CN108899514A - A kind of three-dimensional porous MoS2/ rGO nano material and its preparation method and application - Google Patents
A kind of three-dimensional porous MoS2/ rGO nano material and its preparation method and application Download PDFInfo
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- CN108899514A CN108899514A CN201810718112.9A CN201810718112A CN108899514A CN 108899514 A CN108899514 A CN 108899514A CN 201810718112 A CN201810718112 A CN 201810718112A CN 108899514 A CN108899514 A CN 108899514A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
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- 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
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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
- H01M4/58—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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of three-dimensional porous MoS2/ rGO nano material and its preparation method and application, belongs to sodium ion battery electrode material preparation technical field.During the preparation process with solid phase method fabricated in situ three-dimensional porous nano structure MoS2/ rGO nano material.The features such as relative to the methods of heat treatment after most of hydro-thermal method reported in the literature or elder generation's hydro-thermal, this method has process simple, reacts easily-controllable, repeatability height, yield is big.H is realized by control argon gas volume flow on this basis2CNSNH2Reduction MoO can both be played by decomposing the gas generated3It can satisfy the effect of pore-creating again.The experimental results showed that through three-dimensional porous nano structure MoS made from the method for the present invention2/ rGO shows excellent electric conductivity, cyclical stability and high specific discharge capacity, can be widely used as anode material of lithium-ion battery.
Description
Technical field
The invention belongs to sodium ion battery electrode material preparation technical fields, and in particular to a kind of three-dimensional porous MoS2/rGO
Nano material and its preparation method and application.
Background technique
With the fast development in electric car and moving electronic components market, the requirement to battery material is higher and higher.
Suitable battery material is found to have a great impact to the function of electronic equipment.The main composition of lithium ion battery is anode, is born
Pole and electrolyte.Positive and negative anodes are the basic materials that electrochemical reaction occurs, and are the bases that chemical energy is converted into electric energy, and electrolyte
It is the carrier of battery intermediate ion transmission.However lithium resource is rare, limits it and further develops.Sodium-ion battery has high
Energy density and it is longer using birthday noodle and it is environmental-friendly the features such as, by it is believed that being most possibly to be deposited as the energy
The system of storage.Sodium-ion battery material, one of the branch as new energy materials, more receives extensive research
Molybdenum disulfide (MoS2), theoretical capacity is up to 670mAh g-1, it is expected to become next-generation sodium-ion battery cathode material
Material.MoS2Sandwich layer structure with S-Mo-S, atom is combined by strong covalent bond in layer, there is weak model moral between layers
Magnificent power effect.But as the negative electrode material of sodium-ion battery in use, due to charge and discharge process intermediate ion insertion and abjection, especially
It is that the deintercalation process of sodium ion can make the MoS with high surface energy2Lamellar structure collapse accumulation, it is forthright again to reduce it
Can and cyclical stability, and then affect the electric conductivity of electrons/ions between the lamella of S-Mo-S, reduce its electrochemistry
Energy.
Summary of the invention
The purpose of the present invention is to provide a kind of three-dimensional porous MoS2/ rGO nano material and its preparation method and application, should
Method preparation process is simple, reacts easily-controllable, and reaction time is short, and low energy consumption, and repeatability is high, and yield is high, is suitble to large-scale production；Through
MoS made from this method2Composite granule purity is high, pattern is porous structure, and uniform particle sizes may be used as the secondary electricity of sodium ion
Pond negative electrode material.
The present invention is to be achieved through the following technical solutions：
The invention discloses a kind of three-dimensional porous MoS2The preparation method of/rGO nano material, includes the following steps：
1) it disperses graphene in water, H is then added2CNSNH2, stir, obtained solution A；Wherein, used
Graphene and H2CNSNH2Mass ratio be (0.04~0.12)：(1.0~3.0)；
2) by MoO3It is added in solution A, heating evaporation is handled while stirring, and precast body is made；
3) precast body under an argon atmosphere, is heated to 600~800 DEG C by room temperature, 2.0~4.0h is kept the temperature, is cooled to room
Temperature；
4) by after product after cooling washing, drying, three-dimensional porous MoS is made2/ rGO nano material.
Preferably, in step 1), the amount ratio of graphene and water used is (0.04~0.12) g：50mL.
Preferably, in step 1), stirring is to utilize magnetic stirrer 2~6 hours.
Preferably, in step 3), during being heated to 600~800 DEG C by room temperature, heating rate is 5~10 DEG C of min-1。
Preferably, in step 3), the flow velocity for the argon gas being passed through is controlled：When temperature is by room temperature to 100~300
DEG C when, control argon gas volume flow be 0~50sccm；After isothermal holding, control argon gas volume flow is 100
~200sccm.
It preferably, is to be freeze-dried 8~12h after product is cleaned 3~6 times with deionized water in step 4).
The invention discloses using three-dimensional porous MoS made from above-mentioned preparation method2/ rGO nano material.
The invention also discloses above-mentioned three-dimensional porous MoS2/ rGO nano material is as anode material of lithium-ion battery
Using.
