CN108899514B - Three-dimensional porous MoS2rGO nano material and preparation method and application thereof - Google Patents

Three-dimensional porous MoS2rGO nano material and preparation method and application thereof Download PDF

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CN108899514B
CN108899514B CN201810718112.9A CN201810718112A CN108899514B CN 108899514 B CN108899514 B CN 108899514B CN 201810718112 A CN201810718112 A CN 201810718112A CN 108899514 B CN108899514 B CN 108899514B
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CN108899514A (en
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许占位
王天
赵怡星
关伟伟
曹丽云
黄剑锋
沈学涛
冯兰
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Shaanxi Coal And Chemical Technology Research Institute Co Ltd
Shaanxi University of Science and Technology
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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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • 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 three-dimensional porous MoS2A/rGO nano material and a preparation method and application thereof belong to the technical field of preparation of sodium ion battery electrode materials. In-situ synthesis of three-dimensional porous nano-structure MoS by using solid phase method in preparation process2a/rGO nanomaterial. Compared with most of methods reported in literature, such as a hydrothermal method or a method of hydrothermal treatment and heat treatment, the method has the characteristics of simple process, easy control of reaction, high repeatability, high yield and the like. H is realized by controlling the volume flow of argon gas on the basis2CNSNH2The gas generated by decomposition can reduce MoO3But also can satisfy the pore-forming effect. Experimental results show that the three-dimensional porous nano-structure MoS prepared by the method of the invention2the/rGO shows excellent conductivity, cycling stability and high specific discharge capacity, and can be widely used as a negative electrode material of a sodium ion battery.

Description

Three-dimensional porous MoS2rGO nano material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of preparation of electrode materials of sodium-ion batteries, and particularly relates to a three-dimensional porous MoS2a/rGO nano material and a preparation method and application thereof.
Background
With the rapid development of the markets of electric automobiles and mobile electronic devices, the requirements on battery materials are higher and higher. Finding suitable battery materials has a great impact on the functionality of electronic devices. The lithium ion battery mainly comprises a positive electrode, a negative electrode and an electrolyte. The anode and the cathode are basic materials for electrochemical reaction, which are the basis for converting chemical energy into electric energy, and the electrolyte is a carrier for ion transmission in the battery. However, the scarcity of lithium resources limits further development. Sodium ion batteries have the characteristics of high energy density, long service life, environmental friendliness and the like, and are considered to be the most likely system for energy storage. Sodium ion battery materials are widely researched as one of the branches of new energy materials
Molybdenum disulfide (MoS)2) Its theoretical capacity is up to 670mAh g-1And is expected to become the cathode material of the next generation sodium ion battery. MoS2The sandwich layer structure with S-Mo-S has the advantages that atoms in the layers are combined through strong covalent bonds, and weak van der Waals force action exists between the layers. However, when the material is used as a negative electrode material of a sodium ion battery, the MoS with high surface energy is caused by the intercalation and deintercalation of ions in the charge and discharge processes, particularly the deintercalation process of sodium ions2The laminated structure collapses and stacks, the multiplying power performance and the circulation stability of the laminated structure are reduced, the electronic/ionic conductivity between the S-Mo-S laminated layers is further influenced, and the electrochemical performance of the laminated structure is reduced.
Disclosure of Invention
The invention aims to provide a three-dimensional porous MoS2The preparation method has the advantages of simple preparation process, easy control of reaction, short reaction period, low energy consumption, high repeatability and high yield, and is suitable for large-scale production; MoS prepared by the method2The composite powder has high purity, porous structure and homogeneous particle size, and may be used as the negative pole material of secondary sodium ion battery.
