CN106410150A - MoO2-MoS2 negative electrode material of sodium-ion battery with core-shell structure and preparation method of MoO2-MoS2 negative electrode material - Google Patents

MoO2-MoS2 negative electrode material of sodium-ion battery with core-shell structure and preparation method of MoO2-MoS2 negative electrode material Download PDF

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CN106410150A
CN106410150A CN201610963521.6A CN201610963521A CN106410150A CN 106410150 A CN106410150 A CN 106410150A CN 201610963521 A CN201610963521 A CN 201610963521A CN 106410150 A CN106410150 A CN 106410150A
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moo
shell structure
mos
ion battery
preparation
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许占位
王天
姚恺
黄剑锋
杨军
沈学涛
曹丽云
徐鹏飞
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Shaanxi University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a MoO2-MoS2 negative electrode material of a sodium-ion battery with a core-shell structure and a preparation method of the MoO2-MoS2 negative electrode material, and belongs to the technical field of preparation of sodium-ion battery electrode materials. The preparation method comprises the following steps: adopting MoO3 as a precursor to carry out oxidation-reduction reaction with S powder and obtain MoO2, adopting an in-situ synthesis method to grow MoS2 nanosheets on an MoO2 template, and forming an MoO2-MoS2 composite material with the core-shell structure. An MoO2 skeleton plays a role in structure support, so that the superimposition of sheet-shaped MoS2 is avoided, the conductivity of the material is improved, and the cyclic stability of the material is also improved. The preparation process is simple and easy to control, the period is short, the energy consumption is low, the repeatability of products is high, the yield is large, and the benefit for large-scale production is achieved. The MoO2-MoS2 negative electrode material prepared by the method has a three-dimensional core-shell structure and also has the characteristics of high specific-discharge capacity, good cyclic stability and the like.

Description

A kind of core shell structure MoO2-MoS2Anode material of lithium-ion battery and preparation method thereof
Technical field
The invention belongs to sodium ion battery electrode material preparing technical field, it is related to a kind of core shell structure MoO2-MoS2Sodium from Sub- cell negative electrode material and preparation method thereof is and in particular to a kind of prepare the MoO with core shell structure using in-situ synthesis2- MoS2The method of high performance anode material of lithium-ion battery.
Background technology
With the extensive concern to clean energy resource and renewable resource for the people, lithium ion battery has been widely used as various electricity The electrokinetic cell of the working power (mobile phone, notebook computer, digital camera etc.) of sub- product and portable outfit is (electric motor car, latent Ship, MISSILE LAUNCHING etc.).But the rare large-scale application limiting lithium ion battery technology of lithium resource.Comparatively, sodium storage Amount is high compared with lithium, and widely distributed, takes up an area the 2.6% of ball earth crustal mass, therefore sodium-ion battery becomes the right of researchers' concern As.
Graphite crystallinity is high, has the structure of stratiform, and for secondary battery cathode material, it is theoretical in lithium ion battery Capacity is 372mAh g-1, and it is used for sodium-ion battery, its theoretical capacity is about 20mAh g-1.[Qian J,Wu X,Cao Y, et al.High capacity and rate capability of amorphous phosphorus for sodium ion batteries[J].Angewandte Chemie,2013,125(17):4731-4734.], [Zhu Y, Han X, Xu Y,et al.Electrospun Sb/C fibers for a stable and fast sodium-ion battery anode[J].ACS nano,2013,7(7):6378-6386.] constantly explore sodium-ion battery negative pole for this researchers and can replace For material.Wherein, MoS2There is the sandwich stratiform of S-Mo-S (class Graphene) structure, in layer, atom is combined by strong covalent bond, layer There is weak van der Waals interaction and higher theoretical capacity and layer between, therefore suffer from the extensive concern of people.
