CN106207171A - The preparation method of a kind of molybdenum bisuphide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery - Google Patents
The preparation method of a kind of molybdenum bisuphide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of molybdenum bisuphide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery, preparation method step includes hydro-thermal operation, compound working procedure, preparation method of the present invention makes the molybdenum bisuphide of lamellar directly carry out growth in situ at graphenic surface, and this material not only pattern is unique；Having the biggest specific surface area, solve the agglomeration traits of Graphene and molybdenum bisuphide, this materials application, in lithium ion battery negative material, has good cycling stability, specific energy density advantages of higher.
Description
Technical field
The present invention relates to technical field of inorganic nanometer material, particularly to a kind of molybdenum bisuphide/graphene nano composite wood
The preparation method of material, lithium ion battery negative, lithium ion battery.
Background technology
Along with environment goes from bad to worse, energy problem highlights the most day by day, in recent years for the research day of lithium-ion energy storage material
Gradually normalization.Lithium ion battery, as a kind of emerging energy storage instrument, can make full use of regenerative resource, solve it restricted simultaneously
Problem, lithium ion battery is with low cost, and energy storage capacity is good, and conversion efficiency is high, good cycling stability.
Molybdenum bisuphide two-dimensional slice structure provides possibility for the more preferable deintercalation of lithium ion, and molybdenum bisuphide has phase simultaneously
To higher specific capacity (1334mAh/g), but due to molybdenum bisuphide poorly conductive, and cyclical stability is poor thus limits it
Development.Three-dimensional grapheme structure is always treated as the ideal structure of lithium ion battery negative material, and graphene three-dimensional structure is very big
The electric conductivity of ground reinforcing material, and graphene oxide has the multiple group such as carbonyl, carboxyl, and it can be made multiple with other nano materials
Closing, three-dimensional graphene oxide has the advantage of three-dimensional grapheme, carries a lot of group, beneficially material simultaneously and meets.
There are the advantages such as good conductivity, Stability Analysis of Structures, molybdenum bisuphide and graphene composite material to become one due to Graphene
Individual study hotspot, such as Ye Jianbo et al. (J.Mater.Chem.A, 2015,3,6,884 6893.) is by simple hydro-thermal
Method has synthesized flaky molybdenum disulfide, and this kind of structure specific surface area is big, good conductivity；Jeong Jae-Min et al. (Nanoscale,
2015,7,324 329.) MoS has been synthesized by simple method2@C nucleocapsid structure, this material has for cathode of lithium battery
Superior cycle performance.
But Graphene there is also some problems as lithium ion battery negative material: Graphene is easy to due to Van der Waals force
The most again it is stacked into together, affects lithium ion transmission in Graphene, and then cause the high rate performance of Graphene to decline.Therefore
Structural parameters and surface functional group, fault of construction, the heteroatom such as nitrogen, oxygen, hydrogen etc. of grapheme material are prepared by distinct methods
How to affect the further investigation of its electrochemical lithium storage performance need.In terms of graphene composite material, the overwhelming majority of report at present
Graphene composite material remains being simply mixed of Graphene and active material, and after repeatedly discharge and recharge, active material may be with
Graphene separates, thus causes performance of lithium ion battery to decline.
Summary of the invention
The deficiency existed in view of prior art, the technical problem to be solved is to provide a kind of molybdenum bisuphide/stone
The ink preparation method of alkene nano composite material, lithium ion battery negative, lithium ion battery, the present invention utilizes cheap raw material system
For obtaining three-dimensional column redox graphene, by soaking, be combined, washing, it is dried, obtains by molybdenum bisuphide/Graphene multiple
Condensation material.The present invention is directed to the technical barrier such as cyclical stability improving molybdenum bisuphide as electrode material, it is provided that Yi Zhonggong
Skill is simple, productivity is high, the composite material and preparation method thereof of low cost.