The invention is realized by the following technical scheme:
the invention discloses a three-dimensional porous MoS2Preparation method of/rGO nano materialThe method comprises the following steps:
1) dispersing graphene in water, and then adding H2CNSNH2Fully and uniformly stirring to prepare a solution A; wherein the graphene and H are used2CNSNH2The mass ratio of (0.04-0.12): (1.0-3.0);
2) adding MoO3Adding the mixture into the solution A, and heating and evaporating while stirring to obtain a prefabricated body;
3) heating the prefabricated body from room temperature to 600-800 ℃ in an argon atmosphere, preserving heat for 2.0-4.0 h, and cooling to room temperature;
4) washing and drying the cooled product to obtain the three-dimensional porous MoS2a/rGO nanomaterial.
Preferably, in the step 1), the dosage ratio of the graphene to the water is (0.04-0.12) g: 50 mL.
Preferably, in the step 1), the sufficient stirring is performed by using a magnetic stirrer for 2-6 hours.
Preferably, in the step 3), the temperature is increased at a rate of 5-10 ℃ for min in the process of heating from room temperature to 600-800 DEG C-1。
Preferably, in step 3), the flow rate of the introduced argon is controlled: when the temperature is increased from room temperature to 100-300 ℃, controlling the volume flow of the argon gas to be 0-50 sccm; and after the heat preservation treatment is finished, controlling the volume flow of the argon gas to be 100-200 sccm.
Preferably, in the step 4), the product is washed with deionized water for 3-6 times and then freeze-dried for 8-12 hours.
The invention discloses a three-dimensional porous MoS prepared by the preparation method2a/rGO nanomaterial.
The invention also discloses the three-dimensional porous MoS2The application of the/rGO nano material as a negative electrode material of a sodium ion battery.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a three-dimensional porous MoS2Firstly, Graphene (GO) is dispersed in deionized water to prepare GO/H2O dispersion, then H2CNSNH2Addition to GO/H2Adding MoO into O dispersion3Removing water in the solution by heating and evaporating while stirring to form a preform, wherein the material structure of the formed preform is very stable, then carrying out solid-phase reaction under argon atmosphere, and finally cleaning and drying the prepared product to obtain the three-dimensional porous MoS2a/rGO nanomaterial. The method has the characteristics of simple preparation process, easy control of reaction, short period, low energy consumption, high repeatability, high yield and the like. Meanwhile, the method also breaks through the preparation of MoS by most of documents under hydrothermal conditions or a method of hydrothermal treatment and heat treatment2The bottleneck of/rGO is caused by the problems of poor repeatability and low yield of hydrothermal conditions.
Further, H is realized by controlling the volume flow of argon gas in the reaction process2CNSNH2The gas generated by decomposition can reduce MoO3But also can satisfy the pore-forming effect.
The three-dimensional porous nano-structured MoS prepared by the method2the/rGO shows excellent conductivity, cycling stability and high specific discharge capacity, and can be widely used as a negative electrode material of a sodium ion battery.
Drawings
FIG. 1 shows a three-dimensional porous nanostructured MoS2Raman plot of/rGO;
FIG. 2a shows a three-dimensional porous nanostructured MoS2SEM result graph of/rGO;
FIG. 2b three-dimensional porous nanostructured MoS2TEM result graph of/rGO;
FIG. 3 shows MoS2Cycle performance test plots for/rGO.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
Three-dimensional porous MoS2The preparation method of the/rGO nano material comprises the following steps:
1) dispersing 0.04g GO in about50mL of deionized water, 1.0g H2CNSNH2Addition to GO/H2Stirring the O dispersion for 2 hours on a magnetic stirrer to prepare a solution A;
2) 0.25g of MoO3Adding the mixture into the solution A, and heating and evaporating water in the solution through magnetic stirring to obtain a required prefabricated body;
3) under the condition of argon as protective gas, the preform is heated at 5 ℃ for min-1Heating the mixture from room temperature to 600 ℃, and keeping the temperature for 4.0 h;
in the heat preservation treatment process, when the temperature is raised from room temperature to 100 ℃, the volume flow of the argon gas is controlled to be 0sccm so as to keep high concentration S and MoO3Reacting, adjusting the argon to 100sccm after the reaction is finished to discharge redundant gas, and then naturally cooling to room temperature;
4) washing the obtained product with deionized water for 3 times, and freeze-drying the product for 8h to obtain the three-dimensional porous MoS2a/rGO nanomaterial.
