CN107394127A - A kind of molybdenum disulfide graphene aerogel electrode material preparation method - Google Patents

A kind of molybdenum disulfide graphene aerogel electrode material preparation method Download PDF

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CN107394127A
CN107394127A CN201710443457.3A CN201710443457A CN107394127A CN 107394127 A CN107394127 A CN 107394127A CN 201710443457 A CN201710443457 A CN 201710443457A CN 107394127 A CN107394127 A CN 107394127A
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electrode material
molybdenum disulfide
graphene aerogel
material preparation
aerogel electrode
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刘辉
董婉萌
庞凌燕
梁宇
程乔
程一乔
王子怡
陈南涛
赵向楠
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Shaanxi University of Science and Technology
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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
    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 kind of molybdenum disulfide graphene aerogel electrode material preparation method, specifically implement according to following steps：Step 1, molybdenum trioxide and graphene oxide are added in a certain amount of distilled water, and using ultrasonic cleaner ultrasonic disperse and it is uniformly obtained middle interstitial fluid；Step 2, to sulphur source is added in the middle interstitial fluid obtained through step 1, stir to being well mixed, obtain mixed liquor；Step 3, mixed liquor is transferred to polytetrafluoroethylene (PTFE) hydro-thermal liner by what step 2 obtained, and be put into baking oven, at a certain temperature the hydro-thermal reaction regular hour, after reaction terminates, reactant is naturally cooled into room temperature；Step 4, reactant after cooling wash simultaneously precipitation and separation, isolated precipitation is taken out and is freeze-dried under vacuum, obtains molybdenum disulfide graphene aerogel electrode material.Its preparation process is simple, and cost is low.

Description

A kind of molybdenum disulfide-graphene aerogel electrode material preparation method
Technical field
The invention belongs to nano-functional material preparation method technical field, is related to a kind of molybdenum disulfide-graphene aerogel Electrode material preparation method.
Background technology
Molybdenum disulfide/graphene aerogel electrode material has good elastic characteristic in itself, is very suitable for as soft The electrode material of property battery uses, and can use molybdenum disulfide/electricity of the graphene aerogel composite as lithium ion battery Pole material builds a kind of flexible lithium ion battery, makes full use of the molybdenum disulfide of sandwich layer structure and the two-dimentional honeybee of graphene Nest shape structure, very high electrical conductivity and thermal conductivity, functionalized surface while easy processing can into fexible film, big specific surface area The features such as loading more active materials further improves its chemical property on the basis of flexibility is realized.Molybdenum disulfide/stone It can realize that flexibility can improve the integral energy density of battery again when black alkene material is as electrode.
In recent years, gas gel electrode material has become study hotspot,《Three-dimensional molybdenum disulfide/redox graphene gas Gel is used as macroscopical visible light catalyst》(Zhang R,Wan W,Li D,et al.Three-dimensional MoS2/ reduced graphene oxide aerogel as a macroscopic visible-light photocatalyst [J].Chinese Journal of Catalysis,2017,38(2):313-320.), three-dimensional knot is prepared using hydro-thermal method The molybdenum disulfide of structure/graphene aerogel material is used for photocatalysis field, and prepared material has low-density, and shows good Good adsorption capacity and excellent photocatalysis performance.Yang Zhao et al. prepare the stone of three-dimensional porous structure using hydro-thermal method Black alkene aerogel material (Zhao Y, Liu J, Hu Y, et al.Highly compression-tolerant supercapacitorbased on polypyrrole-mediated graphene foam electrodes[J] .Advanced materials,2013,25(4):591-595.), the flexible performance of graphene aerogel material of preparation Good, density is small, the advantages that excellent electric conductivity, and shows good electrochemical storage performance.
As can be seen here, molybdenum disulfide/graphene aerogel electrode material has very big Research Significance.Study and make simultaneously For the molybdenum disulfide with high power capacity and cyclical stability/graphene aerogel electrode material is gone out, have in flexible material field Great scientific meaning.And the preparation method of the molybdenum disulfide reported at present/graphene aerogel electrode material is mainly with certainly Assembling and phase transfer method are in the majority, and hydrothermal preparing process is less.Self assembly and phase transfer method preparation process are complicated, and process is not easily-controllable System, and production cost is high, also there is certain pollution to environment.
The content of the invention
It is an object of the invention to provide a kind of molybdenum disulfide-graphene aerogel electrode material preparation method, it was prepared Journey is simple, and cost is low.