A kind of preparation method of molybdenum bisuphide/graphene nanocomposite material, step includes:
A, hydro-thermal operation: graphite oxide is dispersed in water ultrasonic prepared graphene oxide and holds liquid, add sulfur in solution
Acid, more ultrasonic it is mixed to get mixed liquor, then mixed liquor being transferred to reacts 18～30 in reactor at 160～260 DEG C little
Time, taking out washing, obtain three-dimensional column redox graphene, it is little that reaction condition preferably reacts 20～24 at 190～220 DEG C
Time；
In described step A, graphene oxide synthesizes by improving Hummers method, concretely comprises the following steps:
Weigh 5.0g graphite and 3.75g NaNO respectively3Put in the beaker of 1L, machinery strong stirring, it is slowly added to
The concentrated sulphuric acid of 150mL, stirs 0.5 hour, is slow added into the KMnO of 20g4, within 0.5 hour, add, after continuing stirring 20 hours,
Owing to reactant viscosity increases, stop stirring, obtain starchiness aubergine material.After placing 5 days, it is respectively added slowly to 500mL
Deionized water and 30mLH2O2, now solution colour becomes obvious glassy yellow, after solution fully reacts, and centrifugal, washing,
Obtain graphite oxide.
In described step A, in mixed liquor, the concentration of graphene oxide is 0.75～1.5g/L, preferably 1.0～1.25g/L；
In described step A, in mixed liquor, the concentration of sulphuric acid is 0.8～1.7mol/L, preferably 1.2～1.4mol/L.
B, compound working procedure: molybdenum salt, sulfur source, carbamide are dissolved in the mixed solvent of water and organic solvent, are made into mixed solution,
Then three-dimensional column redox graphene is put in above-mentioned solution, soak more than 1 day at 3～60 DEG C, preferably 10～30
Soak 1～2 day at DEG C；Finally mixed solution and three-dimensional column redox graphene are transferred in hydrothermal reaction kettle, 160
～react at 240 DEG C 18～30 hours, preferably reacting 20～24 hours at 180～210 DEG C, product is scrubbed and dried,
Obtain molybdenum bisuphide and graphene composite material i.e. molybdenum bisuphide/graphene nanocomposite material.
One or both in sodium molybdate, the ammonium molybdate of molybdenum salt, molybdenum salt concentration in mixed solution in described step B
It is 0.05～0.2mol/L, preferably 0.1～0.2mol/L；
One or more in thioacetamide, thiourea, Cys of sulfur source in described step B, sulfur source is mixed
The concentration closed in solution is 0.15～0.6mol/L, preferably 0.25～0.4mol/L；
In described step B, carbamide concentration in mixed solution is 0.15～0.6mol/L, preferably 0.3～0.5mol/L；
In described step B, three-dimensional column redox graphene concentration in mixed solution is 0.1～4.0mg/mL, excellent
Select 0.6～1.2mg/mL；
One or both in ethanol, the DMF (N-N dimethylformamide) of organic solvent in described step B, preferably
DMF；In described mixed solvent, water is 1:3～3:1, preferably 1:1～1:2 with the volume ratio of organic solvent；
Described step B is dried into being vacuum dried, vacuum drying temperature 30～80 DEG C, drying time 4～12 hours, preferably
It is dried 6～10 hours at 40～60 DEG C.
A kind of lithium ion battery negative, is made up of molybdenum bisuphide/graphene nanocomposite material；
A kind of lithium ion battery, by the lithium ion battery negative including that molybdenum bisuphide/graphene nanocomposite material is made
Make.
The mechanism of the present invention: the present invention with the three-dimensional redox graphene of synthesis in hydrothermal step as template, by
Mixed solution soaks, the group on three-dimensional redox graphene will negative ions in adsorbent solution, then by molten
Agent full-boiled process carries out growth in situ again.
The present invention, with the three-dimensional redox graphene in hydro-thermal operation as template, is immersed in molybdenum salt, sulfur source, carbamide
Mixed solution in, made the molybdenum bisuphide of lamellar directly carry out growth in situ at graphenic surface by solvent-thermal method, this
Material not only pattern is unique；Having the biggest specific surface area, solve the agglomeration traits of Graphene and molybdenum bisuphide, this material should
For lithium ion battery negative material, there are good cycling stability, specific energy density advantages of higher.
The present invention compared with prior art has the advantage that
(1) molybdenum bisuphide/graphene nanocomposite material obtained by, molybdenum bisuphide lamellar is in graphenic surface distribution all
Even；
(2) molybdenum bisuphide obtained by/graphene nanocomposite material stable performance, the most not changeableness, easily
Deposit；
(3) molybdenum bisuphide obtained by/graphene nanocomposite material nanometer sheet thickness is little, and product specific surface area is big；
(4) molybdenum bisuphide/graphene nanocomposite material obtained by is used as lithium ion battery negative material, has bigger
Specific capacity and preferable cycle performance；
(5) experimentation is simple, requires low to experimental instrument and equipment, and raw material is easy to get, and expense is low, can carry out batch raw
Produce.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the molybdenum bisuphide/graphene composite material of embodiment 1 preparation.
