CN109904395A - A kind of molybdenum disulfide-graphene composite material - Google Patents

A kind of molybdenum disulfide-graphene composite material Download PDF

Info

Publication number
CN109904395A
CN109904395A CN201711294243.0A CN201711294243A CN109904395A CN 109904395 A CN109904395 A CN 109904395A CN 201711294243 A CN201711294243 A CN 201711294243A CN 109904395 A CN109904395 A CN 109904395A
Authority
CN
China
Prior art keywords
graphene
preparation
composite material
molybdenum disulfide
graphene oxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711294243.0A
Other languages
Chinese (zh)
Inventor
郭金
张会成
王少军
凌凤香
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Sinopec Dalian Research Institute of Petroleum and Petrochemicals
Original Assignee
China Petroleum and Chemical Corp
Sinopec Dalian Research Institute of Petroleum and Petrochemicals
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Petroleum and Chemical Corp, Sinopec Dalian Research Institute of Petroleum and Petrochemicals filed Critical China Petroleum and Chemical Corp
Priority to CN201711294243.0A priority Critical patent/CN109904395A/en
Publication of CN109904395A publication Critical patent/CN109904395A/en
Pending legal-status Critical Current

Links

Classifications

    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

A kind of molybdenum disulfide-graphene composite material, is prepared by the following method: sulphur powder, molybdenum salt and graphene oxide 1:1-10:1-10 in mass ratio being mixed, is placed in ball mill and is ground;Material after ball milling is placed in microwave reaction chamber, with the heats 10-60min of 300-1000W, obtains the molybdenum disulfide-graphene composite material.Molybdenum disulfide-graphene composite material prepared by the present invention is under solvent-free microwave heating condition, and graphene oxide is heat-treated as graphene, the MoS of generation2Nanometer sheet directly upper growth in situ on the surface of graphene, microwave heating speed is fast, homogeneous heating, so that MoS2Nanometer sheet is firmly combined with graphene, and does not easily cause particle packing, the time needed for greatly shortening synthetic material and alleviates graphene and MoS2The problem of reuniting in long-term heated situation.Above-mentioned composite material shows good cyclical stability and high rate performance as lithium ion battery negative material.

