CN109326784B - Phosphorus doped MoS2Preparation method and application of loaded graphene nanosheet - Google Patents

Phosphorus doped MoS2Preparation method and application of loaded graphene nanosheet Download PDF

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CN109326784B
CN109326784B CN201811221414.1A CN201811221414A CN109326784B CN 109326784 B CN109326784 B CN 109326784B CN 201811221414 A CN201811221414 A CN 201811221414A CN 109326784 B CN109326784 B CN 109326784B
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graphene
mos
phosphorus
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CN109326784A (en
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李丹
张岩
苏行
张建民
李勇盛
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Zhengzhou University
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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
    • 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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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 provides phosphorus-doped MoS with controllable proportion2The preparation method of the loaded graphene nanosheet comprises the steps of preparing graphene oxide; MoS is prepared by loading Mo source on graphene oxide by hydrothermal method2Loading graphene; doping phosphorus into MoS by vapor deposition2Loading graphene to obtain phosphorus-doped MoS2And loading graphene nano sheets. The nanosheet is used as an electrode material of a sodium-ion battery and has excellent energy storage performance.

Description

Phosphorus doped MoS2Preparation method and application of loaded graphene nanosheet
Technical Field
The invention relates to the technical field of composite material preparation, in particular to phosphorus-doped MoS with controllable proportion2A preparation method of a loaded graphene nanosheet and application in energy storage.
Background
With the coming of the electronic information era, people have more and more requirements on electronic products, and lithium ion batteries are widely applied to portable electronic products as energy storage elements. Because the lithium ion natural resource is deficient and the cost is high, the large-scale application of the lithium ion energy storage equipment is greatly limited, and therefore, the search for a metal capable of replacing a lithium source is very important. Sodium ion batteries have attracted much attention due to their abundant resources, low cost, and similar chemical properties of Li and Na.
In recent years, layered transition metal compounds, particularly MoS2It is considered to be a good electrode material due to its unique layered structure and electronic properties. Research shows that MoS2Has 670 mAh g-1The theoretical specific capacity of the graphite is 2 times of that of the traditional graphite carbon. As is well known, MoS2The main reason for the poor electrochemical performance of (A) is due to the fact that sodium ions cause MoS during intercalation and deintercalation2Volume expansion, which in turn causes the electrode material to shatter. Thus, building a special structure for lifting MoS2Electrochemical property ofCan be of critical importance.
Disclosure of Invention
To solve the above technical problems, the present invention provides a phosphorus-doped MoS2Preparation method of loaded graphene nanosheet, and phosphorus-doped MoS obtained by the preparation method2The graphene nanosheets are loaded, the proportion of the doped phosphorus elements is controllable, and the nanosheets can be used as electrode materials in sodium-ion batteries, so that the stability and the energy storage performance of the electrode materials are improved.
In order to achieve the purpose, the invention adopts the technical scheme that:
phosphorus doped MoS2The preparation method of the loaded graphene nanosheet comprises the following steps:
(1) preparing graphene oxide;
(2) MoS is prepared by loading Mo source on graphene oxide by hydrothermal method2Loading graphene;
(3) doping phosphorus into MoS by vapor deposition2Loading graphene to obtain phosphorus-doped MoS2Loading graphene nanosheets;
the specific process of the step (3) is as follows: the MoS prepared in the step (2) is added2Respectively placing the loaded graphene and the phosphorus source in porcelain boats, placing the two porcelain boats in a tube furnace from top to bottom, and calcining under the protection of inert gas to obtain phosphorus-doped MoS2And loading graphene nano sheets.
Preferably, the surface of the graphene oxide prepared in the step (1) is negatively charged.
Preferably, the specific process of step (1) is as follows: placing concentrated sulfuric acid with the mass concentration of 98% in an ice water bath, adding crystalline flake graphite into the concentrated sulfuric acid, and stirring for 20-30 min; then adding potassium permanganate, stirring for 1-3 h, transferring to a constant-temperature water bath kettle at 35 ℃ and stirring at a constant speed until the solution becomes viscous yellow brown; after the reaction is finished, adding deionized water into the solution and continuously stirring until the solution is cooled to room temperature; then adding 30 percent of H by mass2O2Stirring uniformly, and finally using dilute hydrochloric acid with the mass fraction of 5%And washing with deionized water, and carrying out vacuum freeze drying to obtain the graphene oxide. The method for preparing the graphene oxide hydrosol is an optimized and improved Hummer's method.
Preferably, the specific process of step (2) is as follows: ultrasonically dispersing the graphene oxide prepared in the step (1) in deionized water, adding ammonium molybdate tetrahydrate, stirring uniformly, and adding thiourea; transferring the mixed solution into a reaction kettle, and keeping the temperature at 200 ℃ for 24 hours; after the reaction is finished, washing the reaction product by deionized water, and carrying out vacuum freeze drying to obtain MoS2And loading graphene.
