulfide with the thickness of 0.6-10 nm; the molybdenum dioxide is monoclinic phase molybdenum dioxide;
the metallic molybdenum precursor is obtained by the following method: calcination of MoO under inert atmosphere3Obtaining 0.01-0.05g/L molybdenum oxide vapor, introducing the molybdenum oxide vapor into a roasting chamber at 1100-1300 ℃, and blowing H according to 0.005-0.02g/L2Mixing and reacting for 3-8 seconds, leading out the gas-solid mixture, cooling and separating a solid product to obtain the molybdenum powder.
2. The method of claim 1, wherein: the metal molybdenum precursor has at least one dimension less than 100 nm.
3. The method of claim 1, wherein: the temperature of the roasting process is 650-700 ℃.
4. The production method according to claim 1 or 3, characterized in that: after the temperature is increased from room temperature to 450-500 ℃, the temperature is increased to the roasting temperature according to the temperature increase rate of 2-20 ℃/min.
5. The method of claim 4, wherein: the heating rate of heating from room temperature to 450-500 ℃ is 2-5 ℃/min.
6. The method of claim 1, wherein: the roasting time is 30-120 min.
7. The method of claim 1, wherein: the atmosphere containing sulfur dioxide is pure sulfur dioxide gas or mixed gas of sulfur dioxide and protective atmosphere.
8. The molybdenum disulfide-coated molybdenum dioxide negative electrode material prepared by the preparation method of any one of claims 1 to 7 is characterized in that: comprises molybdenum dioxide and a molybdenum disulfide layer coated on the surface of the molybdenum dioxide in situ; the molybdenum disulfide layer is 2H phase molybdenum disulfide with the thickness of 0.6-10 nm; the molybdenum dioxide is monoclinic phase molybdenum dioxide.
9. The use of the molybdenum disulfide coated molybdenum dioxide negative electrode material of claim 8 as a negative electrode material for a lithium ion battery.
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