MoS2A typical layer structure material, between layers be spaced about 0.615nm, be significantly higher than graphite (0.335nm).This is the embedded of sodium ion and abjection provides condition.Sheet MoS2Interlayer relies on Van der Waals force to be connected with each other, It easily causes structure collapses during embedding/removing sodium, thus occurring active material to assemble and big Volume Changes, with sodium ion Circulating battery number of times increases, and capacity also occurs substantially to decay.Simultaneously because the MoS of sheet2Through discharge and recharge occur superposition and its The reasons such as poorly conductive, when as anode material of lithium-ion battery, show poor cyclical stability.[Zhang S,Yu X,Yu H,et al.Growth of Ultrathin MoS2Nanosheets with Expanded Spacing of(002) Plane on Carbon Nanotubes for High-Performance Sodium-Ion Battery Anodes[J] .ACS applied materials&interfaces,2014,6(24):21880-21885.], [Zhang S, Yu X, Yu H,et al.Growth of Ultrathin MoS2Nanosheets with Expanded Spacing of(002)Plane on Carbon Nanotubes for High-Performance Sodium-Ion Battery Anodes[J].ACS applied materials&interfaces,2014,6(24):21880-21885.], [Xu X, Fan Z, Yu X, et al.A Nanosheets‐on‐Channel Architecture Constructed from MoS2and CMK‐3for High‐Capacity and Long‐Cycle‐Life Lithium Storage[J].Advanced Energy Materials,2014,4(17).]
Content of the invention
It is an object of the invention to provide a kind of core shell structure MoO2-MoS2Anode material of lithium-ion battery and its preparation side Method, the method preparation process is simple, easily-controllable, and reaction time is short, and energy consumption is low, and repeatability is high, and yield is big, is obtained through the method MoO2-MoS2Anode material of lithium-ion battery has the features such as three-dimensional core shell structure, specific discharge capacity height, good cycling stability.
The present invention is to be achieved through the following technical solutions：
The invention discloses a kind of core shell structure MoO2-MoS2The preparation method of anode material of lithium-ion battery, including following Step：
1) take ammonium molybdate, after being fully ground uniformly, from after room temperature insulation reaction 1～3h at 400～600 DEG C, cold But to room temperature, product is cleaned, is dried, prepared MoO3Presoma；
2) by MoO3Presoma and S powder are according to 0.5：The mass ratio of (1.0～5.0), after grinding uniformly, in inert conditions Under, from room temperature to 400～600 DEG C, insulation reaction 0.5～2h, then proceed to be warming up to 600～800 DEG C, insulation reaction 0.5～2h, is cooled to room temperature, product is cleaned, is dried, the MoO with core shell structure is obtained2-MoS2Sodium-ion battery is born Pole material.
Step 1) it is to be placed in after ammonium molybdate grinding uniformly in porcelain boat, porcelain boat is placed in tube furnace, in air atmosphere, With 5-10 DEG C of min-1Heating rate rise to 400～600 DEG C from room temperature.
Step 1) in, product deionized water is cleaned 3～6 times, is then vacuum dried 8～12h.
Step 2) it is that the reactant after grinding uniformly is placed in porcelain boat, porcelain boat is placed in tube furnace, in argon gas atmosphere Under react.
When reaction starts, the gas flow rate being passed through argon gas is 100sccm, with 5-10 DEG C of min-1Heating rate, from room temperature After being warming up to 100 DEG C, the gas flow rate controlling argon gas is 0～100sccm, with 5-10 DEG C of min-1Heating rate be continuously heating to 400～600 DEG C, insulation reaction 0.5～2h, then with 5-10 DEG C of min-1Heating rate be continuously heating to 600～800 DEG C, protect Temperature reaction 0.5～2h, reaction adjusts argon gas flow velocity after terminating be 10～100sccm.
Step 2) in, product deionized water is cleaned 3～6 times, is then vacuum dried 8～12h.
The invention also discloses adopting the core shell structure MoO being obtained with the aforedescribed process2-MoS2Anode material of lithium-ion battery.
Compared with prior art, the present invention has following beneficial technique effect：
Core shell structure MoO disclosed by the invention2-MoS2The preparation method of anode material of lithium-ion battery, with the MoO of synthesis3 For presoma, MoO3Redox reaction is occurred to obtain MoO with S powder2, make MoS using in-situ synthesis2Nanometer sheet is wrapped in A small amount of MoO2On nanoparticle template, form the MoO with core shell structure2-MoS2Composite, due to S powder during the course of the reaction Distillation is to be present in reaction environment in the form of a vapor, so allowing S powder and MoO3It is fully contacted, be capable of MoO3Complete It is reduced into MoO2, the MoO of new synthesis2Portion is vulcanized by S powder further, ultimately forms core shell structure MoO2-MoS2, S powder serves as reduction Agent and vulcanizing agent dual role；MoO2Skeleton plays the effect of structural support, it is to avoid the MoS of sheet2Superposition, improves material The cyclical stability of material is also improved while electric conductivity.Preparation process of the present invention is simple and easy to control, cycle is short, and energy consumption is low, produces The repeatability of thing is high, and yield is big, is conducive to large-scale production.