Preferably, in the step (3), the phosphorus source is sodium hypophosphite, MoS2The mass ratio of the loaded graphene to the sodium hypophosphite is 1: 5-1: 20.
Preferably, in the step (3), the inert gas is argon or nitrogen.
Preferably, MoS in the step (3) is adopted2The loaded graphene is positioned above the sodium hypophosphite.
Preferably, the calcining conditions in the step (3) are as follows: the temperature rise rate is 2 ℃/min, and the calcination is carried out for 3-4 h at the temperature of 300-350 ℃.
The phosphorus-doped MoS prepared by the preparation method2The loaded graphene nanosheet is applied to a sodium-ion battery as an electrode material.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention synthesizes MoS by a hydrothermal method2Loading graphene composite material, and then doping phosphorus into MoS by adopting a vapor deposition method2In the loaded graphene composite material, it is worth mentioning that the electronic conductivity of the composite material can be effectively improved by phosphorus doping; the coating of the graphene can improve the conductivity and effectively inhibit MoS2The volume expansion generated in the process of sodium ion embedding and removing improves the stability of the nano sheet as an electrode material, thereby improving the energy storage performance of the nano sheet.
2. According to electrochemical performance tests, the method obtainsPhosphorus doped MoS of2The graphene-loaded nanosheet composite material shows excellent electrochemical performance.
3. The preparation method can obtain phosphorus-doped MoS with controllable proportion2The loaded graphene nanosheet is a sodium-ion battery anode material which is rarely reported, so that the material has practical significance and application value for research and development.
4. The preparation method of the invention does not need to add other surfactants, metal coordination agents and the like, has simple operation steps and low requirement on equipment. Compared with the materials reported in the prior art, the phosphorus-doped MoS with controllable proportion2The loaded graphene nanosheet has a wide application prospect as a novel energy storage electrode material.
Drawings
FIG. 1 is example 1 phosphorus doped MoS2Loaded graphene and MoS2An X-ray diffraction pattern of the loaded graphene;
FIG. 2 is example 1 phosphorus doped MoS2Scanning electron micrographs of the loaded graphene;
FIG. 3 is example 1 phosphorus doped MoS2Carrying out element distribution of a graphene-loaded scanning electron microscope;
FIG. 4 is example 1 phosphorus doped MoS2A cyclic voltammogram of the loaded graphene;
FIG. 5 phosphorus doped MoS of example 12The current density of the loaded graphene is 0.2 A.g-1Cycle performance graph below.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
Phosphorus doped MoS of this example2The preparation method of the loaded graphene nanosheet comprises the following steps:
1. preparing graphene oxide: adding 70 mL of concentrated sulfuric acid with the mass concentration of 98% into a 500 mL three-neck flask and putting the flask into an ice water bath; weighing 2 g of flake graphite, adding the flake graphite into a three-neck flask containing concentrated sulfuric acid, and mechanically stirring for 20 min; 8 g of potassium permanganate are weighed and slowly added into the mixtureStirring the mixed solution for 2 hours in an ice bath, transferring the mixed solution into a constant-temperature water bath kettle at 35 ℃ and stirring the mixed solution for 12 hours at a constant speed (overnight) until the solution becomes viscous yellow brown; removing the three-neck flask out of the water bath kettle, slowly dripping 297 mL of deionized water, and continuously stirring until the temperature is cooled to room temperature; 25 mL of H with the mass fraction of 30 percent is weighed2O2Adding the graphene oxide into the solution, washing the graphene oxide with the diluted hydrochloric acid and the deionized water respectively for three times by using the mass fraction of 5%, and carrying out vacuum freeze drying for 48 hours to obtain graphene oxide with negative electricity on the surface;
2. preparation of MoS2Loading graphene: adding 50 mg of graphene oxide prepared in the step 1 into 30 mL of deionized water, ultrasonically mixing for 2 h, adding 0.1 g of ammonium molybdate tetrahydrate, stirring for 5 min, adding 0.15 g of thiourea, and stirring for 30 min; transferring the solution to a 50 mL hydrothermal kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven at 200 ℃, and keeping the temperature for 24 hours; naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle to obtain a black hydrogel column, soaking and washing with deionized water to remove soluble impurities, and freeze-drying under vacuum to obtain MoS2Loading a graphene composite material;
3. preparation of phosphorus-doped MoS2Loading graphene: 50 mg of the MoS prepared in step 2 was taken2The loaded graphene composite material and 350 mg sodium hypophosphite are respectively loaded in two porcelain boats, and MoS is added2The loaded graphene composite material is arranged at the upstream of the tubular furnace, and the sodium hypophosphite is arranged at the downstream of the tubular furnace and keeps a certain distance; calcining the tube furnace for 3 hours at the temperature rising rate of 2 ℃/min and the constant temperature of 350 ℃ under the protection of argon, and obtaining the phosphorus-doped MoS after the reaction is finished2And loading the graphene nanosheet composite material.