Example 2
Three-dimensional porous MoS2The preparation method of the/rGO nano material comprises the following steps:
1) 0.06g GO was dispersed in about 50mL deionized water, 1.5g H2CNSNH2Addition to GO/H2Stirring the O dispersion for 3 hours on a magnetic stirrer to prepare a solution A;
2) 0.3g of MoO3Adding the solution A into the solution A, and heating and evaporating water in the solution through magnetic stirring to obtain a required prefabricated body;
3) under the condition of argon as protective gas, the preform is heated at 6 ℃ for min-1Heating to 650 ℃ at the speed of the temperature, and keeping the temperature for 3.5 hours;
in the process of heat preservation treatment, when the temperature is raised from room temperature to 150 ℃, the volume flow of the argon gas is controlled to be 10sccm so as to keep high concentration S and MoO3Reacting, adjusting the argon to 120sccm after the reaction is finished to discharge redundant gas, and then naturally cooling to room temperature;
4) washing the obtained product with deionized water for 4 times, freeze drying for 9 hr to obtain three-dimensional productHole MoS2a/rGO nanomaterial.
Example 3
Three-dimensional porous MoS2The preparation method of the/rGO nano material comprises the following steps:
1) 0.08g GO was dispersed in about 50mL deionized water. 2.0g H2CNSNH2Addition to GO/H2Stirring the O dispersion for 4 hours on a magnetic stirrer to prepare a solution A;
2) 0.4g of MoO3Adding the solution A into the solution A, and heating and evaporating water in the solution through magnetic stirring to obtain a required prefabricated body;
3) under the condition of argon as protective gas, the preform is heated at 7 ℃ for min-1Heating to 700 ℃ at the rate of (1), and keeping the temperature for 3.0 h.
In the heat preservation treatment process, when the temperature is raised from room temperature to 200 ℃, the volume flow of the argon gas is controlled to be 0sccm so as to maintain high concentration S and MoO3Reacting, adjusting the argon to 150sccm after the reaction is finished to discharge redundant gas, and then naturally cooling to room temperature;
4) washing the obtained product with deionized water for 4 times, and freeze-drying the product for 10h to obtain the three-dimensional porous MoS2a/rGO nanomaterial.
Example 4
Three-dimensional porous MoS2The preparation method of the/rGO nano material comprises the following steps:
1) 0.10g GO was dispersed in about 50mL deionized water, 2.5g H2CNSNH2Addition to GO/H2Stirring the O dispersion for 5 hours on a magnetic stirrer to prepare a solution A;
2) 0.45g of MoO3Adding the solution A into the solution A, and heating and evaporating water in the solution through magnetic stirring to obtain a required prefabricated body;
3) under the condition of argon as protective gas, the preform is heated at 8 ℃ for min-1Heating to 750 ℃ at the speed of the temperature, and keeping the temperature for 2.5 hours;
during the heat preservation treatment, when the temperature is raised from room temperature to 250 ℃, the volume flow of the argon gas is controlled to be 40sccm so as to keep highConcentration of S and MoO3Reacting, adjusting the argon to 180sccm after the reaction is finished to discharge redundant gas, and then naturally cooling to room temperature;
4) washing the obtained product with deionized water for 5 times, and freeze-drying the product for 11h to obtain the three-dimensional porous MoS2a/rGO nanomaterial.
