CN106207171B - A kind of preparation method of molybdenum disulfide/graphene nanocomposite material, negative electrode of lithium ion battery, lithium ion battery - Google Patents
A kind of preparation method of molybdenum disulfide/graphene nanocomposite material, negative electrode of lithium ion battery, lithium ion battery Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of molybdenum disulfide/graphene nanocomposite material, negative electrode of lithium ion battery, lithium ion battery, preparation method step includes hydro-thermal process, compound working procedure, preparation method of the present invention makes the molybdenum disulfide of sheet directly carry out growth in situ on the surface of graphene, and not only pattern is unique for this material；With very big specific surface area, solve the agglomeration traits of graphene and molybdenum disulfide, which is applied to lithium ion battery negative material, there is the advantages that good cycling stability, specific energy density is high.
Description
Technical field
The present invention relates to technical field of inorganic nanometer material, in particular to a kind of molybdenum disulfide/graphene nano composite wood
The preparation method of material, negative electrode of lithium ion battery, lithium ion battery.
Background technique
With environment worsening, energy problem is also increasingly prominent, in recent years for the research day of lithium-ion energy storage material
Gradually normalization.Lithium ion battery can make full use of renewable energy, while it is restricted to solve its as a kind of emerging energy storage tool
The problem of, lithium ion battery is low in cost, and energy storage capacity is good, high conversion efficiency, good cycling stability.
Molybdenum disulfide two-dimensional slice structure provides possibility for the more preferable deintercalation of lithium ion, while molybdenum disulfide has phase
To higher specific capacity (1334mAh/g), but since molybdenum disulfide poorly conductive and cyclical stability difference are to limit 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 a variety of groups such as carbonyl, carboxyl, it can be made multiple with other nano materials
It closes, three-dimensional graphene oxide has the advantages of three-dimensional grapheme, while carrying many groups, meets conducive to material.
Since graphene has the advantages that good conductivity, stable structure, molybdenum disulfide and graphene composite material become one
A research hotspot, such as Ye Jianbo et al. (J.Mater.Chem.A, 2015,3,6884-6893.) pass through simple hydro-thermal
Method has synthesized flaky molybdenum disulfide, such structure large specific surface area, good conductivity；Jeong Jae-Min et al. (Nanoscale,
2015,7,324-329.) MoS has been synthesized by simple method2@C core-shell structure, this material have for cathode of lithium battery
Superior cycle performance.
But there is also some problems as lithium ion battery negative material for graphene: graphene is easy to due to Van der Waals force
It is stacked into the transmission for influencing lithium ion together in graphene again again, and then the high rate performance of graphene is caused to decline.Therefore
Distinct methods are prepared with structural parameters and surface functional group, fault of construction, the heteroatom such as nitrogen, oxygen, hydrogen etc. of grapheme material
Its electrochemical lithium storage performance how is influenced to need to further investigate.In terms of graphene composite material, the overwhelming majority that reports at present
Graphene composite material is still being simply mixed for graphene and active material, and after multiple charge and discharge, active material may be with
Graphene separation, so as to cause performance of lithium ion battery decline.
Summary of the invention
In view of the shortcomings of the prior art, technical problem to be solved by the invention is to provide a kind of molybdenum disulfide/stones
The preparation method of black alkene nanocomposite, negative electrode of lithium ion battery, lithium ion battery, the present invention utilize cheap raw material system
It is standby to obtain three-dimensional column redox graphene, by immersion, compound, washing, drying, obtain multiple by molybdenum disulfide/graphene
Condensation material.The present invention provides a kind of work for the technical problems such as cyclical stability of the molybdenum disulfide as electrode material are improved
The composite material and preparation method thereof that skill is simple, yield is high, at low cost.