Compared with prior art, the invention has the following beneficial technical effects：
Three-dimensional porous MoS disclosed by the invention2/ rGO nano material and preparation method thereof first disperses graphene (GO)
In deionized water, GO/H is made2O dispersion, then by H2CNSNH2It is added to GO/H2In O dispersion, MoO is added3, lead to
It is removed in solution after the processing of heating evaporation while stirring and forms precast body after moisture, the material structure of the precast body of formation is very steady
Gu solid phase reaction then occurs under an argon atmosphere again, finally by product cleaning obtained, drying, three-dimensional porous MoS is obtained2/
RGO nano material.This method has preparation process simple, reacts easily-controllable, and the period is short, and low energy consumption, and repeatability is high, and yield is big to wait spies
Point.Meanwhile this method has also broken most of document heat-treating methods preparation MoS under hydrothermal conditions or after first hydro-thermal2/
The bottleneck that rGO, because hydrothermal condition has the problem of poor repeatability, low yield.
Further, H is realized by control argon gas volume flow during the reaction2CNSNH2Decompose generation
Gas can both play reduction MoO3It can satisfy the effect of pore-creating again.
Through three-dimensional porous nano structure MoS made from the method for the present invention2/ rGO shows excellent electric conductivity, stable circulation
Property and high specific discharge capacity, can be widely used as anode material of lithium-ion battery.
Detailed description of the invention
Fig. 1 is three-dimensional porous nano structure MoS2The Raman of/rGO schemes；
Fig. 2 a is three-dimensional porous nano structure MoS2The SEM result figure of/rGO；
Fig. 2 b three-dimensional porous nano structure MoS2The TEM result figure of/rGO；
Fig. 3 is MoS2The cycle performance test chart of/rGO.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
A kind of three-dimensional porous MoS2The preparation method of/rGO nano material, includes the following steps：
1) 0.04g GO is dispersed in about 50mL deionized water, by 1.0g H2CNSNH2It is added to GO/H2In O dispersion
And 2h is stirred on magnetic stirring apparatus, obtained solution A；
2) by 0.25g MoO3It is added in above-mentioned solution A, after moisture in magnetic agitation and heating evaporation solution, obtains
To required precast body；
3) under the conditions of argon gas is as protective gas, by precast body with 5 DEG C of min-1Rate be heated to 600 DEG C by room temperature,
Keep the temperature 4.0h；
During isothermal holding, when temperature reaches 100 DEG C by room temperature, control argon gas volume flow is
0sccm, to keep high concentration S and MoO3Reaction, argon gas is adjusted to 100sccm after reaction, extra gas is discharged, then
Cooled to room temperature；
4) product obtained is cleaned 3 times with deionized water, freeze-drying 8h is carried out to product, is made three-dimensional porous
MoS2/ rGO nano material.
Embodiment 2
A kind of three-dimensional porous MoS2The preparation method of/rGO nano material, includes the following steps：
1) 0.06g GO is dispersed in about 50mL deionized water, by 1.5g H2CNSNH2It is added to GO/H2In O dispersion
And 3h is stirred on magnetic stirring apparatus, obtained solution A；
2) by 0.3g MoO3It is added to above-mentioned solution A, after moisture in magnetic agitation and heating evaporation solution, is obtained
Required precast body；
3) under the conditions of argon gas is as protective gas, by precast body with 6 DEG C of min-1Rate be heated to 650 DEG C, heat preservation
3.5h；
During isothermal holding, when temperature reaches 150 DEG C by room temperature, control argon gas volume flow is
10sccm, to keep high concentration S and MoO3Reaction, argon gas is adjusted to 120sccm after reaction, extra gas is discharged, with
Cooled to room temperature afterwards；
4) product obtained is cleaned 4 times with deionized water, freeze-drying 9h is carried out to product, is made three-dimensional porous
MoS2/ rGO nano material.
Embodiment 3
A kind of three-dimensional porous MoS2The preparation method of/rGO nano material, includes the following steps：
1) 0.08g GO is dispersed in about 50mL deionized water.By 2.0g H2CNSNH2It is added to GO/H2In O dispersion
And 4h is stirred on magnetic stirring apparatus, obtained solution A；
2) by 0.4g MoO3It is added to above-mentioned solution A, after moisture in magnetic agitation and heating evaporation solution, is obtained
Required precast body；
3) under the conditions of argon gas is as protective gas, by precast body with 7 DEG C of min-1Rate be heated to 700 DEG C, heat preservation
3.0h。
During isothermal holding, when temperature reaches 200 DEG C by room temperature, control argon gas volume flow is
0sccm, to keep high concentration S and MoO3Reaction, argon gas is adjusted to 150sccm after reaction, extra gas is discharged, then
Cooled to room temperature；
4) product obtained is cleaned 4 times with deionized water, freeze-drying 10h is carried out to product, is made three-dimensional porous
MoS2/ rGO nano material.