Example 5
Three-dimensional porous MoS2The preparation method of the/rGO nano material comprises the following steps:
1) 0.12g GO was dispersed in about 50mL deionized water, 3.0g H2CNSNH2Addition to GO/H2Stirring for 6 hours in the O dispersion on a magnetic stirrer to prepare a solution A;
2) 0.5g of MoO3Adding the solution A into the solution A, and heating and evaporating water in the solution through magnetic stirring to obtain a required prefabricated body;
3) under the condition of argon as protective gas, the preform is heated at 10 ℃ for min-1Heating to 800 ℃ at the speed of (1), and keeping the temperature for 2.0 h;
in the process of heat preservation treatment, when the temperature is raised from room temperature to 300 ℃, the volume flow of the argon gas is controlled to be 50sccm so as to keep high concentration S and MoO3Reacting, adjusting the argon to 200sccm after the reaction is finished to discharge redundant gas, and then naturally cooling to room temperature;
4) washing the obtained product with deionized water for 6 times, and freeze-drying the product for 12h to obtain the three-dimensional porous MoS2a/rGO nanomaterial.
Referring to FIG. 1, from FIG. 1, sulfur vapor and MoO can be obtained3The reaction is carried out to generate MoS2Finally preparing the MoS with the three-dimensional porous structure2a/rGO nanomaterial.
Referring to FIG. 2, from FIG. 2a, a scanning electron micrograph of a sample, it can be seen that MoS2the/rGO nano material presents a three-dimensional porous structure, and the size of a sample is uniform and the distribution is uniform. Such MoS2The stable existence of the/rGO three-dimensional porous nano structure ensures that the/rGO three-dimensional porous nano structure can have good circulation stability in a sodium ion battery. From FIG. 2b, i.e. transmission of the sampleAs can be seen in the mirror image, MoS2The exact combination with rGO was successful. Namely MoS2Uniformly attached to the surface of rGO.
Referring to FIG. 3, as can be seen from FIG. 3, MoS2the/rGO composite material has a high current density of 1000mA g-1After the lower cycle of 100 circles, the discharge capacity of the lithium ion battery is still as high as 280mA h g-1。

Claims (6)

1. Three-dimensional porous MoS2The preparation method of the/rGO nano material is characterized by comprising the following steps:
1) dispersing graphene in water, and then adding H2CNSNH2Fully and uniformly stirring to prepare a solution A; wherein the graphene and H are used2CNSNH2The mass ratio of (0.04-0.12): (1.0-3.0);
the dosage ratio of the used graphene to water is (0.04-0.12) g: 50 mL;
2) adding MoO3Adding the mixture into the solution A, and heating and evaporating while stirring to obtain a prefabricated body;
3) heating the prefabricated body from room temperature to 600-800 ℃ in an argon atmosphere, preserving heat for 2.0-4.0 h, and cooling to room temperature;
controlling the flow rate of the introduced argon: when the temperature is increased from room temperature to 100-300 ℃, controlling the volume flow of the argon gas to be 0-50 sccm; after the heat preservation treatment is finished, controlling the volume flow of the argon gas to be 100-200 sccm;
4) washing and drying the cooled product to obtain the three-dimensional porous MoS2a/rGO nanomaterial.
2. The three-dimensional porous MoS of claim 12The preparation method of the/rGO nano material is characterized in that in the step 1), the magnetic stirrer is used for stirring for 2-6 hours when the nano material is fully and uniformly stirred.
3. The three-dimensional porous MoS of claim 12The preparation method of/rGO nano material is characterized in that in the step 3), the temperature is raised to be 5 to 800 ℃ from room temperature10℃min-1。
4. The three-dimensional porous MoS of claim 12The preparation method of the/rGO nano material is characterized in that in the step 4), the product is washed by deionized water for 3-6 times and then is frozen and dried for 8-12 hours.
5. Three-dimensional porous MoS prepared by the preparation method of any one of claims 1 to 42a/rGO nanomaterial.
6. The three-dimensional porous MoS of claim 52The application of the/rGO nano material as a negative electrode material of a sodium ion battery.
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