A kind of preparation method of molybdenum disulfide/graphene nanocomposite material, step include:
A, hydro-thermal process: graphite oxide is dispersed in water the obtained graphene oxide of ultrasound and holds liquid, sulphur is added into solution
Acid, then ultrasonic mixing obtain mixed liquor, and it is small that mixed liquor is then transferred in reaction kettle the reaction 18~30 at 160~260 DEG C
When, washing is taken out, obtains three-dimensional column redox graphene, it is small that reaction condition reacts 20~24 preferably at 190~220 DEG C
When；
Graphene oxide is by improving the synthesis of Hummers method, specific steps in the step A are as follows:
5.0g graphite and 3.75g NaNO are weighed respectively3It is put into the beaker of 1L, mechanical strong stirring is slowly added to
The concentrated sulfuric acid of 150mL stirs 0.5 hour, is slow added into the KMnO of 20g4, it adds within 0.5 hour, after continuing stirring 20 hours,
Since reactant viscosity increases, stops stirring, obtain the purplish red color substance of starchiness.After placing 5 days, it is respectively added slowly to 500mL
Deionized water and 30mLH2O2, solution colour becomes obvious glassy yellow at this time, after solution sufficiently reacts, centrifugation, washing,
Obtain graphite oxide.
The concentration of graphene oxide is 0.75~1.5g/L, preferably 1.0~1.25g/L in mixed liquor in the step A；
The concentration of sulfuric acid is 0.8~1.7mol/L, preferably 1.2~1.4mol/L in mixed liquor in the step A.
B, molybdenum salt, sulphur source, urea: being dissolved in the in the mixed solvent of water and organic solvent, is made into mixed solution by compound working procedure,
Then three-dimensional column redox graphene is put into above-mentioned solution, impregnates 1 day or more at 3~60 DEG C, preferably 10~30
It is impregnated 1~2 day at DEG C；Finally mixed solution and three-dimensional column redox graphene are transferred in hydrothermal reaction kettle, 160
It reacts 18~30 hours at~240 DEG C, is reacted 20~24 hours preferably at 180~210 DEG C, after product is washed and dry,
Obtain molybdenum disulfide and graphene composite material i.e. molybdenum disulfide/graphene nanocomposite material.
Molybdenum salt is selected from one or both of sodium molybdate, ammonium molybdate, concentration of the molybdenum salt in mixed solution in the step B
For 0.05~0.2mol/L, preferably 0.1~0.2mol/L；
Sulphur source is selected from one or more of thioacetamide, thiocarbamide, L-cysteine in the step B, and sulphur source is mixed
Closing the concentration in solution is 0.15~0.6mol/L, preferably 0.25~0.4mol/L；
Concentration of the urea in mixed solution is 0.15~0.6mol/L, preferably 0.3~0.5mol/L in the step B；
Concentration of the three-dimensional column redox graphene in mixed solution is 0.1~4.0mg/mL in the step B, excellent
Select 0.6~1.2mg/mL；
Organic solvent is selected from one or both of ethyl alcohol, DMF (N-N dimethylformamide) in the step B, preferably
DMF；The volume ratio of the in the mixed solvent water and organic solvent is 1:3~3:1, preferably 1:1~1:2；
It is dry to be dried in vacuo in the step B, 30~80 DEG C of vacuum drying temperature, drying time 4~12 hours, preferably
It is 6~10 hours dry at 40~60 DEG C.
A kind of negative electrode of lithium ion battery is made of molybdenum disulfide/graphene nanocomposite material；
A kind of lithium ion battery, including negative electrode of lithium ion battery made of molybdenum disulfide/graphene nanocomposite material
It is made.
Mechanism of the invention: the present invention using the three-dimensional redox graphene synthesized in hydrothermal step as template, by
Impregnated in mixed solution, the group on three-dimensional redox graphene will negative ions in adsorbent solution, then by molten
Agent thermal method carries out growth in situ again.
The present invention is immersed in molybdenum salt, sulphur source, urea using the three-dimensional redox graphene in hydro-thermal process as template
Mixed solution in, make the molybdenum disulfide of sheet directly carry out growth in situ on the surface of graphene by solvent-thermal method, it is this
Not only pattern is unique for material；With very big specific surface area, solve the agglomeration traits of graphene and molybdenum disulfide, which answers
For lithium ion battery negative material, there is the advantages that good cycling stability, specific energy density is high.