The technical solution adopted in the present invention is a kind of molybdenum disulfide-graphene aerogel electrode material preparation method, tool Body is implemented according to following steps：
Step 1, molybdenum trioxide and graphene oxide are added in a certain amount of distilled water, and surpassed using ultrasonic cleaner Sound disperses and it is uniformly obtained middle interstitial fluid；
Step 2, to sulphur source is added in the middle interstitial fluid obtained through step 1, stir to being well mixed, obtain mixed liquor；
Step 3, mixed liquor is transferred to polytetrafluoroethylene (PTFE) hydro-thermal liner by what step 2 obtained, and be put into baking oven, one The hydro-thermal reaction regular hour at fixed temperature, after reaction terminates, reactant is naturally cooled into room temperature；
Step 4, reactant after cooling wash simultaneously precipitation and separation, isolated precipitation taken out and in vacuum bar It is freeze-dried under part, obtains molybdenum disulfide-graphene aerogel electrode material.
The features of the present invention also resides in,
The amount of the material of molybdenum trioxide is 1mmol~10mmol in the middle interstitial fluid of step 1, and the quality of graphene oxide is 10mg~50mg, the volume of distilled water is 200mL~500mL.
The ultrasonic cleaner that ultrasonic cleaner in step 1 is 200W~600W, carry out the ultrasound temperature of ultrasonic disperse Spend for 20 DEG C~40 DEG C, the time of ultrasonic disperse is 12h~24h.
Sulphur source in step 2 is thiocarbamide or Cys.
The amount that the material for adding sulphur source is given in middle interstitial fluid in step 2 be 1mmol~10mmol, mixing time for 5min~ 30min。
Polytetrafluoroethylene (PTFE) hydro-thermal liner packing ratio in step 3 is 50~70%.
The temperature of hydro-thermal reaction in step 3 is 120~200 DEG C, and the time of hydro-thermal reaction is 12h~36h.
Reactant after cooling is washed with deionized water and absolute ethyl alcohol in step 4.
Freeze-drying temperature in step 4 is -20~-50 DEG C, and sublimation drying is 24h~48h.
Stirring uses magnetic stirring apparatus in step 2, and speed of agitator is 500~800r/min.
The invention has the advantages that the present invention by control molybdenum trioxide, graphene, sulphur source quality, control simultaneously Hydrothermal temperature and time and the mixing time of each step, obtain a kind of molybdenum disulfide/graphene aerogel electrode material, this Electrode material has preferable elastic performance, and with electrical conductivity and thermal conductivity well, available for flexible battery.
The preparation method of the present invention is simple and environmentally-friendly, controllable, is easy to industrialized production, obtained molybdenum disulfide-graphene gas Gel rubber material novel and unique, great novelty.
Brief description of the drawings
Fig. 1 is prepared by a kind of molybdenum disulfide-graphene aerogel electrode material preparation method embodiment 1 of the present invention The XRD spectrum of molybdenum disulfide/graphene aerogel electrode material；
Fig. 2 is prepared by a kind of molybdenum disulfide-graphene aerogel electrode material preparation method embodiment 3 of the present invention The SEM photograph of molybdenum disulfide/graphene aerogel electrode material；
Fig. 3 is prepared by a kind of molybdenum disulfide-graphene aerogel electrode material preparation method embodiment 6 of the present invention The constant current charge-discharge test figure of molybdenum disulfide/graphene aerogel electrode material.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of molybdenum disulfide-graphene aerogel electrode material preparation method of the present invention, it is specifically real according to following steps Apply：
Step 1, molybdenum trioxide and graphene oxide are added in a certain amount of distilled water, and surpassed using ultrasonic cleaner Sound disperses and it is uniformly obtained middle interstitial fluid；Wherein, the amount of the material of molybdenum trioxide is 1mmol~10mmol in middle interstitial fluid, oxygen The quality of graphite alkene is 10mg~50mg, and the volume of distilled water is 200mL~500mL, and used ultrasonic cleaner is 200W~600W ultrasonic cleaner, the ultrasonic temperature for carrying out ultrasonic disperse is 20 DEG C~40 DEG C, and the time of ultrasonic disperse is 12h~24h.
