CN106058206A - Composite material of flower-like carbon-loaded MoS2 nanoparticles and preparation method and application thereof - Google Patents

Composite material of flower-like carbon-loaded MoS2 nanoparticles and preparation method and application thereof Download PDF

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CN106058206A
CN106058206A CN201610625215.1A CN201610625215A CN106058206A CN 106058206 A CN106058206 A CN 106058206A CN 201610625215 A CN201610625215 A CN 201610625215A CN 106058206 A CN106058206 A CN 106058206A
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flower
carbon
nano
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composite material
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王雄伟
武培怡
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Fudan 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
    • 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 belongs to the field of energy storing materials, in particular to a composite material for flower-like carbon-loaded MoS2 nanoparticles and a preparation method and application thereof. The preparation method comprises the following steps: performing high-temperature thermal treatment and acid etching by taking flower-like ZnO as a template and taking biomass as a precursor through a simple hydrothermal method to obtain a flower-like carbon substrate; performing solvent thermal treatment on flower-like carbon and ammonium tetrathiomolybdate to obtain the composite material in which the MoS2 nanoparticles are uniformly loaded on the flower-like carbon. The prepared composite material has high energy storing capacity, superior cycling stability and superior rate capability when being taken as a negative electrode material of a lithium battery. Biomass with a wide source is taken as the flower-like precursor, and a hydrothermal and solvent-thermal two-step method is adopted; the composite material has the advantage of easiness in operation, low production cost, low environmental pollution, easiness in bath production and large-scale production, good industrial production basis and wide application prospect.

Description

A kind of flower-shaped carbon load MoS2Composite of nano-particle and preparation method thereof and Application
Technical field
The invention belongs to energy storage material technical field, be specifically related to a kind of lithium cell cathode material and preparation method thereof and answer With.
Background technology
In the past ten years, the fast development of wearable electronic and electric automobile causes having high energy storage appearance The wilderness demand of the lithium battery material of amount and excellent cycling stability.And the theoretical stored energy capacitance of traditional commercial graphite electrode is only It is 372 mAh g-1, it is very difficult to meet the energy storage demand quickly increased.Recently, molybdenum bisuphide is as one typical sulfur family mistake Cross metallic compound to be paid close attention to widely owing to it has special two-dimentional S-Mo-S three-decker.Molybdenum bisuphide is further It is stacked by weak Van der Waals force by these two-dimensional slice, and the distance between lamella is significantly larger than graphite electrode (0.65 nm), the intercalation being therefore highly suitable for lithium ion stores.Theoretical Calculation think molybdenum bisuphide theoretical capacity up to 670 mAh g-1But, owing to electrical conductivity is poor present in charge and discharge process and the problem such as easy reunion makes their circulation Stability and high rate performance are the most unsatisfactory.
For solving these problems, substantial amounts of research is mainly devoted to carry out nano molybdenum disulfide with various conducting bases It is combined and obtains nano composite material.The electric charge that these conducting bases are possible not only to strengthen between nano molybdenum disulfide and collector turns Shifting can also effectively suppress the reunion of molybdenum bisuphide in charge and discharge process and buffer the change in volume that it is big.Wherein Graphene The material with carbon element of base is wherein to use most conducting bases, and this is owing to graphene-based conducting base typically has high electronics Conductivity, good flexibility and high chemical stability.Therefore, the composite of a large amount of molybdenum bisuphide-graphene-based carbon base body, Such as by nano molybdenum disulfide particulate load to graphene aerogel (ACS appl. Mater. Interfaces, 2016, 8,3320), grapheme foam (Adv. Funct. Mater., 2013,23,5326), CNT (ACS appl. Mater. Interfaces, 2016,8,1398) and graphene paper (Nanoscale, 2016,8,8042) is by greatly Amount ground report.