Further, during the course of the reaction, Ar gas flow rate is controlled to be 0-100sccm after temperature rises to 100 DEG C, its mesh Be by control Ar gas flow rate make MoO3It is fully contacted with the S steam after the distillation of S powder.Reaction adjusts argon gas after terminating Gas flow rate is 10-100sccm, to discharge superfluous S in reaction environment.
Further, it is continuously heating to 600-800 DEG C, be incubated 0.5-2h again, to guarantee S steam and MoO3Fully anti- Should.
Brief description
The MoO that Fig. 1 is obtained for the present invention2-MoS2The XRD of product；
The MoO that Fig. 2 is obtained for the present invention2-MoS2The SEM photograph of product；
The MoO that Fig. 3 is obtained for the present invention2-MoS2Cycle performance test chart.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, described be explanation of the invention and It is not to limit.
A kind of core shell structure MoO disclosed by the invention2-MoS2The preparation method of anode material of lithium-ion battery, including following Step：
Step 1, take ammonium molybdate, after being fully ground uniformly, from room temperature at 400～600 DEG C insulation reaction 1～3h Afterwards, it is cooled to room temperature, product is cleaned, is dried, prepared MoO3Presoma；
Step 2, by MoO3Presoma and S powder are according to 0.5：The mass ratio of (1.0～5.0), after grinding uniformly, in inertia bar Under part, from room temperature to 400～600 DEG C, insulation reaction 0.5～2h, then proceed to be warming up to 600～800 DEG C, insulation reaction 0.5～2h, is cooled to room temperature, product is cleaned, is dried, the MoO with core shell structure is obtained2-MoS2Sodium-ion battery is born Pole material.
It is to exist in the form of a vapor and reflect in environment because sulphur powder distils during the course of the reaction, so its object is to Allow S powder and MoO3It is fully contacted, to realize MoO3It is completely reduced into MoO2, the then MoO of new synthesis2Portion is by S powder sulphur further Change, ultimately form core shell structure MoO2-MoS2, S powder serves as reducing agent and vulcanizing agent dual role.
MoO3+S→MoO2+SO2↑
MoO2+S→MoS2+SO2↑
Specific embodiment is as follows：
Embodiment 1
A kind of core shell structure MoO2-MoS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1st, presoma MoO3Preparation
1) take ammonium molybdate, put in mortar and be fully ground.Sample after grinding is placed in porcelain boat, with 5 in tube furnace ℃min-1Heating rate rise to 400 DEG C, insulation 1h after, under the conditions of air atmosphere, Pintsch process obtains MoO3；
2) reaction is cooled to room temperature after terminating, and product deionized water is cleaned 3 times, is vacuum dried 8h, you can obtain pure Phase MoO3Presoma.
2、MoO2-MoS2Preparation
1) take presoma MoO3With S powder m (MoO3:S)=0.5:1.0 ratio, makes it mix by grinding, will grind Sample after mill is placed in porcelain boat, reacts under the conditions of tube-type atmosphere furnace argon gas atmosphere；
2) reaction is passed through Ar gas flow rate when starting is 100sccm it is ensured that reaction is carried out under inert conditions.With 5 DEG C min-1Heating rate, after temperature rises to 100 DEG C control Ar gas flow rate be 0sccm, continue to rise to 400 DEG C, be incubated 0.5h To guarantee that in presoma, ammonium molybdate cracks completely；
3) again with 5 DEG C of min-1Heating rate rise to 600 DEG C, again be incubated 0.5h.Reaction adjusts argon gas after terminating Flow velocity is 100sccm, to discharge superfluous S in reaction environment；
4) naturally cool to room temperature after question response terminates, product deionized water cleaned 3 times, be vacuum dried 8h, you can Obtain the MoO of core shell structure2-MoS2Product.