Step 2, it is 1mmol~10mmol thiocarbamides or L- half to the amount that material is added in the middle interstitial fluid obtained through step 1 Cystine, magnetic stirring apparatus, speed of agitator are 500~800r/min, and stirring 5min~30min is mixed to being well mixed Liquid；
Step 3, by step 2 obtain mixed liquor is transferred to packing ratio be 50~70% be in polytetrafluoroethylene (PTFE) hydro-thermal Lining, and be put into baking oven, hydro-thermal reaction 12h~36h at a temperature of 120~200 DEG C, it is after reaction terminates, reactant is natural It is cooled to room temperature；
Step 4, reactant after cooling wash simultaneously precipitation and separation with deionized water and absolute ethyl alcohol, will be isolated Precipitation take out and under vacuum, freeze-drying temperature be -20~-50 DEG C, freeze-drying freeze-drying temperature for 24h~ 48h, obtain molybdenum disulfide-graphene aerogel electrode material.
Embodiment 1
2mmol molybdenum trioxides and 10mg graphene oxides are added in 300mL distilled water, are in ultrasonic power 300W, under the conditions of ultrasonic temperature is 25 DEG C, scattered 12h simultaneously makes it uniformly obtain middle interstitial fluid；Again 1mmol sulphur is added to middle interstitial fluid Urea stirs 30min in the case where rotating speed is 700r/min to being well mixed, and obtains mixed liquor；Mixed liquor is transferred to polytetrafluoroethylene (PTFE) water Hot liner is simultaneously put into baking oven, packing ratio 60%, the hydro-thermal reaction 24h at a temperature of 180 DEG C, and reaction naturally cools to after terminating Room temperature, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation, isolated precipitation is taken out and in vacuum Under the conditions of be freeze-dried, cryogenic temperature be -40 DEG C, cooling time 24h, obtain molybdenum disulfide/graphene aerogel electrode material Material.
Embodiment 2
3mmol molybdenum trioxides and 20mg graphene oxides are added in 300mL distilled water, are in ultrasonic power 300W, under the conditions of ultrasonic temperature is 25 DEG C, ultrasonic disperse 12h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 2mmol thiocarbamides stir 30min in the case where rotating speed is 700r/min to being well mixed, and obtain mixed liquor；Mixed liquor is transferred to poly- four PVF hydro-thermal liner is simultaneously put into baking oven, packing ratio 60%, the hydro-thermal reaction 24h at a temperature of 180 DEG C, reacts after terminating certainly Room temperature so is cooled to, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation, isolated precipitation is taken out And be freeze-dried under vacuum, cryogenic temperature is -40 DEG C, cooling time 24h, obtains molybdenum disulfide/graphene airsetting Gel electrode material.
Embodiment 3
6mmol molybdenum trioxides and 30mg graphene oxides are added in 300mL distilled water, are in ultrasonic power 300W, under the conditions of ultrasonic temperature is 25 DEG C, ultrasonic disperse 12h simultaneously makes it uniformly obtain middle interstitial fluid；Give in middle interstitial fluid and add again 2mmol thiocarbamides, 30min is stirred in the case where rotating speed is 700r/min to being well mixed, obtains mixed liquor；Mixed liquor is transferred to poly- four PVF hydro-thermal liner is simultaneously put into baking oven, packing ratio 60%, the hydro-thermal reaction 18h at a temperature of 200 DEG C, reacts after terminating certainly Room temperature so is cooled to, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation, isolated precipitation is taken out And be freeze-dried under vacuum, cryogenic temperature is -40 DEG C, cooling time 24h, obtains molybdenum disulfide/graphene airsetting Gel electrode material.
Embodiment 4
3mmol molybdenum trioxides and 40mg graphene oxides are added in 300mL distilled water, are in ultrasonic power 300W, under the conditions of ultrasonic temperature is 25 DEG C, ultrasonic disperse 12h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 3mmol Cys, 30min is stirred in the case where rotating speed is 700r/min to being well mixed, obtains mixed liquor；Mixed liquor is turned Move to polytetrafluoroethylene (PTFE) hydro-thermal liner and be put into baking oven, packing ratio 60%, the hydro-thermal reaction 24h at a temperature of 180 DEG C, reaction Room temperature is naturally cooled to after end, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation will be isolated Precipitation is taken out and is freeze-dried under vacuum, and cryogenic temperature is -40 DEG C, cooling time 24h, obtains molybdenum disulfide/stone Black alkene gas gel electrode material.