Although conductive carbon matrix based on Graphene or the various structures of CNT is widely used for loading two in situ Molybdenum sulfide, but the operation of the preparation process of these Graphene derivative is complex, relatively costly, and due to strong acid Strong oxdiative The use of agent also can pollute the environment of surrounding.Because a kind of method developing flexibility is to have very much to prepare carbon matrix material Significant.Recently, biomass are subject in terms of preparing material with carbon element as a kind of reproducible and nature rich content resource Arrive increasing concern.Hydro-thermal method is a kind of method using widest these biomass of conversion, because this method Low cost, environmental friendliness and easily operated.By can be further to the at high temperature heat treatment of the biomass after hydrothermal carbonization Accelerate carbonization and the graphitization of hydro-thermal carbon, thus significantly improve the electric conductivity of material.Previous work has shown that biomass-based The compound chemical property that can be effectively improved molybdenum bisuphide of material with carbon element and nano molybdenum disulfide.Such as Luo etc. synthesize Carbon ball surface in situ in G/W thermosetting grows the composite of molybdenum disulfide nano sheet, and they find the introducing of carbon ball The cyclical stability (Chem. Eur. J., 2014,20,5219) of molybdenum bisuphide can be significantly improved.In addition the report such as cao Road flower-like structure molybdenum bisuphide surface in situ be coated with one layer of glucosyl group carbon-coating can also improve molybdenum bisuphide lithium storage Sustainability energy (J. Mater. Chem. A, 2014,2,7862).But still there are some if these work and limit, than Such as insufficient electric charge transfer, limited material and the contact area of electrolyte.Construct the structure of 3-dimensional multi-layered time by large quantities Experiment proves a kind of available strategy solving the problems referred to above.
This work is based on this thought to prepare nanometer MOS 2 particle growth in situ on flower-shaped material with carbon element Composite.First we utilize zinc oxide as hard template by carrying out hydrothermal treatment consists with glucose and and combining high annealing With the flower-shaped carbon base body that acid etch obtains porous.Recycling solvent-thermal method is received at flower-shaped carbon base body surface in situ growth molybdenum bisuphide Rice grain, obtains final nano composite material.Due to unique three-dimensional flower-shaped structure, FC-MoS2 composite is used as lithium electricity The negative material in pond has higher reversible capacity (at 0.2A g-1Under electric current density, the capacity of the second circle circulation is 1033 mAh g-1), (circulate the capacity after 50 times is 958 mAh g to excellent cyclical stability-1) and good high rate performance.
Summary of the invention
It is an object of the invention to provide the flower-shaped carbon load MoS that a kind of low cost, environmental friendliness and energy-storage property are excellent2 Nano composite material of nano-particle and its preparation method and application.
The MoS that the present invention provides2Nano-particle is supported on the nano composite material on flower-shaped carbon, is to be existed by solvent-thermal method Flower-shaped carbon surface growth in situ MoS2Nano-particle.The introducing of the flower-shaped carbon of conduction, is possible not only to be effectively improved the electronics of material Transmission capacity, it is also possible to suppression MoS2Reunion and expand and the contact area of electrolyte, thus obtain good energy storage effect.
