CN104600315A - Flake MoS2/graphene composite aerogel and preparation method thereof - Google Patents
Flake MoS2/graphene composite aerogel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a flake MoS2/graphene composite aerogel and a preparation method thereof and belongs to the technical field of anode materials of lithium ion batteries. The preparation method comprises the following steps: ultrasonically dispersing a certain quantity of graphene oxide solution into deionized water, adding a certain quantity of water-soluble molybdate and thiourea, then adding 0.1-3mL organic amine solution, taking out a cylindrical product after hydrothermal reaction at the temperature of 160-240 DEG C, freeze-drying, and then carrying out thermal treatment for 2h in the mixed atmosphere of argon and hydrogen at the temperature of 800 DEG C to obtain the flake MoS2/graphene composite aerogel. According to the flake MoS2/graphene composite aerogel and the preparation method thereof disclosed by the invention, thin layers of graphene are connected with one another in a staggering mode to form a three-dimensional ordered conductive network and form micron pore canals, MoS2 is uniformly dispersed on the ultra-large superficial area, and thus, the problems of volume expansion and crushing materials are effectively solved; meanwhile, the structure stability and the cycle performance of the flake MoS2/graphene composite aerogel, serving as the anode material, are improved.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, particularly a kind of sheet MoS
2/ Graphene composite aerogel and preparation method thereof, belongs to inorganic composite nano material, technical field of lithium ion battery electrode.
Background technology
Chemical power source realizes the device that electric energy and chemical energy change mutually, is can the important medium of more reasonable energy utilization.The excellent properties such as the lithium ion battery of a new generation has that operating voltage is high, volume is little, specific capacity is high, lightweight, memory-less effect.Commercial Li-ion battery many employings material with carbon element is as negative pole, graphite is good cyclical stability because design feature has, but its shortcoming also can not be ignored, first the restriction of theoretical capacity can not adapt to the requirement of height ratio capacity, secondly intercalation potential and lithium metal sedimentation potential close, lithium metal may produce dendrite at electrode surface and separate out, concerning battery, have safety issue.In recent years about the large quantity research of negative material also round raising battery capacity, strengthen the cyclical stability of battery and improve security performance and launch, iting is desirable to meet social demand.
Graphene is as a kind of New Type of Carbon material of preparation by graphite, individual layer or thin layer graphite (multi-layer graphenes of 2 ~ 10 layers) have good conductivity, chemical stability and wide electrochemical window, get a good chance of being applied in high power capacity lithium storage materials.With graphite-phase ratio, Graphene has very large specific area (2600m
2/ g), and the conductivity of superelevation is more conducive to the deintercalation of lithium ion.Therefore, Graphene becomes the focus of research in the application of high-capacity lithium ion cell.
The discovery of Graphene makes people to the MoS of structural similarity with it
2create great interest.Molybdenum bisuphide is as cell negative electrode material, although there is higher capacity, but owing to having obvious deformation at Lithium-ion embeding with when deviating from, to cause after repeatedly discharge and recharge capacity attenuation than very fast, cyclical stability is bad, and simultaneously because molybdenum bisuphide is semi-conducting material, its electronic conductivity is lower, therefore need to select to strengthen the deformation that produces when molybdenum bisuphide structural stability alleviates lithiumation and de-lithium, have again material compared with high conductivity to carry out compound.
For above-mentioned shortcoming, this patent is by a kind of sheet MoS of one-step method Hydrothermal Synthesis
2/ Graphene aerogel composite.Form Graphene being prepared into aeroge is not only conducive to making full use of its surface area, can also improve its conductivity at Inner Constitution three-dimensional conductive network.Therefore, if preparation MoS
2with the composite material of graphene aerogel, the high conductivity of graphene aerogel can improve the electric conductivity of composite material further, is conducive to the electron transmission in electrochemical electrode reaction, the chemical property of reinforced composite.In addition, this special three-dimensional porous structure can very easily be infiltrated by electrolyte, improves the chemical property of composite material.
Summary of the invention
The object of the invention is, provides a kind of sheet MoS
2/ Graphene composite aerogel and preparation method thereof, this composite material is made up of graphene aerogel and flaky molybdenum disulfide compound, effectively improves conductivity and the structural stability of electrode, improves multiplying power charge and discharge and the cycle performance of material.