Referring to Fig. 1, can obtain from Fig. 1, can enter to prepare MoO by in-situ synthesis2-MoS2(red curve), its XRD Each of diffracting spectrum diffraction maximum all can be with MoO2And MoS2The diffraction maximum of standard card is corresponding, indicates it preferable Crystallinity and higher purity.
Referring to Fig. 2, as can be seen from the figure MoO2-MoS2Particle size be nanoscale, it is equal that particle surface is dispersed with size Even MoS2Nanometer sheet.
Referring to Fig. 3, Fig. 3 indicates the MoO of core shell structure2-MoS2(red curve) has excellent cyclical stability and puts Electric specific capacity.In 50mA g-1Current density under, MoO2-MoS2Negative material is used for sodium-ion battery, through 20 circle circulations, Capacity still may remain in 200mAh g-1More than, and coulombic efficiency is maintained at more than 96%.This shows core shell structure MoO2-MoS2Preferable in terms of specific discharge capacity and cyclical stability.
Embodiment 2
A kind of core shell structure MoO2-MoS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1st, presoma MoO3Preparation
1) take ammonium molybdate, put in mortar and be fully ground.Sample after grinding is placed in porcelain boat, with 6 in tube furnace ℃min-1Heating rate rise to 400 DEG C, insulation 1.5h after, under the conditions of air atmosphere, Pintsch process obtains MoO3；
2) reaction is cooled to room temperature after terminating, and product deionized water is cleaned 4 times, is vacuum dried 9h, you can obtain pure Phase MoO3Presoma.
2、MoO2-MoS2Preparation
1) take presoma MoO3With S powder m (MoO3:S)=0.5:2.0 ratio, makes it mix by grinding, will grind Sample after mill is placed in porcelain boat, reacts under the conditions of tube-type atmosphere furnace argon gas atmosphere；
2) reaction is passed through Ar gas flow rate when starting is 100sccm it is ensured that reaction is carried out under inert conditions.With 6 DEG C min-1Heating rate, after temperature rises to 100 DEG C control Ar gas flow rate be 25sccm, continue to rise to 450 DEG C, be incubated 0.8h To guarantee that in presoma, ammonium molybdate cracks completely；
3) again with 6 DEG C of min-1Heating rate rise to 650 DEG C, again be incubated 0.8h.Reaction adjusts argon gas after terminating Flow velocity is 100sccm, to discharge superfluous S in reaction environment；
4) naturally cool to room temperature after question response terminates, product deionized water cleaned 4 times, be vacuum dried 9h, you can Obtain the MoO of core shell structure2-MoS2Product.
Embodiment 3
A kind of core shell structure MoO2-MoS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1st, presoma MoO3Preparation
1) take ammonium molybdate, put in mortar and be fully ground.Sample after grinding is placed in porcelain boat, with 7 in tube furnace ℃min-1Heating rate rise to 500 DEG C, insulation 2h after, under the conditions of air atmosphere, Pintsch process obtains MoO3；
2) reaction is cooled to room temperature after terminating, and product deionized water is cleaned 5 times, is vacuum dried 10h, you can obtain pure Phase MoO3Presoma.
2、MoO2-MoS2Preparation
1) take presoma MoO3With S powder m (MoO3:S)=0.5:3.0 ratio, makes it mix by grinding, will grind Sample after mill is placed in porcelain boat, reacts under the conditions of tube-type atmosphere furnace argon gas atmosphere；
2) reaction is passed through Ar gas flow rate when starting is 100sccm it is ensured that reaction is carried out under inert conditions.With 7 DEG C min-1Heating rate, after temperature rises to 100 DEG C control Ar gas flow rate be 50sccm, continue to rise to 500 DEG C, be incubated 1.2h To guarantee that in presoma, ammonium molybdate cracks completely；
3) again with 7 DEG C of min-1Heating rate rise to 700 DEG C, again be incubated 1.2h.Reaction adjusts argon gas after terminating Flow velocity is 100sccm, to discharge superfluous S in reaction environment；
4) naturally cool to room temperature after question response terminates, product deionized water cleaned 5 times, be vacuum dried 10h, you can Obtain the MoO of core shell structure2-MoS2Product.