The flower-shaped carbon load MoS that the present invention provides2The nano composite material preparation method of nano-particle, concretely comprises the following steps:
(1) the flower-shaped ZnO of 50 ~ 500 mg synthesis is dispersed in 5 ~ 20 ml deionized waters, ultrasonic 5 ~ 20 min, is subsequently adding Certain biomass of 50 ~ 500 mg, ultrasonic 5 ~ 15 min；Then mixed liquor is transferred in autoclave pressure, be placed in 120 ~ 250 DEG C of bakings Case reacts 8 ~ 24 h；After naturally cooling to room temperature, product taking-up dehydrated alcohol is centrifuged repeatedly washing 3 ~ 8 times；Subsequently Product is placed in 2-24 h in 50 ~ 150 DEG C of baking ovens dry, powdered；
(2) powder taking 0.1 ~ 1.0 g drying is placed in tube furnace, under nitrogen protection with the heating rate of 2 ~ 10 DEG C/min It is heated to 400 ~ 1000 DEG C, is incubated 1 ~ 5 h；It is cooled to room temperature under gas shield；Then by the material after heat treatment with 0.5 ~ 5 M HCl processes 0.5-6 h, then by deionized water and ethanol eccentric cleaning repeatedly, dries, obtain flower-shaped in 50 ~ 150 DEG C of baking ovens Carbon；
(3) weighing 5 ~ 50mg four thio ammonium molybdate and join in 10 ml solvents, ultrasonic 5 ~ 60 min make four thio ammonium molybdate abundant Dissolve；Being subsequently adding 2 ~ 20 flower-shaped carbon of mg, ultrasonic 10 ~ 120 min help dispersion；Add 0.1 ~ 1.0 ml mono-hydrazine hydrate, subsequently Mixed liquor is transferred in autoclave pressure, be placed in 100 ~ 250 DEG C of baking ovens reaction 6 ~ 24 h；After naturally cooling to room temperature, will material Liquid takes out uses deionized water centrifuge washing 3 ~ 10 times；Then product is placed in 30 ~ 120 DEG C of vacuum drying ovens after 2 ~ 24 h drying, Heat treatment 1 ~ 5 h under nitrogen is protected in the tube furnace of 500 ~ 800 DEG C again, obtains final flower-shaped carbon load MoS2Nano-particle Composite.
In the present invention, biomass used in step (1) are the one in cellulose, glucose, chitosan, or the most several The mixture planted；
In the present invention, solvent used in step (3) is the one in DMF, acetone, oxolane, or its In several mixed solvent.
MoS prepared by the present invention2Nano-particle is supported on the nano composite material on flower-shaped carbon, is by simple hydro-thermal Realize with solvent thermal two-step method.First with biomass as carbon matrix precursor, with flower-shaped ZnO as template, by hydro-thermal method and subsequently High annealing and acid etch obtain three-dimensional porous flower-shaped carbon.The most again with flower-shaped carbon as substrate, by with tetrathio molybdic acid The solvent heat treatment of ammonium obtains flower-shaped carbon load MoS2The composite of nano-particle.This material is as the negative pole material of lithium battery Material, shows good excellent electrochemical energy storage performance: have higher reversible capacity, excellent cyclical stability, high electricity Stream toleration and recovery.This is owing to the introducing of flower-shaped carbon is possible not only to the electronic conduction ability of reinforcing material, the most also may be used Effectively to suppress MoS2Reunion and expand and the contact area of electrolyte.This alienation shape carbon and MoS2Between strong interaction Can also effectively buffer MoS2Structural stress big in charge and discharge process.
The present invention is easy to operate, and preparation condition is simple, and production cost is low, relatively environmental protection, it is easy to mass, large-scale production, There is the application prospect that good industrialized production is basic and wide.
Accompanying drawing explanation
Fig. 1. the scanning electron microscope (SEM) photograph (a) of flower-shaped carbon and transmission electron microscope picture (b).
Fig. 2. add the flower-shaped carbon load MoS that 22 mg four thio ammonium molybdates obtain2The scanning of nano particle composite material Electronic Speculum figure.
Fig. 3. add the flower-shaped carbon load MoS that 22 mg four thio ammonium molybdates obtain2The transmission of nano particle composite material Electronic Speculum figure.
Fig. 4. add the flower-shaped carbon load MoS that 22 mg four thio ammonium molybdates obtain2Nano particle composite material and pure MoS2At 200 mA g-1Under the cycle performance of discharge and recharge.
Fig. 5. add the flower-shaped carbon load MoS that 22 mg four thio ammonium molybdates obtain2Nano particle composite material is in difference The high rate performance of discharge and recharge under electric current density.
Fig. 6. the pure MoS that four thio ammonium molybdate solvent thermal obtains2Scanning electron microscopy (a) and transmission electron microscopy Figure (b).
Fig. 7. add the flower-shaped carbon load MoS that 10 mg four thio ammonium molybdates obtain2The scanning of nano particle composite material Electronic Speculum figure (a) and transmission electron microscope picture (b).