Example 2
Phosphorus doped MoS of this example2The preparation method of the loaded graphene nanosheet comprises the following steps:
1. preparing graphene oxide: adding 70 mL of concentrated sulfuric acid with the mass concentration of 98% into a 500 mL three-neck flask and putting the flask into an ice water bath; weighing 2 g of flake graphite, adding the flake graphite into a three-neck flask containing concentrated sulfuric acid, and mechanically stirring for 25 min; 8 g of potassium permanganate is weighed and slowly added into the mixed solutionStirring for 2 h in ice bath, transferring to a constant-temperature water bath kettle at 35 ℃ and stirring at constant speed for 12 h (overnight) until the solution becomes viscous yellow brown; removing the three-neck flask out of the water bath kettle, slowly dripping 297 mL of deionized water, and continuously stirring until the temperature is cooled to room temperature; 25 mL of H with the mass fraction of 30 percent is weighed2O2Adding the graphene oxide into the solution, washing the graphene oxide with the diluted hydrochloric acid and the deionized water respectively for three times by using the mass fraction of 5%, and carrying out vacuum freeze drying for 48 hours to obtain graphene oxide with negative electricity on the surface;
2. preparation of MoS2Loading graphene: adding 50 mg of graphene oxide prepared in the step 1 into 30 mL of deionized water, ultrasonically mixing for 2 h, adding 0.1 g of ammonium molybdate tetrahydrate, stirring for 5 min, adding 0.15 g of thiourea, and stirring for 30 min; transferring the solution to a 50 mL hydrothermal kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven at 200 ℃, and keeping the temperature for 24 hours; naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle to obtain a black hydrogel column, soaking and washing with deionized water to remove soluble impurities, and freeze-drying under vacuum to obtain MoS2Loading a graphene composite material;
3. preparation of phosphorus-doped MoS2Loading graphene: 50 mg of the MoS prepared in step 2 was taken2Loading graphene composite material and 500 mg sodium hypophosphite into two porcelain boats, and packaging MoS2The loaded graphene composite material is arranged at the upstream of the tubular furnace, and the sodium hypophosphite is arranged at the downstream of the tubular furnace and keeps a certain distance; calcining the tube furnace for 3 hours at the temperature rising rate of 2 ℃/min and the constant temperature of 350 ℃ under the protection of argon, and obtaining the phosphorus-doped MoS after the reaction is finished2And loading the graphene nanosheet composite material.
Example 3
Phosphorus doped MoS of this example2The preparation method of the loaded graphene nanosheet comprises the following steps:
1. preparing graphene oxide: adding 70 mL of concentrated sulfuric acid with the mass concentration of 98% into a 500 mL three-neck flask and putting the flask into an ice water bath; weighing 2 g of flake graphite, adding the flake graphite into a three-neck flask containing concentrated sulfuric acid, and mechanically stirring for 30 min; weighing 8 g of potassium permanganate, slowly adding the potassium permanganate into the mixed solution, and carrying out ice bathStirring for 2 h, transferring into 35 deg.C constant temperature water bath, and stirring at constant speed for 12 h (overnight) until the solution becomes viscous yellow brown; removing the three-neck flask out of the water bath kettle, slowly dripping 297 mL of deionized water, and continuously stirring until the temperature is cooled to room temperature; 25 mL of H with the mass fraction of 30 percent is weighed2O2Adding the graphene oxide into the solution, washing the graphene oxide with the diluted hydrochloric acid and the deionized water respectively for three times by using the mass fraction of 5%, and carrying out vacuum freeze drying for 48 hours to obtain graphene oxide with negative electricity on the surface;
2. preparation of MoS2Loading graphene: adding 50 mg of graphene oxide prepared in the step 1 into 30 mL of deionized water, ultrasonically mixing for 2 h, adding 0.1 g of ammonium molybdate tetrahydrate, stirring for 5 min, adding 0.15 g of thiourea, and stirring for 30 min; transferring the solution to a 50 mL hydrothermal kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven at 200 ℃, and keeping the temperature for 24 hours; naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle to obtain a black hydrogel column, soaking and washing with deionized water to remove soluble impurities, and freeze-drying under vacuum to obtain MoS2Loading a graphene composite material;
3. preparation of phosphorus-doped MoS2Loading graphene: 50 mg of the MoS prepared in step 2 was taken2Loading graphene composite material and 750 mg sodium hypophosphite into two porcelain boats, and packaging MoS2The loaded graphene composite material is arranged at the upstream of the tubular furnace, and the sodium hypophosphite is arranged at the downstream of the tubular furnace and keeps a certain distance; calcining the tube furnace for 3 hours at the temperature rising rate of 2 ℃/min and the constant temperature of 350 ℃ under the protection of argon, and obtaining the phosphorus-doped MoS after the reaction is finished2And loading the graphene nanosheet composite material.