Fig. 2 is the SEM figure of the molybdenum bisuphide/graphene composite material of embodiment 2 preparation.
Fig. 3 is the XRD figure of the molybdenum bisuphide/graphene composite material of embodiment 2 preparation.
Fig. 4 is the SEM figure of the molybdenum bisuphide/graphene composite material of embodiment 3 preparation.
Fig. 5 is the SEM figure of the molybdenum bisuphide/graphene composite material of embodiment 4 preparation.
Fig. 6 is the SEM figure of the molybdenum bisuphide/graphene composite material of embodiment 5 preparation.
Fig. 7 is that the molybdenum bisuphide/graphene composite material of embodiment 5 preparation exists as lithium ion battery negative material
Cyclical stability test figure under 100mA/g electric current density.
Detailed description of the invention
Embodiment 1
The preparation of graphite oxide: weigh 5.0g graphite and 3.75g NaNO respectively3Putting in the beaker of 1L, machinery strength is stirred
Mix, be slowly added to the concentrated sulphuric acid of 150mL, stir 0.5 hour, be slow added into the KMnO of 20g4, within 0.5 hour, add, continue to stir
After mixing 20 hours, reactant viscosity increases, and stops stirring, obtains starchiness aubergine material.After placing 5 days, the most slowly add
Enter 500mL deionized water and 30mL H2O2, now solution colour becomes obvious glassy yellow, after solution fully reacts, from
The heart, washing, obtain graphite oxide.
Hydro-thermal operation: be dissolved in 80ml deionized water by 70mg graphene oxide, adds 7ml concentrated sulphuric acid (ρ=1.84g/
cm3), ultrasonic disperse 3 hours, transfer it in reactor, 190 DEG C of isothermal reactions 23 hours, it is thus achieved that three-dimensional column is also
Former oxidation graphene oxide, washing is collected.
Compound working procedure: by 0.4g sodium molybdate, 0.3g thiourea, 0.2g carbamide, is dissolved into mixed solvent (8ml water and 8ml
DMF) in, joining in above-mentioned mixed solution by 14mg three-dimensional redox graphene, 3 DEG C are soaked 3 days, are then transferred to
In reactor, 210 DEG C of isothermal reactions 30 hours, product is washed, 60 DEG C are vacuum dried 7 hours, collect and obtain molybdenum bisuphide/stone
Ink alkene composite.
Embodiment 2
The preparation method of graphite oxide is with embodiment 1.
Hydro-thermal operation: be dissolved in 80ml deionized water by 120mg graphene oxide, adds 6ml concentrated sulphuric acid (ρ=1.84g/
cm3), ultrasonic disperse 2 hours, transfer it in reactor, 160 DEG C of isothermal reactions 20 hours, it is thus achieved that three-dimensional column is also
Former oxidation graphene oxide, washing is collected.
Compound working procedure: by 0.5g ammonium molybdate, 0.4g thioacetamide, 0.5g carbamide, be dissolved into mixed solvent (4ml water and
12ml DMF) in, 24mg three-dimensional redox graphene is joined in above-mentioned mixed solution, 10 DEG C are soaked 1 day, subsequently by it
Being transferred in reactor, 200 DEG C of isothermal reactions 18 hours, washed by product, 30 DEG C are vacuum dried 12 hours, collect and obtain two sulfur
Change molybdenum/graphene composite material.
Embodiment 3
The preparation method of graphite oxide is with embodiment 1.
Hydro-thermal operation: be dissolved in 80ml deionized water by 90mg graphene oxide, adds 9ml concentrated sulphuric acid (ρ=1.84g/
cm3), ultrasonic disperse 3 hours, transfer it in reactor, 260 DEG C of isothermal reactions 30 hours, it is thus achieved that three-dimensional column is also
Former graphene oxide, washing is collected.
Compound working procedure: by 0.6g sodium molybdate, 0.7g thiourea, 0.6g carbamide, is dissolved into mixed solvent (12ml water and 4ml second
Alcohol) in, 18mg three-dimensional redox graphene is joined in above-mentioned mixed solution, 30 DEG C are soaked 3 days, are then transferred to
In reactor, 180 DEG C of isothermal reactions 30 hours, product is washed, 40 DEG C are vacuum dried 12 hours, collect obtain molybdenum bisuphide/
Graphene composite material.