Fig. 8. add the flower-shaped carbon load MoS that 40 mg four thio ammonium molybdates obtain2The scanning of nano particle composite material Electronic Speculum figure (a) and transmission electron microscope picture (b).
Detailed description of the invention
Further describe the present invention flower-shaped carbon load MoS by the following examples2The system of nano particle composite material Preparation Method and catalytic activity of hydrogen evolution thereof, this embodiment is merely possible to provide explanation rather than limit the present invention.
Embodiment 1
(1) the flower-shaped ZnO of 100 mg synthesis is dispersed in 10 ml deionized waters, ultrasonic 20 min, is subsequently adding 100 mg Glucose, ultrasonic 10 min；Then mixed liquor is transferred in pressure good fortune still, be placed in 180 DEG C of baking ovens and react 12 h；Treat nature After being cooled to room temperature, product taking-up dehydrated alcohol is centrifuged repeatedly washing 5 times；Subsequently product is placed in 6 h in 60 DEG C of baking ovens Dry.
(2) powder taking 1.0 g drying is placed in tube furnace, heats with the heating rate of 5 DEG C/min under nitrogen protection It is incubated 2 h at 800 DEG C；Finally under gas shield, it is cooled to room temperature.Then by the material after heat treatment with 2 M HCl process 1 h, then uses deionized water and ethanol eccentric cleaning repeatedly, dries, obtain flower-shaped carbon in 60 DEG C of baking ovens.
(3) weighing 22 mg four thio ammonium molybdates and join in 10 ml DMF, ultrasonic 10 min make four thio ammonium molybdate fill Divide and dissolve；Being subsequently adding the 10 flower-shaped carbon of mg, ultrasonic 30 min help dispersion；Add 0.1 ml mono-hydrazine hydrate, subsequently by mixed liquor Transfer in autoclave pressure, be placed in 200 DEG C of baking ovens and react 18 h；After naturally cooling to room temperature, by feed liquid taking-up deionization Water centrifuge washing 6 times；Then product is placed in 60 DEG C of vacuum drying ovens after 6 h drying, then nitrogen in the tube furnace of 500 DEG C Lower heat treatment 2 h of protection, obtains final flower-shaped carbon load MoS2Nano particle composite material.
The most flower-shaped carbon presents three dimensional structure, and containing some big holes.Warp and 22 mg four thio ammonium molybdates By the scanning electron microscopy in Fig. 2 it can be seen that the certain uniform load of flower-shaped carbon surface has substantial amounts of MoS after solvent heat treatment2 Nano-particle.Transmission electron microscope figure in Fig. 3 further demonstrates flower-shaped carbon surface MoS2The load of nano-particle, and have High-resolution transmission plot is it can be seen that MoS2Small-sized (less than 10 nm) of crystal, and and matrix between have preferably Interact.From the charge and discharge cycles stability diagram of Fig. 4 it can be seen that add the lithium electrical feature capacity of the composite of flower-shaped carbon It is intended to be significantly higher than pure MoS with cyclical stability2Nano-particle, illustrates that flower-shaped carbon can improve MoS2Electrochemical energy storage Energy.Fig. 5 shows that the composite adding flower-shaped carbon has more excellent high electric current toleration further, simultaneously returns to low current Time also there is extraordinary capacity recovery.
Embodiment 2
Weighing 40 mg four thio ammonium molybdates and join in 10 ml DMF, ultrasonic 10 min make four thio ammonium molybdate fully dissolve； Add 0.1 ml mono-hydrazine hydrate, subsequently mixed liquor is transferred in autoclave pressure, be placed in 200 DEG C of baking ovens and react 18 h；Treat nature After being cooled to room temperature, by feed liquid taking-up deionized water centrifuge washing 6 times；Then product is placed in 6 h in 60 DEG C of vacuum drying ovens After drying, then in the tube furnace of 500 DEG C nitrogen protection under heat treatment 2 h, obtain final MoS2Nano-particle liberation of hydrogen is catalyzed Material.
As seen from Figure 6, four thio ammonium molybdate self solvent thermal obtains nano flower-like structure.