Embodiment 4
Embodiment 3
A kind of core shell structure MoO2-MoS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1st, presoma MoO3Preparation
1) take ammonium molybdate, put in mortar and be fully ground.Sample after grinding is placed in porcelain boat, with 8 in tube furnace ℃min-1Heating rate rise to 550 DEG C, insulation 2.5h after, under the conditions of air atmosphere, Pintsch process obtains MoO3；
2) reaction is cooled to room temperature after terminating, and product deionized water is cleaned 6 times, is vacuum dried 11h, you can obtain pure Phase MoO3Presoma.
2、MoO2-MoS2Preparation
1) take presoma MoO3With S powder m (MoO3:S)=0.5:4.0 ratio, makes it mix by grinding, will grind Sample after mill is placed in porcelain boat, reacts under the conditions of tube-type atmosphere furnace argon gas atmosphere；
2) reaction is passed through Ar gas flow rate when starting is 100sccm it is ensured that reaction is carried out under inert conditions.With 8 DEG C min-1Heating rate, after temperature rises to 100 DEG C control Ar gas flow rate be 75sccm, continue to rise to 550 DEG C, be incubated 1.5h To guarantee that in presoma, ammonium molybdate cracks completely；
3) again with 8 DEG C of min-1Heating rate rise to 750 DEG C, again be incubated 1.5h.Reaction adjusts argon gas after terminating Flow velocity is 100sccm, to discharge superfluous S in reaction environment；
4) naturally cool to room temperature after question response terminates, product deionized water cleaned 6 times, be vacuum dried 11h, you can Obtain the MoO of core shell structure2-MoS2Product.
Embodiment 5
Embodiment 3
A kind of core shell structure MoO2-MoS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1st, presoma MoO3Preparation
1) take ammonium molybdate, put in mortar and be fully ground.Sample after grinding is placed in porcelain boat, with 10 in tube furnace ℃min-1Heating rate rise to 600 DEG C, insulation 3h after, under the conditions of air atmosphere, Pintsch process obtains MoO3；
2) reaction is cooled to room temperature after terminating, and product deionized water is cleaned 5 times, is vacuum dried 12h, you can obtain pure Phase MoO3Presoma.
2、MoO2-MoS2Preparation
1) take presoma MoO3With S powder m (MoO3:S)=0.5:5.0 ratio, makes it mix by grinding, will grind Sample after mill is placed in porcelain boat, reacts under the conditions of tube-type atmosphere furnace argon gas atmosphere；
2) reaction is passed through Ar gas flow rate when starting is 100sccm it is ensured that reaction is carried out under inert conditions.With 10 DEG C min-1Heating rate, after temperature rises to 100 DEG C control Ar gas flow rate be 50sccm, continue to rise to 600 DEG C, insulation 2h with Guarantee that in presoma, ammonium molybdate cracks completely；
3) again with 10 DEG C of min-1Heating rate rise to 800 DEG C, again be incubated 2h.Reaction adjusts argon gas stream after terminating Speed is 100sccm, to discharge superfluous S in reaction environment；
4) naturally cool to room temperature after question response terminates, product deionized water cleaned 5 times, be vacuum dried 12h, you can Obtain the MoO of core shell structure2-MoS2Product.
The present invention is with MoO3For presoma, it occurs redox reaction to obtain MoO with S powder2, made using in-situ synthesis Obtain MoS2Nanometer length of a film is in MoO2In template, form the MoO with three-dimensional core shell structure2-MoS2Composite.Three-dimensional nucleocapsid knot Structure has insertion, the features such as specific surface area is big.Three-dimensional core shell structure electrode material can make secondary cell during charge/discharge Stability Analysis of Structures, can be prevented effectively from subsiding of two-dimensional electrode material structure, by two-dimentional MoS2Structure is optimized, to build three-dimensional Core shell structure MoO2-MoS2For anode material of lithium-ion battery, thus improving the chemical property of sodium-ion battery.

Claims (7)

1. a kind of core shell structure MoO2-MoS2The preparation method of anode material of lithium-ion battery is it is characterised in that include following walking Suddenly：
1) take ammonium molybdate, after being fully ground uniformly, from after room temperature insulation reaction 1～3h at 400～600 DEG C, be cooled to Room temperature, product is cleaned, is dried, prepared MoO3Presoma；
2) by MoO3Presoma and S powder are according to 0.5：The mass ratio of (1.0～5.0), after grinding uniformly, under inert conditions, from room Temperature is warming up to 400～600 DEG C, insulation reaction 0.5～2h, then proceedes to be warming up to 600～800 DEG C, insulation reaction 0.5～2h, It is cooled to room temperature, product is cleaned, is dried, the MoO with core shell structure is obtained2-MoS2Anode material of lithium-ion battery.