Embodiment 4
The preparation method of graphite oxide is with embodiment 1.
Hydro-thermal operation: be dissolved in 80ml deionized water by 100mg graphene oxide, adds 10ml concentrated sulphuric acid (ρ=1.84g/
cm3), ultrasonic disperse 4 hours, transfer it in reactor, 190 DEG C of isothermal reactions 21 hours, it is thus achieved that three-dimensional column is also
Former graphene oxide, washing is collected.
Compound working procedure: by 0.2g ammonium molybdate, 0.2g Cys, 0.4g carbamide, be dissolved into mixed solvent (9ml water and
7ml DMF) in, 20mg three-dimensional redox graphene is joined in above-mentioned mixed solution, 40 DEG C are soaked 2 days, subsequently by it
Being transferred in reactor, 240 DEG C of isothermal reactions 20 hours, washed by product, 70 DEG C are vacuum dried 7 hours, collect and obtain two sulfur
Change molybdenum/graphene composite material.
Embodiment 5
The preparation method of graphite oxide is with embodiment 1.
Hydro-thermal operation: be dissolved in 80ml deionized water by 80mg graphene oxide, adds 12ml concentrated sulphuric acid (ρ=1.84g/
cm3), ultrasonic disperse 3 hours, transfer it in reactor, 220 DEG C of isothermal reactions 19 hours, it is thus achieved that three-dimensional column is also
Former graphene oxide, washing is collected.
Compound working procedure: by 0.3g sodium molybdate, 0.4g Cys, 0.7g carbamide, be dissolved into mixed solvent (8ml water and
8ml ethanol) in, 16mg three-dimensional redox graphene is joined in above-mentioned mixed solution, 60 DEG C are soaked 2 days, subsequently by it
Being transferred in reactor, 160 DEG C of isothermal reactions 24 hours, washed by product, 80 DEG C are vacuum dried 4 hours, collect and obtain two sulfur
Change molybdenum/graphene composite material.
Using the composite of embodiment 5 gained end product molybdenum bisuphide/Graphene as the negative pole material of lithium ion battery
Material, the mass ratio using composite, acetylene black and CMC is 80:5:15, is modulated into uniform pulpous state using water as solvent；Will slurry
Shape thing is applied on Copper Foil, with scraper by its even spread patches, is attached to copper foil surface equably.The coating made is put
In baking oven, dry 12 hours with 110 DEG C；Drying moves in vacuum drying oven after completing, and is vacuum dried 10 hours with 120 DEG C；
Again dried composite coating employing twin rollers or tablet machine etc. are carried out tabletting process；Use machinery slitter cutting
Electrode slice, using lithium sheet as to electrode, electrolyte is commercially available 1mol/L LiPF6/ EC+DMC solution, utilizes cell tester to enter
Row charge-discharge performance is tested, and products therefrom is as lithium ion battery negative material stable circulation under 100mA/g electric current density
Property test result is as shown in Figure 7.From accompanying drawing 7, the good cycling stability of battery, after circulating 100 times, battery capacity is the most steady
It is scheduled on 1140mAh/g.
Claims (11)
1. a preparation method for molybdenum bisuphide/graphene nanocomposite material, step includes:
A, hydro-thermal operation: graphite oxide is dispersed in water ultrasonic prepared graphene oxide solution, add sulphuric acid in solution, then
Ultrasonic it is mixed to get mixed liquor, then transfers to mixed liquor reactor reacts 18～30 hours at 160～260 DEG C, take
Going out washing, obtain three-dimensional column redox graphene, reaction condition preferably reacts 20～24 hours at 190～220 DEG C；
B, compound working procedure: molybdenum salt, sulfur source, carbamide are dissolved in the mixed solvent of water and organic solvent, are made into mixed solution, then
Three-dimensional column redox graphene is put in above-mentioned solution, soak more than 1 day at 3～60 DEG C, at preferably 10～30 DEG C
Soak 1～2 day；Finally mixed solution and three-dimensional column redox graphene are transferred in hydrothermal reaction kettle, 160～
Reacting at 240 DEG C 18～30 hours, preferably react 20～24 hours at 180～210 DEG C, product is scrubbed and dried,
To molybdenum bisuphide and graphene composite material i.e. molybdenum bisuphide/graphene nanocomposite material.