For achieving the above object, the present invention adopts following technical scheme:
A kind of sheet MoS
2/ Graphene composite aerogel, to have the graphene aerogel of tridimensional network for conducting matrix grain, MoS
2nanometer sheet is dispersed on crosslinked graphene sheet layer uniformly, sheet MoS
2be of a size of 200-500nm.
A kind of sheet MoS
2the preparation method of/Graphene composite aerogel, comprises the steps:
A () measures 15 ~ 50mL concentration is that the graphene oxide solution of 3mg/mL is poured in the beaker of 100mL, adds appropriate amount of deionized water magnetic agitation, mixes;
B () takes 0.3 ~ 2g water-soluble molybdenum hydrochlorate and is dissolved in 15mL deionized water, the ratio of the amount of substance of molybdate and graphene oxide is 0.2:1 ~ 1:1, magnetic agitation 20min, pours in the graphene oxide solution in step (a);
C () takes 0.5 ~ 2.5g thiocarbamide and is dissolved in 15mL deionized water, pour in the solution of step (b) gained, magnetic agitation 1h;
D () measures in the mixed solution that 0.1 ~ 3mL By Amine Solutions pours in step (c), magnetic agitation 20min;
E the mixed solution of step (d) gained proceeds in polytetrafluoro water heating kettle by (), at 160 DEG C ~ 240 DEG C, keep 10 ~ 25h, room temperature is down to by question response still, cylindric product is taken out washing, alcohol wash each three times, lyophilized overnight at-52 DEG C;
F (), by the solid product of step (e) gained 800 DEG C of heat treatment 2h in argon gas/hydrogen mixed gas atmosphere, namely obtains sheet MoS
2/ Graphene aerogel composite.
Described step (b) is stoichiometrically prepared burden with the molybdate described in step (c) and thiocarbamide.
Compare with existing technology, method of the present invention has following outstanding feature:
(1) this experiment is by realizing the compound of molybdenum bisuphide and graphene aerogel with the synchronous reduction of graphene oxide, by special construction and the fabulous electrical conductance of Graphene, carry out the deformation of stable molybdenum bisuphide in charge and discharge process, improve its stability, strengthen its electrical conductance.
(2) found by TEM test, MoS
2be evenly distributed on graphene aerogel, size is about 200-500nm.This structure effectively can alleviate MoS
2volumetric expansion in charge and discharge process, avoids the rapid decay of capacity after repeatedly discharge and recharge.
(3) MoS
2/ Graphene aerogel composite charge/discharge capacity is high, good rate capability, and cycle performance is excellent.The composite material that synthesis obtains and lithium sheet are assembled into half-cell and test, and with the electric discharge of 100mA/g current density, discharge capacity reaches 1035.6mAh/g first.
(4) curing molybdenum layer and the rare aeroge of graphite form new heterogeneous interlayer structure, and this heterogeneous interlayer structure newly certainly exists new interaction, thus give composite nano materials new performance.
Accompanying drawing explanation
Fig. 1 is MoS
2the XRD collection of illustrative plates of/Graphene aerogel composite.
Fig. 2 is MoS
2the SEM picture of/Graphene aerogel composite.
Fig. 3 is MoS
2the TEM picture of/Graphene aerogel composite.
Fig. 4 is MoS
2the charging and discharging curve figure of/Graphene aerogel composite.
Fig. 5 is MoS
2the cycle performance figure of/Graphene aerogel composite.
Embodiment
The present invention is further illustrated below by embodiment.
embodiment 1
The graphene oxide used adopts Conventional processing methods to obtain, and its preparation method is as follows:
By potassium peroxydisulfate (K
2s
2o
8) 2.5g, phosphorus pentoxide (P
2o
5) 2.5g, be dissolved in the 12mL concentrated sulfuric acid, be heated to 80 DEG C; Then 3g native graphite is added above-mentioned solution, be incubated 80 DEG C, 4.5 hours; Be cooled to room temperature, after the dilution of 500mL deionized water, hold over night; Filter, remove residual acid with 0.2mmfilter is floating; Dry in 60 DEG C of vacuum drying chambers; The pre-oxidation thing obtained is joined in the concentrated sulfuric acid of 120mL ice bath, under agitation slowly adds 15gKMnO
4, in the process added, maintain the temperature at less than 20 DEG C.Then be that temperature controls to stir 2h at 35 DEG C.Add the dilution of 250mL deionized water, temperature in dilution, also will be made in ice bath lower than 50 DEG C.Stir 2h again, then add 0.7L deionized water, and add the H of 20mL30% at once
2o
2, mixture produces bubble, and color becomes glassy yellow by brown, reaction terminating after about 0.5h.Said mixture is filtered, and washs with the 1:10 watery hydrochloric acid of 1L, filter to remove part metals ion; Filter with 1L water washing, to remove unnecessary acid again; By above-mentioned solubilize in 1L water, then ultrasonic about 0.5h under 100W ultrasonic power, obtains graphene oxide solution (GO).