Phosphorus-doped MoS prepared by the invention2The loaded graphene nanosheet shows good electrochemical capacity performance when being used as a sodium ion electrode material, and has a very wide market application prospect in the aspect of energy storage. FIG. 1 shows the MoS obtained2Loaded graphene and phosphorus doped MoS2X-ray diffraction pattern of loaded graphene composite material, wherein MoS is the lowest line2Standard card 00-037-2Initial phase, MoS after phosphorus doping only2Load(s)The lattice spacing of the graphene composite material is slightly widened and the peak intensity is weakened. The obtained phosphorus-doped MoS2The scanning electron micrograph of the loaded graphene composite material is shown in fig. 2, which shows that the phosphorus is doped with MoS2The graphene-loaded composite material is a sheet structure. FIG. 3 is a phosphorus doped MoS2Scanning electron microscope element picture of loaded graphene composite material shows that phosphorus element is successfully doped to MoS2Loading graphene composite materials. FIG. 4 shows the resulting phosphorus-doped MoS2And (3) a cyclic voltammogram of the loaded graphene composite material. FIG. 5 is the phosphorus doped MoS produced2The current density of the loaded graphene composite material is 0.2 A.g-1Cycle performance graph below. The above experimental results show that the phosphorus-doped MoS prepared by the invention2The loaded graphene nanosheet composite material has excellent electrochemical performance in the aspect of preparing an electrode material of a sodium-ion battery.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. Phosphorus doped MoS2The preparation method of the loaded graphene nanosheet is characterized by comprising the following steps:
(1) preparing graphene oxide;
(2) MoS is prepared by loading Mo source on graphene oxide by hydrothermal method2Loading graphene;
(3) doping phosphorus into MoS by vapor deposition2Loading graphene to obtain phosphorus-doped MoS2Loading graphene nanosheets;
the specific process of the step (3) is as follows: the MoS prepared in the step (2) is added2Respectively placing the loaded graphene and the phosphorus source in porcelain boats, placing the two porcelain boats in a tube furnace from top to bottom, and calcining under the protection of inert gas to obtain phosphorus-doped MoS2Loading graphene nanosheets;
the steps of (A), (B), (C2) The specific process comprises the following steps: ultrasonically dispersing the graphene oxide prepared in the step (1) in deionized water, adding ammonium molybdate tetrahydrate, uniformly stirring, and adding thiourea to form a mixed solution; transferring the mixed solution into a reaction kettle, and keeping the temperature at 200 ℃ for 24 hours; after the reaction is finished, washing the reaction product by deionized water, and carrying out vacuum freeze drying to obtain MoS2Loading graphene;
the phosphorus source in the step (3) is sodium hypophosphite or MoS2The mass ratio of the loaded graphene to the sodium hypophosphite is 1: 5-1: 20;
the inert gas in the step (3) is argon or nitrogen;
MoS in the step (3)2The loaded graphene is positioned above the sodium hypophosphite;
the calcining conditions in the step (3) are as follows: the temperature rise rate is 2 ℃/min, and the calcination is carried out for 3-4 h at the temperature of 300-350 ℃.
2. The phosphorus doped MoS of claim 12The preparation method of the loaded graphene nanosheet is characterized in that the surface of the graphene oxide prepared in the step (1) is negatively charged.
3. The phosphorus doped MoS of claim 12The preparation method of the loaded graphene nanosheet is characterized in that the specific process of the step (1) is as follows: placing concentrated sulfuric acid with the mass concentration of 98% in an ice water bath, adding crystalline flake graphite into the concentrated sulfuric acid, and stirring for 20-30 min; then adding potassium permanganate, stirring for 1-3 h, transferring to a constant-temperature water bath kettle at 35 ℃ and stirring at a constant speed until the solution becomes viscous yellow brown; after the reaction is finished, adding deionized water into the solution and continuously stirring until the solution is cooled to room temperature; then adding 30 percent of H by mass2O2And uniformly stirring, washing with 5% by mass of dilute hydrochloric acid and deionized water, and performing vacuum freeze drying to obtain the graphene oxide.
4. The phosphorus doped MoS of any of claims 1 to 32Preparation of loaded graphene nanosheetPhosphorus-doped MoS prepared by preparation method2And loading graphene nano sheets.
5. The phosphorus doped MoS of any of claims 1 to 32Phosphorus-doped MoS prepared by preparation method of loaded graphene nanosheet2The loaded graphene nanosheet is applied to a sodium-ion battery as an electrode material.
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