Compared with the prior art, the present invention has the following advantages:
(1) molybdenum disulfide/graphene nanocomposite material obtained by, molybdenum disulfide sheet are distributed on the surface of graphene
It is even；
(2) molybdenum disulfide obtained by/graphene nanocomposite material performance is stablized, in air not mutability, is easy
Storage；
(3) molybdenum disulfide/graphene nanocomposite material nanometer sheet thickness obtained by is small, product large specific surface area；
(4) molybdenum disulfide/graphene nanocomposite material obtained by is used as lithium ion battery negative material, has larger
Specific capacity and preferable cycle performance；
(5) experimentation is simple, low to experimental instrument and equipment requirement, and raw material is easy to get to expense is low, and it is raw can to carry out batch
It produces.
Detailed description of the invention
Fig. 1 is molybdenum disulfide/graphene composite material SEM figure prepared by embodiment 1.
Fig. 2 is molybdenum disulfide/graphene composite material SEM figure prepared by embodiment 2.
Fig. 3 is molybdenum disulfide/graphene composite material XRD diagram prepared by embodiment 2.
Fig. 4 is molybdenum disulfide/graphene composite material SEM figure prepared by embodiment 3.
Fig. 5 is molybdenum disulfide/graphene composite material SEM figure prepared by embodiment 4.
Fig. 6 is molybdenum disulfide/graphene composite material SEM figure prepared by embodiment 5.
Fig. 7 is that molybdenum disulfide/graphene composite material prepared by embodiment 5 exists as lithium ion battery negative material
Cyclical stability test chart under 100mA/g current density.
Specific embodiment
Embodiment 1
The preparation of graphite oxide: 5.0g graphite and 3.75g NaNO are weighed respectively3It is put into the beaker of 1L, mechanical strength is stirred
It mixes, is slowly added to the concentrated sulfuric acid of 150mL, stir 0.5 hour, be slow added into the KMnO of 20g4, add within 0.5 hour, continue to stir
After mixing 20 hours, reactant viscosity increases, and stops stirring, obtains the purplish red color substance of starchiness.After placing 5 days, slowly add respectively
Enter 500mL deionized water and 30mL H2O2, solution colour becomes obvious glassy yellow at this time, after solution sufficiently reacts, from
The heart, washing, obtain graphite oxide.
Hydro-thermal process: 70mg graphene oxide is dissolved in 80ml deionized water, and the 7ml concentrated sulfuric acid (ρ=1.84g/ is added
cm3), ultrasonic disperse 3 hours, transfer it in reaction kettle, 190 DEG C isothermal reaction 23 hours, obtain three-dimensional column also
Original oxidation graphene oxide, washing are collected.
Compound working procedure: by 0.4g sodium molybdate, 0.3g thiocarbamide, 0.2g urea is dissolved into mixed solvent (8ml water and 8ml
DMF in), 14mg three-dimensional redox graphene is add to the above mixed solution, 3 DEG C are impregnated 3 days, are then transferred to
In reaction kettle, 210 DEG C isothermal reaction 30 hours, product is washed, 60 DEG C be dried in vacuo 7 hours, collection obtain molybdenum disulfide/stone
Black alkene composite material.
Embodiment 2
The preparation method is the same as that of Example 1 for graphite oxide.
Hydro-thermal process: 120mg graphene oxide is dissolved in 80ml deionized water, and the 6ml concentrated sulfuric acid (ρ=1.84g/ is added
cm3), ultrasonic disperse 2 hours, transfer it in reaction kettle, 160 DEG C isothermal reaction 20 hours, obtain three-dimensional column also
Original oxidation graphene oxide, washing are collected.
Compound working procedure: by 0.5g ammonium molybdate, 0.4g thioacetamide, 0.5g urea, be dissolved into mixed solvent (4ml water and
12ml DMF) in, 24mg three-dimensional redox graphene is add to the above mixed solution, 10 DEG C are impregnated 1 day, then by it
Be transferred in reaction kettle, 200 DEG C isothermal reaction 18 hours, product is washed, 30 DEG C be dried in vacuo 12 hours, collection obtain two sulphur
Change molybdenum/graphene composite material.
Embodiment 3
The preparation method is the same as that of Example 1 for graphite oxide.