preparation sheet MoS
2
/ Graphene aerogel composite:
1) measuring 15mL concentration is that the graphene oxide solution of 3mg/mL is poured in the beaker of 100mL, adds 10mL deionized water magnetic agitation 30min and mixes;
2) taking 0.31g sodium molybdate is dissolved in 15mL deionized water, and magnetic agitation 20min pours in the graphene oxide solution in step 1);
3) taking 0.47g thiocarbamide is dissolved in 15mL deionized water, and thiocarbamide is sulphur source is also reducing agent, and magnetic agitation 20min, pours step 2 into) in the solution of gained, magnetic agitation 1h;
4) measuring 0.1mL1-propylamine solution pours in the mixed solution in step 3), magnetic agitation 20min;
5) proceed in polytetrafluoro water heating kettle by the mixed solution of step 4) gained, at 160 DEG C, keep 25h, room temperature is down to by question response still, and cylindric product is taken out washing, alcohol wash each three times; The cylindric product of gained is put into freeze drier, lyophilized overnight at-52 DEG C.
6) by the solid product of step 5) gained 800 DEG C of heat treatment 2h in argon gas/hydrogen mixed gas atmosphere, namely sheet MoS is obtained
2/ Graphene aerogel composite.
sheet MoS
2
the electric performance test method of/Graphene aerogel composite:
Gained aeroge being cut into the thick disk of about 1mm, being then pressed on copper mesh under a certain pressure, is to electrode with metal lithium sheet, is assembled into CR2032 type button cell and carries out experiment test.
As shown in Figure 1, the present invention has successfully prepared MoS to the XRD of product as seen from the figure
2/ Graphene aerogel composite, MoS
2diffraction peak and bibliographical information consistent, there is no other impurity phases as seen from the figure in compound product.Fig. 2 is ESEM (SEM) photo of obtained composite material, can find out MoS
2/ Graphene aerogel composite is three-dimensional net structure, aperture be 0.6 ~ 3 μm not etc.Fig. 3 is transmission electron microscope (TEM) photo, can find out sheet MoS
2well be dispersed on Graphene.Fig. 4 is the charging and discharging curve of composite material in 0.005 ~ 3.0V voltage range, and the first charge-discharge specific capacity of this material under 100mA/g current density is respectively 1045mAh/g and 837mAh/g.Fig. 5 is the cycle performance figure of this composite material when 100mA/g, and after 50 circulations, specific discharge capacity still has 590mAh/g, illustrates that this composite material has higher specific capacity and good cyclical stability.
embodiment 2
The preparation method of graphene oxide is with embodiment 1.
preparation sheet MoS
2
/ Graphene aerogel composite:
1) measuring 25mL concentration is that the graphene oxide solution of 3mg/mL is poured in the beaker of 100mL, adds 20mL deionized water magnetic agitation 30min and mixes;
2) taking 0.45g ammonium molybdate is dissolved in 15mL deionized water, and magnetic agitation 20min pours in the graphene oxide solution in step 1);
3) taking 0.57g thiocarbamide is dissolved in 15mL deionized water, and thiocarbamide is sulphur source is also reducing agent, and magnetic agitation 20min, pours step 2 into) in the solution of gained, magnetic agitation 1h;
4) measure in the mixed solution that 1mL ethylenediamine solution pours in step 3), magnetic agitation 20min;
5) proceed in polytetrafluoro water heating kettle by the mixed solution of step 4) gained, at 200 DEG C, keep 20h, room temperature is down to by question response still, and cylindric product is taken out washing, alcohol wash each three times; The cylindric product of gained is put into freeze drier, lyophilized overnight at-52 DEG C.
6) by the solid product of step 5) gained 800 DEG C of heat treatment 2h in argon gas/hydrogen mixed gas atmosphere, namely sheet MoS is obtained
2/ Graphene aerogel composite.