2. core shell structure MoO according to claim 12-MoS2The preparation method of anode material of lithium-ion battery, its feature It is, step 1) it is to be placed in after ammonium molybdate grinding uniformly in porcelain boat, porcelain boat is placed in tube furnace, in air atmosphere, with 5-10℃min-1Heating rate rise to 400～600 DEG C from room temperature.
3. core shell structure MoO according to claim 12-MoS2The preparation method of anode material of lithium-ion battery, its feature It is, step 1) in, product deionized water is cleaned 3～6 times, is then vacuum dried 8～12h.
4. core shell structure MoO according to claim 12-MoS2The preparation method of anode material of lithium-ion battery, its feature It is, step 2) it is that the reactant after grinding uniformly is placed in porcelain boat, porcelain boat is placed in tube furnace, sends out under an argon atmosphere Raw reaction.
5. core shell structure MoO according to claim 42-MoS2The preparation method of anode material of lithium-ion battery, its feature It is, when reaction starts, the gas flow rate being passed through argon gas is 100sccm, with 5-10 DEG C of min-1Heating rate, from room temperature To after 100 DEG C, the gas flow rate controlling argon gas is 0～100sccm, with 5-10 DEG C of min-1Heating rate be continuously heating to 400 ～600 DEG C, insulation reaction 0.5～2h, then with 5-10 DEG C of min-1Heating rate be continuously heating to 600～800 DEG C, insulation is anti- Answer 0.5～2h, reaction adjusts argon gas flow velocity after terminating be 10～100sccm.
6. core shell structure MoO according to claim 12-MoS2The preparation method of anode material of lithium-ion battery, its feature It is, step 2) in, product deionized water is cleaned 3～6 times, is then vacuum dried 8～12h.
7. adopt the core shell structure MoO that in claim 1～6, the method described in any one is obtained2-MoS2Sodium-ion battery is born Pole material.
CN201610963521.6A 2016-11-04 2016-11-04 MoO2-MoS2 negative electrode material of sodium-ion battery with core-shell structure and preparation method of MoO2-MoS2 negative electrode material Pending CN106410150A (en)

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CN109768246A (en) * 2018-12-29 2019-05-17 湖南中科星城石墨有限公司 A kind of nano-silicon composite anode materials and preparation method thereof for lithium ion battery
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CN110048095A (en) * 2019-03-25 2019-07-23 天津大学 A method of preparing the molybdenum disulfide molybdenum dioxide composite material for sodium ion negative electrode material
CN111701597A (en) * 2020-05-20 2020-09-25 北京航空航天大学 Multi-metal-doped molybdenum disulfide material and preparation method and application thereof
CN111755672A (en) * 2019-05-14 2020-10-09 中南大学 Molybdenum disulfide coated molybdenum dioxide negative electrode material and preparation method and application thereof
CN111799467A (en) * 2020-07-20 2020-10-20 陕西科技大学 MoS for negative electrode of sodium-ion battery2/MoS2Nanocomposite and method for preparing same
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CN115634661A (en) * 2022-10-25 2023-01-24 唐山师范学院 Efficient adsorbent and preparation method and application thereof

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CN107069003A (en) * 2017-04-10 2017-08-18 中国石油大学(华东) A kind of nano composite material and its preparation method and application
CN107069003B (en) * 2017-04-10 2019-07-05 中国石油大学(华东) A kind of nanocomposite and its preparation method and application
CN107159268B (en) * 2017-04-25 2020-02-11 郑州大学 Hollow molybdenum disulfide/molybdenum trioxide flower-shaped heterostructure nano material, preparation method and application
CN107159268A (en) * 2017-04-25 2017-09-15 郑州大学 A kind of hollow molybdenum disulfide/molybdenum trioxide flower ball-shaped heterojunction structure nano material, preparation method and application