Embodiment 5
5mmol molybdenum trioxides and 40mg graphene oxides are added in 300mL distilled water, are in ultrasonic power 300W, under the conditions of ultrasonic temperature is 25 DEG C, ultrasonic disperse 12h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 3mmol Cys, 30min is stirred in the case where rotating speed is 700r/min to being well mixed, obtains mixed liquor；Mixed liquor is turned Move to polytetrafluoroethylene (PTFE) hydro-thermal liner and be put into baking oven, packing ratio 60%, the hydro-thermal reaction 18h at a temperature of 200 DEG C, reaction Room temperature is naturally cooled to after end, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation will be isolated Precipitation is taken out and is freeze-dried under vacuum, and cryogenic temperature is -40 DEG C, cooling time 24h, obtains molybdenum disulfide/stone Black alkene gas gel electrode material.
Embodiment 6
2mmol molybdenum trioxides and 40mg graphene oxides are added in 300mL distilled water, are in ultrasonic power 300W, under the conditions of ultrasonic temperature is 25 DEG C, ultrasonic disperse 12h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 5mmol Cys, 30min is stirred in the case where rotating speed is 700r/min to being well mixed, obtains mixed liquor；Mixed liquor is turned Move to polytetrafluoroethylene (PTFE) hydro-thermal liner and be put into baking oven, packing ratio 60%, the hydro-thermal reaction 18h at a temperature of 200 DEG C, reaction Room temperature is naturally cooled to after end, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation will be isolated Precipitation is taken out and is freeze-dried under vacuum, and cryogenic temperature is -40 DEG C, cooling time 24h, obtains molybdenum disulfide/stone Black alkene gas gel electrode material.
Embodiment 7
1mmol molybdenum trioxides and 30mg graphene oxides are added in 200mL distilled water, are in ultrasonic power 200W, under the conditions of ultrasonic temperature is 20 DEG C, ultrasonic disperse 18h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 1mmol Cys, 5min is stirred in the case where rotating speed is 500r/min to being well mixed, obtains mixed liquor；Mixed liquor is shifted To polytetrafluoroethylene (PTFE) hydro-thermal liner and baking oven is put into, packing ratio 70%, the hydro-thermal reaction 36h at a temperature of 120 DEG C, reaction knot Room temperature is naturally cooled to after beam, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation will be isolated heavy Form sediment and take out and be freeze-dried under vacuum, cryogenic temperature is -20 DEG C, cooling time 48h, obtains molybdenum disulfide/graphite Alkene gas gel electrode material.
Embodiment 8
10mmol molybdenum trioxides and 30mg graphene oxides are added in 500mL distilled water, are in ultrasonic power 400W, under the conditions of ultrasonic temperature is 30 DEG C, ultrasonic disperse 24h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 10mmol Cys, 25min is stirred in the case where rotating speed is 800r/min to being well mixed, obtains mixed liquor；Mixed liquor is turned Move to polytetrafluoroethylene (PTFE) hydro-thermal liner and be put into baking oven, packing ratio 70%, the hydro-thermal reaction 24h at a temperature of 200 DEG C, reaction Room temperature is naturally cooled to after end, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation will be isolated Precipitation is taken out and is freeze-dried under vacuum, and cryogenic temperature is -50 DEG C, cooling time 36h, obtains molybdenum disulfide/stone Black alkene gas gel electrode material.
Embodiment 9
8mmol molybdenum trioxides and 50mg graphene oxides are added in 400mL distilled water, are in ultrasonic power 600W, under the conditions of ultrasonic temperature is 40 DEG C, ultrasonic disperse 24h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 5mmol thiocarbamides, 15min is stirred in the case where rotating speed is 700r/min to being well mixed, obtains mixed liquor；Mixed liquor is transferred to poly- four PVF hydro-thermal liner is simultaneously put into baking oven, packing ratio 50%, the hydro-thermal reaction 36h at a temperature of 200 DEG C, reacts after terminating certainly Room temperature so is cooled to, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation, isolated precipitation is taken out And be freeze-dried under vacuum, cryogenic temperature is -30 DEG C, cooling time 48h, obtains molybdenum disulfide/graphene airsetting Gel electrode material.
Embodiment 10
7mmol molybdenum trioxides and 50mg graphene oxides are added in 500mL distilled water, are in ultrasonic power 500W, under the conditions of ultrasonic temperature is 30 DEG C, ultrasonic disperse 18h, and it is uniformly obtained middle interstitial fluid；Give in middle interstitial fluid and add again 10mmol thiocarbamides, 30min is stirred in the case where rotating speed is 800r/min to being well mixed, obtains mixed liquor；Mixed liquor is transferred to poly- Tetrafluoroethene hydro-thermal liner is simultaneously put into baking oven, packing ratio 70%, the hydro-thermal reaction 36h at a temperature of 200 DEG C, after reaction terminates Room temperature is naturally cooled to, with deionized water and each centrifuge washing of absolute ethyl alcohol 3 times, precipitation and separation, isolated precipitation is taken Go out and be freeze-dried under vacuum, cryogenic temperature is -40 DEG C, cooling time 48h, obtains molybdenum disulfide/graphene gas Gel electrode material.