Description

A kind of molybdenum disulfide-graphene composite material
Technical field
The present invention relates to a kind of molybdenum disulfide-graphene hierarchical structure lithium cell cathode materials, and provide preparation method, Belong to nanocomposite and its applied technical field.
Background technique
Lithium ion battery is widely used in hand due to its high-energy density, high working voltage and longer service life Machine, the modern times such as electric car power storage system.The electrochemical properties of negative electrode material directly affect the entirety of lithium ion battery Performance.Due to high coulombic efficiency, the advantages that good cyclical stability, nature rich reserves, is widely used in graphite Lithium ion battery negative material.However its lower specific capacity (372mAh g-1) and poor high rate performance be unable to satisfy future The demand of portable equipment and electric car, therefore, urgent need develop the lithium cell cathode material of novel high-performance.
Transient metal chalcogenide compound is an important component in Material Field, due to its special physics, chemistry Property and extensive concern and dense research interest are caused in the application value that every field is dived, and increasingly shown Many unique performances, such as photoelectricity performance, magnetic force performance and superconductivity.Section transitions metal chalcogenides have only Special layer structure, interlayer can introduce otheralkali metal or other atoms.Wherein, MoS2As a kind of typical transition gold Belong to chalcogen compound, there is the layer structure and high theoretical capacity (670 mAh g of similar graphene-1), and it is cheap, surely It is qualitative good, therefore attracted wide attention as a kind of potential high-performance lithium cell negative electrode material.
However MoS2The defects of electric conductivity is poor and cyclical stability is poor hinders its large-scale application.Two-dimensional structure Graphene there is high-specific surface area and excellent electric conductivity, and electrochemical stability is good, so that MoS2/ graphene nano Composite material becomes research hotspot.
CN106207171A, which is provided, a kind of prepares MoS2The method of/graphene nanocomposite material, mainly passes through hydro-thermal Recombination process, the product after hydro-thermal obtain MoS after washing is dry2/ graphene nanocomposite material, by resulting MoS2/ stone Black alkene nanocomposite applications are in lithium cell cathode material, it is shown that more excellent chemical property.But hydro-thermal and molten The hot recombination process of agent generally requires reaction 20h or more there are some problems, such as reaction time are long, be difficult in reaction process by Graphene oxide restores completely, and MoS2It is unstable in conjunction with graphene, the destruction of electrode is easily led in charge and discharge process, Furthermore the product that hydro-thermal obtains also need to be easy to cause by processes such as washing, separation, dryings the accumulation again of graphene to Transmission of the lithium ion in graphene is influenced, and then influences MoS2The chemical property of/graphene nanocomposite material.
Summary of the invention
It is mostly to use hydro-thermal method, or synthesizing to solve molybdenum disulfide-graphene nanocomposite material in the prior art Solvent is needed in journey, the reaction time is generally longer, and product needs complicated separation last handling process, MoS in synthetic material2With stone For black alkene in conjunction with the problem of unstable, charge and discharge easily lead to electrode breakages, the present invention provides a kind of solventless method synthesis of carbon/molybdenum disulfide- The method of graphene composite material, products obtained therefrom are directly available in lithium ion battery anode material without the processes such as washing, separation, dry Material, application performance are good.
To realize the above-mentioned technical purpose, first aspect present invention provides a kind of molybdenum disulfide-graphene composite material Preparation method, comprising the following steps:
Sulphur powder, molybdenum salt and graphene oxide 1:1-10:1-10 in mass ratio are mixed, is placed in ball mill and is ground;Ball Material after mill is placed in microwave reaction chamber, with the heats 10-60min of 300-1000W, obtains the curing Molybdenum-graphene composite material.
In the above preparation method, the power of the microwave reaction is preferably 600 ~ 1000W, and the time is preferably 20 ~ 60min, more preferably 30 ~ 60min.
In the above preparation method, the molybdenum salt is selected from at least one of molybdenum pentachloride, ammonium paramolybdate and sodium molybdate, preferably For ammonium paramolybdate.
In the above preparation method, the mass ratio that feeds intake of mill ball and mixture is 1-20:1 in ball mill when grinding, is turned Speed is 300-3000r/min, milling time 0.5-3h.Mill ball and feed ratio are greater than 1, are conducive to feed intake abundant with mill ball Contact, grinding effect are more preferable.
In the above preparation method, grinding is to carry out under an inert atmosphere.
In the above preparation method, before microwave reaction and in reaction process with nitrogen or inert gas purge microwave reaction Chamber, it is preferred to use argon gas purging.
In the above preparation method, the graphene oxide is especially selected from the graphene oxide having the following properties that: lamella Area is 100 μm2More than, conductivity is 3500S/m or more.
In the above preparation method, the graphene oxide is that graphite is obtained through oxidation, and graphene oxide of the invention is adopted It is synthesized with Hummers method, as more specific embodiment, the present invention discloses the specific preparation method of the graphite oxide such as Under: natural flake graphite is added under agitation into the concentrated sulfuric acid of ice bath, temperature is down to 0-10 DEG C, and sodium nitrate, height is added Potassium manganate is stirred to react, and adds deionized water, is warming up to 50-100 DEG C, isothermal reaction to reaction solution becomes glassy yellow, Xiang Qi Middle addition hydrogen peroxide, is stirred to react, and cooling washs, is dried to obtain graphene oxide, pulverizes spare.