Hydro-thermal process: 90mg graphene oxide is dissolved in 80ml deionized water, and the 9ml concentrated sulfuric acid (ρ=1.84g/ is added
cm3), ultrasonic disperse 3 hours, transfer it in reaction kettle, 260 DEG C isothermal reaction 30 hours, obtain three-dimensional column also
Former graphene oxide, washing are collected.
Compound working procedure: by 0.6g sodium molybdate, 0.7g thiocarbamide, 0.6g urea is dissolved into mixed solvent (12ml water and 4ml second
Alcohol) in, 18mg three-dimensional redox graphene is add to the above mixed solution, 30 DEG C are impregnated 3 days, are then transferred to
In reaction kettle, 180 DEG C isothermal reaction 30 hours, product is washed, 40 DEG C be dried in vacuo 12 hours, collection obtain molybdenum disulfide/
Graphene composite material.
Embodiment 4
The preparation method is the same as that of Example 1 for graphite oxide.
Hydro-thermal process: 100mg graphene oxide is dissolved in 80ml deionized water, and the 10ml concentrated sulfuric acid (ρ=1.84g/ is added
cm3), ultrasonic disperse 4 hours, transfer it in reaction kettle, 190 DEG C isothermal reaction 21 hours, obtain three-dimensional column also
Former graphene oxide, washing are collected.
Compound working procedure: by 0.2g ammonium molybdate, 0.2g L-cysteine, 0.4g urea, be dissolved into mixed solvent (9ml water and
7ml DMF) in, 20mg three-dimensional redox graphene is add to the above mixed solution, 40 DEG C are impregnated 2 days, then by it
Be transferred in reaction kettle, 240 DEG C isothermal reaction 20 hours, product is washed, 70 DEG C be dried in vacuo 7 hours, collection obtain two sulphur
Change molybdenum/graphene composite material.
Embodiment 5
The preparation method is the same as that of Example 1 for graphite oxide.
Hydro-thermal process: 80mg graphene oxide is dissolved in 80ml deionized water, and the 12ml concentrated sulfuric acid (ρ=1.84g/ is added
cm3), ultrasonic disperse 3 hours, transfer it in reaction kettle, 220 DEG C isothermal reaction 19 hours, obtain three-dimensional column also
Former graphene oxide, washing are collected.
Compound working procedure: by 0.3g sodium molybdate, 0.4g L-cysteine, 0.7g urea, be dissolved into mixed solvent (8ml water and
8ml ethyl alcohol) in, 16mg three-dimensional redox graphene is add to the above mixed solution, 60 DEG C are impregnated 2 days, then by it
Be transferred in reaction kettle, 160 DEG C isothermal reaction 24 hours, product is washed, 80 DEG C be dried in vacuo 4 hours, collection obtain two sulphur
Change molybdenum/graphene composite material.
Using 5 gained final product molybdenum disulfide of embodiment/graphene composite material as the cathode material of lithium ion battery
Material, is used the mass ratio of composite material, acetylene black and CMC for 80:5:15, uniform pulpous state is modulated into using water as solvent；It will slurry
Shape object is applied on copper foil, with scraper by its even spread patches, is equably attached to copper foil surface.Manufactured coating is put
In baking oven, dried 12 hours with 110 DEG C；It moves into vacuum oven after the completion of drying, is dried in vacuo 10 hours with 120 DEG C；
The composite coating after drying is subjected to compressing tablet process using twin rollers or tablet press machine etc. again；It is cut using mechanical slitter
Electrode slice, using lithium piece as to electrode, electrolyte is commercially available 1mol/L LiPF6/ EC+DMC solution, using cell tester into
The test of row charge-discharge performance, stable circulation of the products therefrom as lithium ion battery negative material under 100mA/g current density
Property test result is as shown in Fig. 7.By attached drawing 7 as it can be seen that the good cycling stability of battery, battery capacity is still steady after recycling 100 times
It is scheduled on 1140mAh/g.