Electric performance test method is with embodiment 1.
embodiment 3
The preparation method of graphene oxide is with embodiment 1.
preparation sheet MoS
2
/ Graphene aerogel composite:
1) measuring 50mL concentration is that the graphene oxide solution of 3mg/mL is poured in the beaker of 100mL, adds 40mL deionized water magnetic agitation 30min and mixes;
2) taking 0.91g sodium molybdate is dissolved in 15mL deionized water, and magnetic agitation 20min pours in the graphene oxide solution in step 1);
3) taking 1.14g thiocarbamide is dissolved in 15mL deionized water, and thiocarbamide is sulphur source is also reducing agent, and magnetic agitation 20min, pours step 2 into) in the solution of gained, magnetic agitation 1h;
4) measure in the mixed solution that 3mL triethylamine solution pours in step 3), magnetic agitation 20min;
5) proceed in polytetrafluoro water heating kettle by the mixed solution of step 4) gained, at 200 DEG C, keep 25h, room temperature is down to by question response still, and cylindric product is taken out washing, alcohol wash each three times; The cylindric product of gained is put into freeze drier, lyophilized overnight at-52 DEG C.
6) by the solid product of step 5) gained 800 DEG C of heat treatment 2h in argon gas/hydrogen mixed gas atmosphere, namely sheet MoS is obtained
2/ Graphene aerogel composite.
Electric performance test method is with embodiment 1.
embodiment 4
The preparation method of graphene oxide is with embodiment 1.
preparation sheet MoS
2
/ Graphene aerogel composite:
1) measuring 30mL concentration is that the graphene oxide solution of 3mg/mL is poured in the beaker of 100mL, adds 30mL deionized water magnetic agitation 30min and mixes;
2) taking 2g sodium molybdate is dissolved in 15mL deionized water, and magnetic agitation 20min pours in the graphene oxide solution in step 1);
3) taking 2.5g thiocarbamide is dissolved in 15mL deionized water, and thiocarbamide is sulphur source is also reducing agent, and magnetic agitation 20min, pours step 2 into) in the solution of gained, magnetic agitation 1h;
4) measuring 2mL diethylenetriamines solution pours in the mixed solution in step 3), magnetic agitation 20min;
5) proceed in polytetrafluoro water heating kettle by the mixed solution of step 4) gained, at 240 DEG C, keep 10h, room temperature is down to by question response still, and cylindric product is taken out washing, alcohol wash each three times; The cylindric product of gained is put into freeze drier, lyophilized overnight at-52 DEG C.
6) by the solid product of step 5) gained 800 DEG C of heat treatment 2h in argon gas/hydrogen mixed gas atmosphere, namely sheet MoS is obtained
2/ Graphene aerogel composite.
Electric performance test method is with embodiment 1.
Claims (3)
1. a sheet MoS
2/ Graphene composite aerogel, is characterized in that, to have the graphene aerogel of tridimensional network for conducting matrix grain, MoS
2nanometer sheet is dispersed on crosslinked graphene sheet layer uniformly, sheet MoS
2be of a size of 200-500nm.
2. a sheet MoS
2the preparation method of/Graphene composite aerogel, is characterized in that, comprises the steps:
A () measures 15 ~ 50mL concentration is that the graphene oxide solution of 3mg/mL is poured in the beaker of 100mL, adds appropriate amount of deionized water magnetic agitation, mixes;
B () takes 0.3 ~ 2g water-soluble molybdenum hydrochlorate and is dissolved in 15mL deionized water, the ratio of the amount of substance of molybdate and graphene oxide is 0.2:1 ~ 1:1, magnetic agitation 20min, pours in the graphene oxide solution in step (a);
C () takes 0.5 ~ 2.5g thiocarbamide and is dissolved in 15mL deionized water, pour in the solution of step (b) gained, magnetic agitation 1h;
D () measures in the mixed solution that 0.1 ~ 3mL By Amine Solutions pours in step (c), magnetic agitation 20min;
E the mixed solution of step (d) gained proceeds in polytetrafluoro water heating kettle by (), at 160 DEG C ~ 240 DEG C, keep 10 ~ 25h, room temperature is down to by question response still, cylindric product is taken out washing, alcohol wash each three times, lyophilized overnight at-52 DEG C;
F (), by the solid product of step (e) gained 800 DEG C of heat treatment 2h in argon gas/hydrogen mixed gas atmosphere, namely obtains sheet MoS
2/ Graphene aerogel composite.
3. sheet MoS according to claim 2
2the preparation method of/Graphene composite aerogel, is characterized in that, described step (b) is stoichiometrically prepared burden with the molybdate described in step (c) and thiocarbamide.
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