The specification of the natural flake graphite is 100-500 mesh.After completion of the reaction, when post-processing first with deionized water repeatedly Sedimentation removes unreacted graphite particle, then with salt acid centrifuging, cleaning removes the Cl ion in reaction solution, is washed with deionized water To pH value close to neutrality, drying is ground.
Above-mentioned Hummers method charge stripping efficiency is 93% or more, and yield is 90% or more, and gained graphene oxide layer structure is complete Whole degree is high, and lattice is complete after thermal reduction.
The technical purpose of second aspect of the present invention is to provide molybdenum disulfide-graphene composite material of above method preparation, The material is under solvent-free microwave heating condition, and graphene oxide is heat-treated as graphene, the MoS of generation2Nanometer Piece directly goes up growth in situ on the surface of graphene, since microwave heating speed is fast, homogeneous heating, so that MoS2Nanometer sheet and graphite Alkene is firmly combined, and does not easily cause particle packing, the time needed for greatly shortening synthetic material and alleviates graphene And MoS2The problem of reuniting in long-term heated situation.
The technical purpose of third aspect present invention is to provide the application of above-mentioned molybdenum disulfide-graphene composite material, described Material can be used as lithium ion battery negative material, show good cyclical stability and high rate performance.
Compared with the prior art, the present invention has the following advantages:
The present invention prepares molybdenum disulfide-graphene composite material, solvent-free processing side using solvent-free microwave heating method The last handling processes such as the washing, separation and drying of product are omitted in formula, and obtained product can be used directly;Microwave heating speed Fastly, thoroughly, and the aggregately stacked of nano particle in long-term heat treatment process, graphite is effectively relieved in homogeneous heating, graphene reduction Alkene and MoS2It is firmly combined and does not significantly build up, molybdenum disulfide nano sheet is uniformly dispersed on the surface of graphene.Stability of material Good, not mutability, is easy storage in air;Large specific surface area is mentioned as lithium ion battery negative material for lithium ion transport Good channel has been supplied, biggish specific capacity and preferable stable circulation performance are shown.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
Fig. 1 is the XRD diagram of graphene oxide prepared in embodiment 1;
It in current density is 100mAg that Fig. 2, which is molybdenum disulfide-graphene composite material in embodiment 11,-1When charge and discharge follow Ring curve.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with Any mode limits the present invention.
Embodiment 1
The preparation of graphene oxide: the concentrated sulfuric acid of 100mL 98% is taken to be slowly added into the dry there-necked flask of 500mL, Jiang Sankou Bottle ice bath cooling is placed on magnetic stirring apparatus.It quickly is added with stirring 2.0g natural flake graphite (180 mesh), to reaction solution temperature When degree is down to about 0 DEG C, it is slowly added to 4.0g sodium nitrate, continues to stir 2h.Then 10g permanganic acid is slowly added portionwise in 1h Potassium, persistently stirs 2h, and reaction temperature is controlled at 10 DEG C or less.There-necked flask is moved into 40 DEG C of water-baths again, continues to be stirred to react 2h.Then, it is slowly added to 200mL temperature deionized water, reacting liquid temperature is maintained within 100 DEG C.98 DEG C of constant temperature reactions, until anti- Liquid is answered to become glassy yellow.The hydrogen peroxide of 20mL 30% is added into reaction solution, lasting stirring reacts it sufficiently.It, will after cooling Acquired solution replacement deionized water settles repeatedly, removes unreacted graphite particle, with hydrochloric acid eccentric cleaning, removes in reaction solution Cl ion, then be washed with deionized water to pH value close to neutrality.Last 80 DEG C of vacuum drying 12h, obtains graphene oxide, grinding At powdered spare.Its XRD diagram is as shown in Figure 1, be located at 11oLeft and right is typical 001 diffraction maximum of graphene oxide, peak master If caused by being intercalation between graphene sheet layer due to a large amount of oxygen-containing functional groups.Oxidation can be calculated by Scherrer formula Distance is 0.7 nm between graphite flake layer, hence it is evident that greater than 0.3254 nm of interlamellar spacing of graphite.Increased interlamellar spacing mainly due to Caused by being intercalation into the oxygen-containing functional group between graphene sheet layer.
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the matter of 1:3:4 Mixture is placed in the agate pot full of nitrogen by amount than mixing, using ball mill ball milling, the mass ratio of mill ball and mixture For 3:1, after revolving speed 400rpm, ball milling 1h, cooled to room temperature collects product.Material after ball milling is fitted into reaction tube, It is placed in microwave reaction chamber, 1h is purged with the argon gas of 100mL/min.10min is heated with the power microwave of 600W.Under an ar atmosphere It is cooled to room temperature to get molybdenum disulfide-graphene composite material.
Embodiment 2
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:1:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 3: After 1, revolving speed 400rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.10min is heated with the power microwave of 600W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 3
