CN109904398A - A kind of molybdenum disulfide/graphene composite material - Google Patents

A kind of molybdenum disulfide/graphene composite material Download PDF

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CN109904398A
CN109904398A CN201711296626.1A CN201711296626A CN109904398A CN 109904398 A CN109904398 A CN 109904398A CN 201711296626 A CN201711296626 A CN 201711296626A CN 109904398 A CN109904398 A CN 109904398A
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graphene
preparation
composite material
molybdenum disulfide
graphene oxide
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郭金
张会成
王少军
凌凤香
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China Petroleum and Chemical Corp
Sinopec Dalian Research Institute of Petroleum and Petrochemicals
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China Petroleum and Chemical Corp
Sinopec Dalian Research Institute of Petroleum and Petrochemicals
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    • 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: four thio ammonium molybdate and graphene oxide 1-20:1 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 1-15min of 300-1000W, obtains the molybdenum disulfide/graphene composite material.Gained molybdenum disulfide/graphene composite material of the invention is under microwave heating condition, and graphene oxide is heat-treated as graphene, while heated decompose rapidly of single-source precursor generates MoS2, so that MoS2Nanometer sheet directly goes up growth in situ on the surface of graphene, and microwave heating speed is fast, and homogeneous heating makes 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 Black alkene combines unstable, the problem of charge and discharge easily lead to electrode breakages, the present invention provide 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:
Four thio ammonium molybdate and graphene oxide 1-20:1 in mass ratio are mixed, is placed in ball mill and is ground;Ball milling Material afterwards is placed in microwave reaction chamber, with the heats 1-15min of 300-1000W, obtains the molybdenum disulfide/stone Black alkene composite material.
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 Number is 300-3000r/min, milling time 0.5-3h.
In the above preparation method, grinding is to carry out under an inert atmosphere.
In the above preparation method, microwave reaction preferably heats 3 ~ 10min in 500 ~ 1000W.
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 microwave heating condition, and graphene oxide is heat-treated as graphene, while single-source precursor is heated rapidly point Solution generates MoS2, so that MoS2Directly upper growth in situ heats equal nanometer sheet since microwave heating speed is fast on the surface of graphene It is even so that MoS2Nanometer sheet is firmly combined with graphene, and does not easily cause particle packing, is greatly shortened needed for synthetic material Time and alleviate graphene and MoS2The problem of reuniting in long-term heated situation.
The technical purpose of third invention of the 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, mutability, easy storage, large specific surface area are not mentioned as lithium ion battery negative material for lithium ion transport in air 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 example 1;
Fig. 2 is that molybdenum disulfide/graphene composite material in current density is 100mAg in example 9-1When charge and discharge cycles it is bent Line.
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 four thio ammonium molybdate and graphene oxide with the mass ratio of 1:1 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 fitted into reaction tube, is placed in In microwave reaction chamber, 1h is purged with the argon gas of 100mL/min.3min is heated with the power microwave of 600W.It cools down under an ar atmosphere 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
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 2:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 3:1, After revolving speed 400rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, it is anti-to be placed in microwave It answers in chamber, 1h is purged with the argon gas of 100mL/min.3min is heated with the power microwave of 600W.It is cooled to room temperature under an ar atmosphere, Up to molybdenum disulfide/graphene composite material.
Embodiment 3
The preparation method is the same as that of Example 1 for graphene oxide
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 3:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 3:1, After revolving speed 400rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, it is anti-to be placed in microwave It answers in chamber, 1h is purged with the argon gas of 100mL/min.5min is heated with the power microwave of 600W.It is cooled to room temperature under an ar atmosphere, Up to molybdenum disulfide/graphene composite material.
Embodiment 4
The preparation method is the same as that of Example 1 for graphene oxide
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 3:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 4:1, After 400 rpm ball milling 1h of revolving speed, 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.5min 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
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 3:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 5:1, After revolving speed 400rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, it is anti-to be placed in microwave It answers in chamber, 1h is purged with the argon gas of 100mL/min.5min is heated with the power microwave of 600W.It is cooled to room temperature under an ar atmosphere, Up to molybdenum disulfide/graphene composite material.
Embodiment 6
The preparation method is the same as that of Example 1 for graphene oxide
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 3:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 5:1, After revolving speed 600rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, it is anti-to be placed in microwave It answers in chamber, 1h is purged with the argon gas of 100mL/min.8min is heated with the power microwave of 600W.It is cooled to room temperature under an ar atmosphere, Up to molybdenum disulfide/graphene composite material.
Embodiment 7
The preparation method is the same as that of Example 1 for graphene oxide
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 3:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 5:1, After revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, it is anti-to be placed in microwave It answers in chamber, 1h is purged with the argon gas of 100mL/min.8min is heated with the power microwave of 600W.It is cooled to room temperature under an ar atmosphere, Up to molybdenum disulfide/graphene composite material.
Embodiment 8
The preparation method is the same as that of Example 1 for graphene oxide
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 3:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 5:1, After revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, it is anti-to be placed in microwave It answers in chamber, 1h is purged with the argon gas of 100mL/min.8min is heated with the power microwave of 800W.It is cooled to room temperature under an ar atmosphere, Up to molybdenum disulfide/graphene composite material.
Embodiment 9
The preparation method is the same as that of Example 1 for graphene oxide
The preparation of molybdenum disulfide/graphene composite material: four thio ammonium molybdate and graphene oxide are mixed with the mass ratio of 3:1 It closes, mixture is placed in the agate pot full of nitrogen, using ball mill ball milling, the mass ratio of mill ball and mixture is 5:1, After revolving speed 800rpm ball milling 1h, cooled to room temperature collects product.Material after ball milling is packed into reaction tube, it is anti-to be placed in microwave It answers in chamber, 1h is purged with the argon gas of 100mL/min.8min is heated with the power microwave of 1000W.It is cooled to room under an ar atmosphere Temperature is to get molybdenum disulfide/graphene composite material.
Molybdenum disulfide/graphene composite material of embodiment 1 ~ 9 is used for lithium ion battery negative material.With the curing of synthesis Molybdenum/graphene is active component, selects 2016 type battery cases, metal lithium sheet (16 mm of Φ × 1mm), with 1.0M LiPF6Carbon Vinyl acetate (EC)/diethyl carbonate (DEC) mixed liquor (volume ratio 1:1) is electrolyte, poly- third coal of Celgard2300 micropore Film is as battery diaphragm.The above material is assembled into button battery in the glove box full of Ar gas, waits working electrodes electric Solution liquid 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 9 is in 0.01-3.0V voltage In range, 100mAg-1Current density under cyclical stability test result it is as shown in Fig. 2.The charge and discharge for the first time of embodiment 1 ~ 9 Capacitance and the discharge capacity after 100 charge-discharge tests are shown in Table 1.
Table 1
Comparative example 1
Using preparation method same as Example 9, the difference is that not using microwave heating, it is exchanged with conventional Muffle furnace 800 DEG C roasting 3min.Four thio ammonium molybdate does not decompose completely as the result is shown, causes molybdenum disulfide/graphene yield less, by gained Material is used for lithium cell cathode material, and initial discharge capacity only has 590.6mAhg-1