The molybdenum disulfide that the present invention prepares/graphene aerogel composite is the loose porous honeycomb of sandwich stratiform Shape structure, specific surface area is big, together with molybdenum disulfide is effectively combined with graphene, so as to which the insertion for lithium ion and deintercalation carry For more avtive spots, be advantageous to the storage of lithium ion.This method is simple and environmentally-friendly, is easily manipulated, and obtained composite Novel and unique, strong innovation.

Claims (9)

1. a kind of molybdenum disulfide-graphene aerogel electrode material preparation method, it is characterised in that specifically real according to following steps Apply：
Step 1, molybdenum trioxide and graphene oxide are added in a certain amount of distilled water, and using ultrasonic cleaner ultrasound point Dissipate and it is uniformly obtained middle interstitial fluid；
Step 2, to sulphur source is added in the middle interstitial fluid obtained through step 1, stir to being well mixed, obtain mixed liquor；
Step 3, mixed liquor is transferred to polytetrafluoroethylene (PTFE) hydro-thermal liner by what step 2 obtained, and be put into baking oven, certain At a temperature of the hydro-thermal reaction regular hour, reaction terminate after, reactant is naturally cooled into room temperature；
Step 4, reactant after cooling wash simultaneously precipitation and separation, by isolated precipitation taking-up and under vacuum Freeze-drying, obtains molybdenum disulfide-graphene aerogel electrode material.
2. a kind of molybdenum disulfide according to claim 1-graphene aerogel electrode material preparation method, its feature exist In the amount of the material of molybdenum trioxide is 1mmol~10mmol in the middle interstitial fluid described in step 1, and the amount of graphene oxide is 10mg~50mg, the volume of distilled water is 200mL~500mL.
A kind of molybdenum disulfide according to claim 1-graphene aerogel electrode material preparation method, it is characterised in that The ultrasonic cleaner that ultrasonic cleaner described in step 1 is 200W~600W, the ultrasonic temperature for carrying out ultrasonic disperse are 20 DEG C~40 DEG C, the time of ultrasonic disperse is 12h~24h.
3. a kind of molybdenum disulfide according to claim 1-graphene aerogel electrode material preparation method, its feature exist In the sulphur source described in step 2 is thiocarbamide or Cys.
4. a kind of molybdenum disulfide according to claim 3-graphene aerogel electrode material preparation method, its feature exist In, the amount that the material for adding sulphur source is given in middle interstitial fluid in the step 2 be 1mmol~10mmol, mixing time for 5min~ 30min。
5. a kind of molybdenum disulfide according to claim 1-graphene aerogel electrode material preparation method, its feature exist In the polytetrafluoroethylene (PTFE) hydro-thermal liner packing ratio described in step 3 is 50~70%.
6. a kind of molybdenum disulfide according to claim 1-graphene aerogel electrode material preparation method, its feature exist In the temperature of the hydro-thermal reaction described in step 3 is 120~200 DEG C, and the time of hydro-thermal reaction is 12h~36h.
7. a kind of molybdenum disulfide according to claim 1-graphene aerogel electrode material preparation method, its feature exist In reactant after cooling is washed with deionized water and absolute ethyl alcohol in step 4.
8. a kind of molybdenum disulfide according to claim 1-graphene aerogel electrode material preparation method, its feature exist In the freeze-drying temperature described in step 4 is -20~-50 DEG C, and sublimation drying is 24h~48h.
9. a kind of molybdenum disulfide according to claim 4-graphene aerogel electrode material preparation method, its feature exist In the stirring described in step 2 uses magnetic stirring apparatus, and speed of agitator is 500~800r/min.
CN201710443457.3A 2017-06-13 2017-06-13 A kind of molybdenum disulfide graphene aerogel electrode material preparation method Pending CN107394127A (en)

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CN111268732A (en) * 2020-03-09 2020-06-12 常熟理工学院 Method for preparing molybdenum disulfide graphene aerogel by using low-temperature plasma and product thereof
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