Embodiment 3
(1) the flower-shaped ZnO of 100 mg synthesis is dispersed in 10 ml deionized waters, ultrasonic 20 min, is subsequently adding 100 mg Glucose, ultrasonic 10 min；Then mixed liquor is transferred in pressure good fortune still, be placed in 180 DEG C of baking ovens and react 24 h；Treat nature After being cooled to room temperature, product taking-up dehydrated alcohol is centrifuged repeatedly washing 5 times；Subsequently product is placed in 6 h in 60 DEG C of baking ovens Dry.
(2) powder taking 1.0 g drying is placed in tube furnace, heats with the heating rate of 5 DEG C/min under nitrogen protection It is incubated 2 h at 800 DEG C；Finally under gas shield, it is cooled to room temperature.Then by the material after heat treatment with 2 M HCl process 1 h, then uses deionized water and ethanol eccentric cleaning repeatedly, dries, obtain flower-shaped carbon in 60 DEG C of baking ovens.
Embodiment 4
(1) the flower-shaped ZnO of 100 mg synthesis is dispersed in 10 ml deionized waters, ultrasonic 20 min, is subsequently adding 100 mg Glucose, ultrasonic 10 min；Then mixed liquor is transferred in pressure good fortune still, be placed in 180 DEG C of baking ovens and react 24 h；Treat nature After being cooled to room temperature, product taking-up dehydrated alcohol is centrifuged repeatedly washing 5 times；Subsequently product is placed in 6 h in 60 DEG C of baking ovens Dry.
(2) powder taking 1.0 g drying is placed in tube furnace, heats with the heating rate of 5 DEG C/min under nitrogen protection It is incubated 2 h at 800 DEG C；Finally under gas shield, it is cooled to room temperature.Then by the material after heat treatment with 2 M HCl process 1 h, then uses deionized water and ethanol eccentric cleaning repeatedly, dries, obtain flower-shaped carbon in 60 DEG C of baking ovens.
(3) weighing 10 mg four thio ammonium molybdates and join in 10 ml DMF, ultrasonic 10 min make four thio ammonium molybdate fill Divide and dissolve；Being subsequently adding the 10 flower-shaped carbon of mg, ultrasonic 30 min help dispersion；Add 0.1 ml mono-hydrazine hydrate, subsequently by mixed liquor Transfer in autoclave pressure, be placed in 200 DEG C of baking ovens and react 18 h；After naturally cooling to room temperature, by feed liquid taking-up deionization Water centrifuge washing 6 times；Then product is placed in 60 DEG C of vacuum drying ovens after 6 h drying, then nitrogen in the tube furnace of 500 DEG C Lower heat treatment 2 h of protection, obtains final MoS2Nano-particle and the composite of flower-shaped carbon.
It will be seen in fig. 7 that add the composite that obtains of 10 mg four thio ammonium molybdates it can be seen that MoS2Nano-particle It is distributed in flower-shaped carbon surface sparsely.
Embodiment 5
(1) the flower-shaped ZnO of 100 mg synthesis is dispersed in 10 ml deionized waters, ultrasonic 20 min, is subsequently adding 100 mg Glucose, ultrasonic 10 min；Then mixed liquor is transferred in pressure good fortune still, be placed in 180 DEG C of baking ovens and react 24 h；Treat nature After being cooled to room temperature, product taking-up dehydrated alcohol is centrifuged repeatedly washing 5 times；Subsequently product is placed in 6 h in 60 DEG C of baking ovens Dry.
(2) powder taking 1.0 g drying is placed in tube furnace, heats with the heating rate of 5 DEG C/min under nitrogen protection It is incubated 2 h at 800 DEG C；Finally under gas shield, it is cooled to room temperature.Then by the material after heat treatment with 2 M HCl process 1 h, then uses deionized water and ethanol eccentric cleaning repeatedly, dries, obtain flower-shaped carbon in 60 DEG C of baking ovens.