Claims (10)

1. a kind of preparation method of molybdenum disulfide/graphene composite material, comprising the following steps:
Four thio ammonium molybdate and graphene oxide 1-20:1 in mass ratio are mixed, is placed in ball mill and is ground;Ball milling Material afterwards is placed in microwave reaction chamber, with the heats 1-15min of 300-1000W, obtains the molybdenum disulfide/stone Black alkene composite material.
2. 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.
3. preparation method according to claim 1, which is characterized in that milling time 0.5-3h.
4. 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.
5. 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.
6. preparation method according to claim 1, which is characterized in that the graphene oxide is that graphite is obtained through oxidation.
7. preparation method according to claim 6, 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.
8. preparation method according to claim 7, which is characterized in that the specification of the natural flake graphite is 100-500 Mesh.
9. molybdenum disulfide/graphene composite material of the preparation of method described in claim 1 ~ 8 any one.
10. application of the molybdenum disulfide/graphene composite material as claimed in claim 9 as lithium ion battery negative material.
CN201711296626.1A 2017-12-08 2017-12-08 A kind of molybdenum disulfide/graphene composite material Pending CN109904398A (en)

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Publication number Priority date Publication date Assignee Title
CN112750992A (en) * 2019-10-31 2021-05-04 中国石油化工股份有限公司 Molybdenum disulfide/titanium dioxide/graphene composite material
CN113140711A (en) * 2020-01-19 2021-07-20 中国地质大学(北京) Sulfide mineral-based composite material and preparation and application thereof
CN113675391A (en) * 2021-08-05 2021-11-19 常熟理工学院 Heterogeneous layered composite material for lithium ion battery cathode and preparation method thereof

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Application publication date: 20190618