2. preparation method as claimed in claim 1, it is characterised in that: graphene oxide dense in mixed liquor in described step A
Degree is 0.75～1.5g/L, preferably 1.0～1.25g/L.
3. preparation method as claimed in claim 1, it is characterised in that: in described step A, in mixed liquor, the concentration of sulphuric acid is 0.8
～1.7mol/L, preferably 1.2～1.4mol/L.
4. preparation method as claimed in claim 1, it is characterised in that: in described step B, molybdenum salt is in sodium molybdate, ammonium molybdate
One or both, molybdenum salt concentration in mixed solution is 0.05～0.2mol/L, preferably 0.1～0.2mol/L.
5. preparation method as claimed in claim 1, it is characterised in that: in described step B, sulfur source is selected from thioacetamide, sulfur
One or more in urea, Cys, sulfur source concentration in mixed solution is 0.15～0.6mol/L, preferably 0.25～
0.4mol/L。
6. preparation method as claimed in claim 1, it is characterised in that: carbamide concentration in mixed solution in described step B
It is 0.15～0.6mol/L, preferably 0.3～0.5mol/L.
7. preparation method as claimed in claim 1, it is characterised in that: three-dimensional column redox graphene in described step B
Concentration in mixed solution is 0.1～4.0mg/mL, preferably 0.6～1.2mg/mL.
8. preparation method as claimed in claim 1, it is characterised in that: in described step B, organic solvent is in ethanol, DMF
One or both, preferably DMF；In described mixed solvent, water is 1:3～3:1 with the volume ratio of organic solvent, preferably 1:1～1:
2。
9. preparation method as claimed in claim 1, it is characterised in that: described step B is dried into vacuum drying, vacuum drying
Temperature 30～80 DEG C, drying time 4～12 hours, be preferably dried 6～10 hours at 40～60 DEG C.
10. a lithium ion battery negative, is made up of molybdenum bisuphide/graphene nanocomposite material.
11. 1 kinds of lithium ion batteries, by the lithium ion battery negative system including that molybdenum bisuphide/graphene nanocomposite material is made
Become.
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| CN107474469A (en) * | 2017-08-28 | 2017-12-15 | 浙江理工大学 | A kind of preparation method of the flexible sensor electrode of molybdenum disulfide quantum dot modification |
| CN108520832A (en) * | 2018-04-02 | 2018-09-11 | 哈尔滨工业大学 | SiQDs-MoS2/ rGO composite material and preparation methods and application |
| CN109065852A (en) * | 2018-07-04 | 2018-12-21 | 上海电气集团股份有限公司 | A kind of positive electrode and preparation method thereof |
| CN109904398A (en) * | 2017-12-08 | 2019-06-18 | 中国石油化工股份有限公司 | A kind of molybdenum disulfide/graphene composite material |
| CN110794006A (en) * | 2019-11-27 | 2020-02-14 | 西安交通大学 | Molybdenum disulfide-black phosphorus alkene composite material, preparation method and application thereof in NO2Application in gas sensing device |
| CN112939083A (en) * | 2021-02-07 | 2021-06-11 | 哈尔滨工业大学（威海） | Molybdenum disulfide/ferroferric oxide/graphene nanosheet composite wave absorber and preparation method thereof |
| CN113683861A (en) * | 2021-08-24 | 2021-11-23 | 江苏中科睿赛污染控制工程有限公司 | High-wear-resistance and high-thermal-conductivity composite material and preparation method and application thereof |
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| CN108520832A (en) * | 2018-04-02 | 2018-09-11 | 哈尔滨工业大学 | SiQDs-MoS2/ rGO composite material and preparation methods and application |
| CN109065852A (en) * | 2018-07-04 | 2018-12-21 | 上海电气集团股份有限公司 | A kind of positive electrode and preparation method thereof |
| CN110794006A (en) * | 2019-11-27 | 2020-02-14 | 西安交通大学 | Molybdenum disulfide-black phosphorus alkene composite material, preparation method and application thereof in NO2Application in gas sensing device |
| CN112939083A (en) * | 2021-02-07 | 2021-06-11 | 哈尔滨工业大学（威海） | Molybdenum disulfide/ferroferric oxide/graphene nanosheet composite wave absorber and preparation method thereof |
| CN113683861A (en) * | 2021-08-24 | 2021-11-23 | 江苏中科睿赛污染控制工程有限公司 | High-wear-resistance and high-thermal-conductivity composite material and preparation method and application thereof |
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