(3) weighing 40 mg four thio ammonium molybdates and join in 10 ml DMF, ultrasonic 10 min make four thio ammonium molybdate fill Divide and dissolve；Being subsequently adding the 10 flower-shaped carbon of mg, ultrasonic 30 min help dispersion；Add 0.1 ml mono-hydrazine hydrate, subsequently by mixed liquor Transfer in autoclave pressure, be placed in 200 DEG C of baking ovens and react 18 h；After naturally cooling to room temperature, by feed liquid taking-up deionization Water centrifuge washing 6 times；Then product is placed in 60 DEG C of vacuum drying ovens after 6 h drying, then nitrogen in the tube furnace of 500 DEG C Lower heat treatment 2 h of protection, obtains final flower-shaped carbon load MoS2Nano particle composite material.
As seen from Figure 8, composite that 40 mg four thio ammonium molybdates obtain is added it can be seen that exist a large amount of free MoS2Nano flower-like structure, and MoS2There is serious agglomeration.

Claims (5)

1. a flower-shaped carbon load MoS in situ2The preparation method of the composite of nano-particle, it is characterised in that concretely comprise the following steps:
(1) the flower-shaped ZnO of 50 ~ 500 mg synthesis is dispersed in 5 ~ 20 ml deionized waters, ultrasonic 5 ~ 20 min, is subsequently adding 50 ~ 500 mg biomass, ultrasonic 5 ~ 15 min；Then mixed liquor is transferred in autoclave pressure, be placed in 120 ~ 250 DEG C of baking ovens Reaction 8 ~ 24 h；After naturally cooling to room temperature, product is taken out, is centrifuged repeatedly washing 3 ~ 8 times with dehydrated alcohol；To produce subsequently Thing is placed in 2-24 h in 50 ~ 150 DEG C of baking ovens and dries；
(2) powder taking 0.1 ~ 1.0 g drying is placed in tube furnace, under nitrogen protection with the heating rate of 2 ~ 10 DEG C/min It is heated to 400 ~ 1000 DEG C, is incubated 1 ~ 5 h；It is cooled to room temperature under nitrogen protection；By material after heat treatment with 0.5 ~ 5 M HCl processes 0.5-6 h, then uses deionized water and ethanol eccentric cleaning repeatedly, dries, obtain flower-shaped in 50 ~ 150 DEG C of baking ovens Carbon；
(3) weighing 5 ~ 50mg four thio ammonium molybdate and join in 10 ml solvents, ultrasonic 5 ~ 60 min make four thio ammonium molybdate abundant Dissolve；Being subsequently adding 2 ~ 20 flower-shaped carbon of mg, ultrasonic 10 ~ 120 min help dispersion；Add 0.1 ~ 1.0 ml mono-hydrazine hydrate, subsequently Mixed liquor is transferred in autoclave pressure, be placed in 100 ~ 250 DEG C of baking ovens reaction 6 ~ 24 h；After naturally cooling to room temperature, will material Liquid takes out, with deionized water centrifuge washing 3 ~ 10 times；Then product is placed in 2 ~ 24 h in 30 ~ 120 DEG C of vacuum drying ovens dry, then Heat treatment 1 ~ 5 h under nitrogen protection in the tube furnace of 500 ~ 800 DEG C, obtains final flower-shaped carbon load MoS2Nano-particle is multiple Condensation material.
Preparation method the most according to claim 1, it is characterised in that biomass used in step (1) are cellulose, Portugal One in grape sugar, chitosan, or the most several mixture.
Preparation method the most according to claim 1, it is characterised in that solvent used in step (3) is N, N-dimethyl One in Methanamide, acetone, oxolane, or the most several mixed solvents.
4. the flower-shaped carbon that one kind is prepared by one of claim 1-3 preparation method load MoS in situ2Being combined of nano-particle Material.
Flower-shaped carbon the most as claimed in claim 4 load MoS2The composite of nano-particle answering as lithium cell cathode material With.
CN201610625215.1A 2016-08-03 2016-08-03 Composite material of flower-like carbon-loaded MoS2 nanoparticles and preparation method and application thereof Pending CN106058206A (en)

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Application publication date: 20161026