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide/graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 3: After 1, revolving speed 400rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.20min is heated with the power microwave of 600W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 4
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 4: After 1, revolving speed 400rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.20min is heated with the power microwave of 600W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide-graphene composite material
Embodiment 5
The preparation method is the same as that of Example 1 for graphite oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 5: After 1, revolving speed 400rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.40min is heated with the power microwave of 600W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 6
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 5: After 1, revolving speed 600rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.40min is heated with the power microwave of 600W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 7
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 5: After 1, revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.50min is heated with the power microwave of 600W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 8
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 5: After 1, revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.30min is heated with the power microwave of 800W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 9
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 5: After 1, revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.30min is heated with the power microwave of 1000W.It is cooled under an ar atmosphere Room temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 10
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 5: After 1, revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.40min is heated with the power microwave of 1000W.It is cooled under an ar atmosphere Room temperature is to get molybdenum disulfide-graphene composite material.
Embodiment 11
The preparation method is the same as that of Example 1 for graphene oxide
Molybdenum disulfide-graphene composite material preparation: by sulphur powder, ammonium paramolybdate and graphene oxide with the mass ratio of 1:2:4 Mixing, mixture is placed in the agate pot full of nitrogen, and using ball mill ball milling, the mass ratio of mill ball and mixture is 5: After 1, revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, is placed in microwave In reaction chamber, 1h is purged with the argon gas of 100mL/min.50min is heated with the power microwave of 1000W.It is cooled under an ar atmosphere Room temperature is to get molybdenum disulfide-graphene composite material.
Molybdenum disulfide-graphene composite material of embodiment 1 ~ 11 is used for lithium ion battery negative material.With two sulphur of synthesis Change molybdenum-graphene is active component, selects 2016 type battery cases, metal lithium sheet (16 mm of Φ × 1mm), with 1.0M LiPF6's Ethylene carbonate (EC)/diethyl carbonate (DEC) mixed liquor (volume ratio 1:1) is electrolyte, Celgard2300 micropore poly- third Coal film is as battery diaphragm.The above material is assembled into button battery in the glove box full of Ar gas, waits working electrodes quilt Electrolyte is tested again after sufficiently infiltrating.It is specifically divided into following five steps:
(1) it sizes mixing
Material used is since specific surface is larger, the moisture being easy in absorption air, so first having to prepare the material of electrode It is sufficiently dry in 120 DEG C of vacuum oven, remove surface moisture.Then by active material, conductive additive (acetylene black) Dispersing agent is added to according to the proportion of mass percent 80:10:10 with binder (PVDF)NMethyl pyrrolidone (NMP) mixing Grinding, mixes material uniformly, viscous paste is made.
(2) film
Obtained viscous paste is uniformly coated on copper foil (thickness is about 100 μm).Concrete operations are as follows: 1) shearing is good big Small moderate copper foil, and tiled on the table.2) copper foil surface spot is removed.3) slurry is dispersed on copper foil, is used Slurry is uniformly laid on copper foil by mold.4) copper foil for being coated with slurry is dried into 12h in 120 DEG C of vacuum ovens.
(3) it rolls
After drying completely, the copper foil for being coated with slurry is rolled with small-sized roller, to prevent electrode material from copper foil surface It falls off.
(4) tabletting
The film after rolling is cut into several circular electric pole pieces, diameter 12mm with hand microtome.Film is filling in order to prevent It falls off during discharge cycles, tabletting is carried out to it with hydraulic press.Weighing is taken out after drying, to packed battery.
(5) assembled battery
The process for assembling button cell carries out in the glove box full of Ar gas.According to negative battery shell/electrolyte/working electrode Piece/electrolyte/diaphragm/lithium piece/positive battery shell sequence is assembled into battery.It places for 24 hours, liquid to be electrolysed carries out after sufficiently infiltrating Electro-chemical test.
By assembled button-shaped simulated battery, charge-discharge test is carried out.The material of embodiment 11 is in 0.01-3.0V voltage In range, 100mAg-1Current density under cyclical stability test result it is as shown in Fig. 2.Embodiment 1 ~ 11 is filled for the first time Discharge capacity and the discharge capacity after 100 charge-discharge tests are shown in Table 1.
Table 1
Comparative example 1
Using preparation method identical with embodiment 11, the difference is that not using microwave heating, it is exchanged with conventional Muffle furnace 800 DEG C roasting 30min.Ammonium paramolybdate does not react completely as the result is shown, causes molybdenum disulfide-graphene yield less, by resulting materials For lithium cell cathode material, initial discharge capacity only has 525.2mAhg-1