CN107452631A (en) * 2017-05-08 2017-12-08 北京大学 A kind of method that electronic device electrode is prepared using metallic transition metals chalcogen compound
CN107344099A (en) * 2017-06-30 2017-11-14 西北大学 A kind of one-dimentional structure MoO2‑MoS2The preparation method of elctro-catalyst
CN107344099B (en) * 2017-06-30 2019-04-05 西北大学 A kind of one-dimentional structure MoO2-MoS2The preparation method of elctro-catalyst
CN107742585A (en) * 2017-09-29 2018-02-27 江苏科技大学 A kind of height ratio capacity MoS2/Mn2O3Nano-hollow ball combination electrode material and preparation method and application
CN107742585B (en) * 2017-09-29 2019-06-25 江苏科技大学 A kind of height ratio capacity MoS2/Mn2O3Nano-hollow ball combination electrode material and the preparation method and application thereof
CN108963215A (en) * 2018-07-03 2018-12-07 陕西科技大学 The fixed porous MoS of N doped graphene flexible substrates with three-dimensional structure2Nano material and its preparation method and application
CN108963215B (en) * 2018-07-03 2021-04-30 陕西科技大学 N-doped graphene flexible substrate fixed porous MoS with three-dimensional structure2Nano material and preparation method and application thereof
CN108899514B (en) * 2018-07-03 2021-04-30 陕西科技大学 Three-dimensional porous MoS2rGO nano material and preparation method and application thereof
CN108899514A (en) * 2018-07-03 2018-11-27 陕西科技大学 A kind of three-dimensional porous MoS2/ rGO nano material and its preparation method and application
CN109659527A (en) * 2018-12-03 2019-04-19 郑州科技学院 A kind of preparation method of molybdenum disulfide-molybdenum dioxide Core-shell structure material
CN109659527B (en) * 2018-12-03 2021-09-07 郑州科技学院 Preparation method of molybdenum disulfide-molybdenum dioxide core-shell structure ion battery anode material
CN109768246A (en) * 2018-12-29 2019-05-17 湖南中科星城石墨有限公司 A kind of nano-silicon composite anode materials and preparation method thereof for lithium ion battery
CN109830657A (en) * 2019-01-14 2019-05-31 陕西科技大学 A kind of MoS2/MoO2The preparation method of/three-dimensional carbon lithium ion battery negative material
CN110048095A (en) * 2019-03-25 2019-07-23 天津大学 A method of preparing the molybdenum disulfide molybdenum dioxide composite material for sodium ion negative electrode material
CN109950509B (en) * 2019-04-09 2021-08-20 武汉轻工大学 MoO (MoO)2/MoS2Composite electrode material and preparation method thereof
CN109950509A (en) * 2019-04-09 2019-06-28 武汉轻工大学 A kind of MoO2/MoS2Combination electrode material and preparation method thereof
CN111755672A (en) * 2019-05-14 2020-10-09 中南大学 Molybdenum disulfide coated molybdenum dioxide negative electrode material and preparation method and application thereof
CN111755672B (en) * 2019-05-14 2021-11-12 中南大学 Molybdenum disulfide coated molybdenum dioxide negative electrode material and preparation method and application thereof
CN111701597A (en) * 2020-05-20 2020-09-25 北京航空航天大学 Multi-metal-doped molybdenum disulfide material and preparation method and application thereof
CN111701597B (en) * 2020-05-20 2021-09-24 北京航空航天大学 Multi-metal-doped molybdenum disulfide material and preparation method and application thereof
CN111799467A (en) * 2020-07-20 2020-10-20 陕西科技大学 MoS for negative electrode of sodium-ion battery2/MoS2Nanocomposite and method for preparing same
CN111799467B (en) * 2020-07-20 2022-11-18 陕西科技大学 MoS for negative electrode of sodium-ion battery 2 /MoS 2 Nanocomposite and method for preparing same
CN114609197A (en) * 2022-03-25 2022-06-10 电子科技大学 Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor
CN114609197B (en) * 2022-03-25 2023-11-21 电子科技大学 Gas-sensitive material, preparation method and NH (NH) thereof 3 Application in gas sensor
CN115634661A (en) * 2022-10-25 2023-01-24 唐山师范学院 Efficient adsorbent and preparation method and application thereof
CN115634661B (en) * 2022-10-25 2023-11-21 唐山师范学院 Efficient adsorbent and preparation method and application thereof

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