Claims (11)
1. a kind of preparation method of molybdenum disulfide/graphene nanocomposite material, step include:
A, hydro-thermal process: being dispersed in water the obtained graphene oxide solution of ultrasound for graphite oxide, sulfuric acid be added into solution, then
Ultrasonic mixing obtains mixed liquor, and then mixed liquor is transferred in reaction kettle and is reacted 18~30 hours at 160~260 DEG C, is taken
It washs out, obtains three-dimensional column redox graphene, reaction condition reacts 20~24 hours preferably at 190~220 DEG C；
B, molybdenum salt, sulphur source, urea: being dissolved in the in the mixed solvent of water and organic solvent by compound working procedure, is made into mixed solution, then
Three-dimensional column redox graphene is put into above-mentioned solution, is impregnated at 1 day or more, preferably 10~30 DEG C at 3~60 DEG C
It impregnates 1~2 day；Finally mixed solution and three-dimensional column redox graphene are transferred in hydrothermal reaction kettle, 160~
It reacts 18~30 hours at 240 DEG C, is reacted 20~24 hours preferably at 180~210 DEG C, after product is washed and dry, obtained
To molybdenum disulfide and graphene composite material, that is, molybdenum disulfide/graphene nanocomposite material.
2. preparation method as described in claim 1, it is characterised in that: in the step A in mixed liquor graphene oxide it is dense
Degree is 0.75~1.5g/L, preferably 1.0~1.25g/L.
3. preparation method as described in claim 1, it is characterised in that: the concentration of sulfuric acid is 0.8 in mixed liquor in the step A
~1.7mol/L, preferably 1.2~1.4mol/L.
4. preparation method as described in claim 1, it is characterised in that: molybdenum salt is in sodium molybdate, ammonium molybdate in the step B
One or two, concentration of the molybdenum salt in mixed solution be 0.05~0.2mol/L, preferably 0.1~0.2mol/L.
5. preparation method as described in claim 1, it is characterised in that: sulphur source is selected from thioacetamide, sulphur in the step B
One or more of urea, L-cysteine, concentration of the sulphur source in mixed solution be 0.15~0.6mol/L, preferably 0.25~
0.4mol/L。
6. preparation method as described in claim 1, it is characterised in that: concentration of the urea in mixed solution in the step B
For 0.15~0.6mol/L, preferably 0.3~0.5mol/L.
7. preparation method as described in claim 1, it is characterised in that: three-dimensional column redox graphene in the step B
Concentration in mixed solution is 0.1~4.0mg/mL, preferably 0.6~1.2mg/mL.
8. preparation method as described in claim 1, it is characterised in that: organic solvent is in ethyl alcohol, DMF in the step B
One or two, preferably DMF；The volume ratio of the in the mixed solvent water and organic solvent is 1:3~3:1, preferably 1:1~1:
2。
9. preparation method as described in claim 1, it is characterised in that: dry for vacuum drying, vacuum drying in the step B
It is 30~80 DEG C of temperature, drying time 4~12 hours, 6~10 hours dry preferably at 40~60 DEG C.
10. a kind of negative electrode of lithium ion battery, the molybdenum disulfide/graphene nano prepared by preparation method described in claim 1
Composite material is made.
11. a kind of lithium ion battery, by the molybdenum disulfide/graphene nano for including preparation method described in claim 1 preparation
Negative electrode of lithium ion battery made of composite material is made.
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| 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 |
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| 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 |
| CN110794006B (en) * | 2019-11-27 | 2021-05-28 | 西安交通大学 | Molybdenum disulfide-black phosphorus alkene composite material in NO2Application in gas sensing device |
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| CN104857976A (en) * | 2015-04-03 | 2015-08-26 | 浙江理工大学 | Three-dimensional molybdenum disulfide nanoflower-graphene composite material and application thereof |
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| 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 |
| CN102142551A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Graphene nano sheet/MoS2 composite nano material and synthesis method thereof |
| CN103094563A (en) * | 2013-01-08 | 2013-05-08 | 哈尔滨工程大学 | Graphene and MoS2 nano-composite with three-dimensional structure and preparation method and application |
| CN104617300A (en) * | 2015-02-09 | 2015-05-13 | 天津师范大学 | Method for preparing lithium ion battery anode/cathode material from reduced graphene oxide |
| CN104857976A (en) * | 2015-04-03 | 2015-08-26 | 浙江理工大学 | Three-dimensional molybdenum disulfide nanoflower-graphene composite material and application thereof |
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