Claims (11)

1. a kind of preparation method of molybdenum disulfide-graphene composite material, comprising the following steps:
Sulphur powder, molybdenum salt and graphene oxide 1:1-10:1-10 in mass ratio are mixed, is placed in ball mill and is ground;Ball Material after mill is placed in microwave reaction chamber, with the heats 10-60min of 300-1000W, obtains the curing Molybdenum-graphene composite material.
2. preparation method according to claim 1, which is characterized in that molybdenum salt is selected from molybdenum pentachloride, ammonium paramolybdate and molybdic acid At least one of sodium.
3. preparation method according to claim 1, which is characterized in that when grinding in ball mill mill ball and mixture throwing Material mass ratio is 1-20:1.
4. preparation method according to claim 1, which is characterized in that milling time 0.5-3h.
5. preparation method according to claim 1, which is characterized in that with nitrogen or lazy before microwave reaction and in reaction process Property gas purge microwave reaction chamber.
6. preparation method according to claim 1, which is characterized in that the graphene oxide is selected from and has the following properties that Graphene oxide: lamella area is 100 μm2More than, conductivity is 3500S/m or more.
7. preparation method according to claim 1, which is characterized in that the graphene oxide is that graphite is obtained through oxidation.
8. preparation method according to claim 7, which is characterized in that the graphene oxide is synthesized using Hummers method, Specifically the preparation method is as follows: natural flake graphite is added under agitation into the concentrated sulfuric acid of ice bath, temperature is down to 0-10 DEG C, Sodium nitrate, potassium permanganate is added, is stirred to react, adds deionized water, is warming up to 50-100 DEG C, isothermal reaction to reaction solution becomes For glassy yellow, hydrogen peroxide is added thereto, is stirred to react, cools down, washs, is dried to obtain graphene oxide, pulverize spare.
9. preparation method according to claim 8, which is characterized in that the specification of the natural flake graphite is 100-500 Mesh.
10. molybdenum disulfide-graphene composite material of the preparation of method described in claim 1 ~ 9 any one.
11. application of the molybdenum disulfide-graphene composite material described in any one of claim 10 as lithium ion battery negative material.
CN201711294243.0A 2017-12-08 2017-12-08 A kind of molybdenum disulfide-graphene composite material Pending CN109904395A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711294243.0A CN109904395A (en) 2017-12-08 2017-12-08 A kind of molybdenum disulfide-graphene composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711294243.0A CN109904395A (en) 2017-12-08 2017-12-08 A kind of molybdenum disulfide-graphene composite material

Publications (1)

Publication Number Publication Date
CN109904395A true CN109904395A (en) 2019-06-18

Family

ID=66940339

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711294243.0A Pending CN109904395A (en) 2017-12-08 2017-12-08 A kind of molybdenum disulfide-graphene composite material

Country Status (1)

Country Link
CN (1) CN109904395A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357162A (en) * 2019-07-22 2019-10-22 金堆城钼业股份有限公司 A method of efficiently synthesizing high pure alcohol
CN110436525A (en) * 2019-07-22 2019-11-12 金堆城钼业股份有限公司 A kind of preparation method of micro-/ nano molybdenum disulfide
CN111302445A (en) * 2020-02-25 2020-06-19 中国科学院东北地理与农业生态研究所 GO/MoS for removing lead ions in water body by electrochemical method2Electrode preparation method
CN111924881A (en) * 2020-07-30 2020-11-13 内蒙古凯金新能源科技有限公司 Molybdenum disulfide battery negative electrode material and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101908628A (en) * 2010-08-18 2010-12-08 天津久聚能源科技发展有限公司 Transition metal composite oxide catalytic material and microwave preparation method thereof
CN102142541A (en) * 2011-02-25 2011-08-03 浙江大学 High capacity and stable cyclic performance lithium ion battery electrode and preparation method thereof
CN102142537A (en) * 2011-02-25 2011-08-03 浙江大学 Graphene/MoS2 compound nano material lithium ion battery electrode and preparation method thereof
CN103456948A (en) * 2013-09-25 2013-12-18 新疆师范大学 Preparation method of lithium ion secondary battery manganese titanate (III) lithium anode material
US20150280217A1 (en) * 2013-03-11 2015-10-01 William Marsh Rice University Three-dimensional graphene-backboned architectures and methods of making the same
WO2016007612A1 (en) * 2014-07-08 2016-01-14 Kansas State University Research Foundation Silicon-based polymer-derived ceramic composites comprising h-bn nanosheets

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101908628A (en) * 2010-08-18 2010-12-08 天津久聚能源科技发展有限公司 Transition metal composite oxide catalytic material and microwave preparation method thereof
CN102142541A (en) * 2011-02-25 2011-08-03 浙江大学 High capacity and stable cyclic performance lithium ion battery electrode and preparation method thereof
CN102142537A (en) * 2011-02-25 2011-08-03 浙江大学 Graphene/MoS2 compound nano material lithium ion battery electrode and preparation method thereof
US20150280217A1 (en) * 2013-03-11 2015-10-01 William Marsh Rice University Three-dimensional graphene-backboned architectures and methods of making the same
CN103456948A (en) * 2013-09-25 2013-12-18 新疆师范大学 Preparation method of lithium ion secondary battery manganese titanate (III) lithium anode material
WO2016007612A1 (en) * 2014-07-08 2016-01-14 Kansas State University Research Foundation Silicon-based polymer-derived ceramic composites comprising h-bn nanosheets