Embodiment 4
A kind of three-dimensional porous MoS2The preparation method of/rGO nano material, includes the following steps：
1) 0.10g GO is dispersed in about 50mL deionized water, by 2.5g H2CNSNH2It is added to GO/H2In O dispersion
And 5h is stirred on magnetic stirring apparatus, obtained solution A；
2) by 0.45g MoO3It is added to above-mentioned solution A, after moisture in magnetic agitation and heating evaporation solution, is obtained
Required precast body；
3) under the conditions of argon gas is as protective gas, by precast body with 8 DEG C of min-1Rate be heated to 750 DEG C, heat preservation
2.5h；
During isothermal holding, when temperature reaches 250 DEG C by room temperature, control argon gas volume flow is
40sccm, to keep high concentration S and MoO3Reaction, argon gas is adjusted to 180sccm after reaction, extra gas is discharged, with
Cooled to room temperature afterwards；
4) product obtained is cleaned 5 times with deionized water, freeze-drying 11h is carried out to product, is made three-dimensional porous
MoS2/ rGO nano material.
Embodiment 5
A kind of three-dimensional porous MoS2The preparation method of/rGO nano material, includes the following steps：
1) 0.12g GO is dispersed in about 50mL deionized water, by 3.0g H2CNSNH2It is added to GO/H2In O dispersion
And 6h is stirred on magnetic stirring apparatus, obtained solution A；
2) by 0.5g MoO3It is added to above-mentioned solution A, after moisture in magnetic agitation and heating evaporation solution, is obtained
Required precast body；
3) under the conditions of argon gas is as protective gas, by precast body with 10 DEG C of min-1Rate be heated to 800 DEG C, heat preservation
2.0h；
During this during isothermal holding, when temperature reaches 300 DEG C by room temperature, argon gas body is controlled
Product flow is 50sccm, to keep high concentration S and MoO3Reaction, argon gas is adjusted to 200sccm after reaction, extra to be discharged
Gas, subsequent cooled to room temperature；
4) product obtained is cleaned 6 times with deionized water, freeze-drying 12h is carried out to product, is made three-dimensional porous
MoS2/ rGO nano material.
It referring to Fig. 1, can be obtained from Fig. 1, sulfur vapor and MoO3It carries out reaction and generates MoS2, finally preparing has three-dimensional more
The MoS of pore structure2/ rGO nano material.
Referring to fig. 2, from Fig. 2 a, i.e., as can be seen that MoS in the scanning electron microscope (SEM) photograph of sample2/ rGO nano material shows three
Porous structure is tieed up, sample size is uniform and is evenly distributed.This MoS2/ rGO three-dimensional porous nano structure is stabilized
It ensure that it can possess good cyclical stability in sodium-ion battery.It, i.e., can in the transmission electron microscope picture of sample from Fig. 2 b
To find out, MoS2With rGO compound success really.That is MoS2Uniformly adhere on the surface rGO.
Referring to Fig. 3, from figure 3, it can be seen that MoS2/ rGO composite material is in high current density 1000mA g-1Lower circulation 100
After circle, discharge capacity is still up to 280mA h g-1。
Claims (8)
1. a kind of three-dimensional porous MoS2The preparation method of/rGO nano material, which is characterized in that include the following steps：
1) it disperses graphene in water, H is then added2CNSNH2, stir, obtained solution A；Wherein, graphite used
Alkene and H2CNSNH2Mass ratio be (0.04~0.12)：(1.0~3.0)；
2) by MoO3It is added in solution A, heating evaporation is handled while stirring, and precast body is made；
3) precast body under an argon atmosphere, is heated to 600~800 DEG C by room temperature, 2.0~4.0h is kept the temperature, is cooled to room temperature；
4) by after product after cooling washing, drying, three-dimensional porous MoS is made2/ rGO nano material.
2. three-dimensional porous MoS according to claim 12The preparation method of/rGO nano material, which is characterized in that step 1)
In, the amount ratio of graphene and water used is (0.04~0.12) g：50mL.
3. three-dimensional porous MoS according to claim 12The preparation method of/rGO nano material, which is characterized in that step 1)
In, stirring is to utilize magnetic stirrer 2~6 hours.
4. three-dimensional porous MoS according to claim 12The preparation method of/rGO nano material, which is characterized in that step 3)
In, during being heated to 600~800 DEG C by room temperature, heating rate is 5~10 DEG C of min-1。
5. three-dimensional porous MoS according to claim 12The preparation method of/rGO nano material, which is characterized in that step 3)
In, the flow velocity for the argon gas being passed through is controlled：When temperature by room temperature to 100~300 DEG C when, control argon gas volume
Flow is 0~50sccm；After isothermal holding, control argon gas volume flow is 100~200sccm.
6. three-dimensional porous MoS according to claim 12The preparation method of/rGO nano material, which is characterized in that step 4)
In, it is to be freeze-dried 8~12h after product is cleaned 3~6 times with deionized water.
7. using three-dimensional porous MoS made from preparation method described in any one of claim 1~62/ rGO nano material.
8. three-dimensional porous MoS as claimed in claim 72Application of/rGO the nano material as anode material of lithium-ion battery.
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Cited By (1)
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| CN109686954A (en) * | 2018-12-27 | 2019-04-26 | 陕西科技大学 | A kind of C-O-Mo key bridge joint monolithic taper MoS2/ NG sodium ion negative electrode material and preparation method thereof |
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