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DUCK HYUN YOUN 等: "Fabrication of grapheme-based electrode in less than a minute through hydrid microwave annealing", 《SCIENTIFIC REPORTS》 *
NING LIU 等: "Microwave-assisted synthesis of MoS2/grapheme nanocomposites for efficient hydrodesuldurization", 《FUEL》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357162A (en) * 2019-07-22 2019-10-22 金堆城钼业股份有限公司 A method of efficiently synthesizing high pure alcohol
CN110436525A (en) * 2019-07-22 2019-11-12 金堆城钼业股份有限公司 A kind of preparation method of micro-/ nano molybdenum disulfide
CN110436525B (en) * 2019-07-22 2021-09-28 金堆城钼业股份有限公司 Preparation method of micro/nano molybdenum disulfide
CN110357162B (en) * 2019-07-22 2021-11-09 金堆城钼业股份有限公司 Method for efficiently synthesizing high-purity molybdenum disulfide
CN111302445A (en) * 2020-02-25 2020-06-19 中国科学院东北地理与农业生态研究所 GO/MoS for removing lead ions in water body by electrochemical method2Electrode preparation method
CN111924881A (en) * 2020-07-30 2020-11-13 内蒙古凯金新能源科技有限公司 Molybdenum disulfide battery negative electrode material and preparation method thereof
CN111924881B (en) * 2020-07-30 2022-12-06 内蒙古凯金新能源科技有限公司 Molybdenum disulfide battery cathode material and preparation method thereof

Similar Documents

Publication Publication Date Title
CN105895886B (en) A kind of sodium-ion battery transition metal phosphide/porous anode composite and preparation method thereof
Hao et al. Electrospun single crystalline fork-like K2V8O21 as high-performance cathode materials for lithium-ion batteries
CN108598390A (en) A kind of preparation method and lithium-sulfur cell of positive material for lithium-sulfur battery
CN109904395A (en) A kind of molybdenum disulfide-graphene composite material
Xie et al. ZnO/Ni/C composite hollow microspheres as anode materials for lithium ion batteries
CN111710860B (en) Nitrogen-phosphorus co-doped carbon composite material modified by cobalt-molybdenum phosphide particles and preparation method and application thereof
CN106960954A (en) A kind of preparation method and application of Prussian blue/graphene/sulphur composite
Shen et al. Ionic liquid assist to prepare Si@ N-doped carbon nanoparticles and its high performance in lithium ion batteries
CN106410199B (en) A kind of lithium ion battery graphene/ferro-tin alloy composite negative pole material preparation method
CN104393272A (en) Lithium titanate cathode composite material and preparation method
CN109904400A (en) A kind of molybdenum disulfide/three-dimensional graphene composite material
CN107611374A (en) A kind of preparation method of new lithium sulfur battery anode material
CN105000545A (en) Method for preparing lithium ion battery artificial graphite/coke anode material
CN103972580B (en) A kind of lithium-sulfur cell
CN107658461B (en) Method for preparing ferric fluoride/carbon composite material by taking organic iron compound as raw material
CN109904398A (en) A kind of molybdenum disulfide/graphene composite material
CN108899499A (en) Based on phosphatic negative electrode material of Sb/Sn and preparation method thereof and the application in sodium-ion battery
CN108649191B (en) Preparation method of antimony/nitrogen-doped graphene composite for sodium ion battery, and obtained material and application thereof
CN109037623B (en) Positive electrode material of magnesium secondary battery and preparation method thereof
CN113871605A (en) Pre-lithiated silicon-based negative electrode material and preparation method and application thereof
CN114242961A (en) Graphene/silicon oxide-coated nano-silicon composite material, and preparation method and application thereof
Dai et al. Fabrication of MnO@ C-CNTs composite by CVD for enhanced performance of lithium ion batteries
CN109904396A (en) A kind of molybdenum disulfide-three-dimensional graphene composite material
CN110729478B (en) Antimony trisulfide nano-dot/sulfur-doped carbon composite material, preparation method thereof and application thereof in sodium/potassium ion battery
CN112201785B (en) Lithium-philic and sulfur-philic co-doped two-dimensional layered graphitized porous carbon material and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190618