CN108039459A - A kind of preparation method of yolk-shell structures molybdenum disulfide@carbon electrode materials - Google Patents
A kind of preparation method of yolk-shell structures molybdenum disulfide@carbon electrode materials Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of yolk shell structures molybdenum disulfide@carbon electrode materials.Utilize molybdenum disulfide presoma solvent heat（Ethylene glycol）Obtain single dispersing molybdenum disulfide nano ball；Dopamine obtains molybdenum disulfide@poly-dopamine core shell structures in the auto polymerization of molybdenum disulfide particles interface, and molybdenum disulfide@poly-dopamines progress high temperature cabonization is handled to obtain core shell structure molybdenum disulfide@carbon nano-particles；Molybdenum disulfide@carbon is dispersed in hydrogen peroxide solution, yolk shell structure molybdenum disulfide@carbon materials are obtained through hydrogen peroxide etching processing.Gap between molybdenum disulfide and carbon shell can realize good regulation and control by adjusting the concentration of hydrogen peroxide.When the concentration of hydrogen peroxide is 0.4 vol%, the yolk shell structure molybdenum disulfide@carbon lithium ions battery cathode being prepared is up to 1167 mAh g in the specific discharge capacity of the second circle‑1, the specific discharge capacity after 200 circle circulations is 880mAh g‑1, capacity retention ratio 75.4%, and its high rate performance protrudes.
Description
Technical field
The present invention relates to a kind of controllable yolk-shell structure molybdenum disulfide@carbon lithium ion batteries in simple preparation gap
The method of negative material, is specifically that a kind of add etches agent hydrogen peroxide to etch the preparation method of core shell structure molybdenum disulfide carbon,
Belong to field of nanocomposite materials.
Background technology
In decades recently, the reserves of conventional energy resource are constantly being reduced, and have triggered a series of global crisis and society to ask
Topic.For this reason, the regenerative resource including solar energy, wind energy, water energy, Hydrogen Energy etc. is developed.And these energy
Use need efficient equipment that it is stored and changed in a manner of electric energy.In energy conversion field, including battery, super electricity
Energy storage device including container, the research of particularly electrode material is the most important thing.With to MoS2Deng metal sulfide two dimension
The discovery and further investigation of material, its property and excellent chemical property open for exploitation high performance lithium ion battery
One new road.
Molybdenum disulfide is a kind of typical graphite-like structure material, it attracts heap by two-dimentional S-Mo-S lamellas through Van der Waals force
It is folded to form.In negative electrode of lithium ion battery material, molybdenum disulfide has high theoretical specific capacity due to four electron transfer reaction mechanism
669 mAh g-1.However, molybdenum disulfide is but limited to its poorly conductive, Yi Ji as the practical application of ion cathode material lithium
The volumetric expansion of embedding reason process（It causes electrode dusting, active material to come off from collector, finally so that electrode cycle is stablized
Property is poor, high rate performance is poor）.In order to solve the problems, such as these, people have done numerous studies, can be summarized as following two solutions
Scheme：（1）Reduce molybdenum disulphide particles size, the pattern of molybdenum disulphide particles, such as molybdenum disulfide are designed on nanoscale
Nanometer sheet, nanosphere, nano flower, nanotube.This method alleviates of molybdenum disulfide volumetric expansion generation to a certain extent
Power, shorten lithium ion mobility distance, facilitate Lithium-ion embeding/abjection.（2）It is compound with other conductive materials, structure electric conductivity and
Structural stability more preferably compound, such as molybdenum disulfide/graphene, molybdenum disulfide/carbon nanotubes, molybdenum disulfide/carbon, curing
Molybdenum/conducting polymer.
Molybdenum-disulfide radical nanosizing hollow structure materials application has unique advantage when lithium ion battery negative material：
（a）The volumetric expansion that gap can be given after embedding reason provides sufficient space；（b）Prevent nano particle from assembling；（c）With bigger
Electrode/electrolyte interface；（d）Shorten lithium ion diffusion admittance.However, in past research, hollow structure material due to
Its pore size is difficult control and causes invalid void space to reduce particle density, and the volume energy for ultimately resulting in electrode is close
Degree/power density is lost.And we have successfully prepared the yolk-shell structures MoS of size uniformity here2@C nanos ball electricity
Pole material, it can be very good to overcome problem above.This nano particle is by molybdenum disulfide（yolk）, carbon shell and intermediate gaps group
Into it has the advantages that prominent：Particle size is homogeneous, intermediate gaps size can easily be accommodated, carbon shell reinforcing material electric conductivity and fills
Work as cushion.Therefore, when the concentration of hydrogen peroxide is 0.4 vol%, the yolk-shell structure molybdenum disulfide@carbon that is prepared
With optimal pore size, 1167 mAh g are up in the specific discharge capacity of the second circle when it is used as negative electrode of lithium ion battery-1,
Specific discharge capacity after 200 circle circulations is 880mAh g-1, capacity retention ratio 75.4%, and high rate performance protrudes.
The content of the invention
It is an object of the invention to provide one kind can significantly improve molybdenum-disulfide radical lithium ion battery negative material electrification
Learn the preparation method of the yolk-shell structure molybdenum disulfide@carbon electrode materials of performance.
The present invention in ethylene glycol by adding presoma sulphur and molybdenum trioxide, by obtaining molybdenum disulfide after solvent heat
Nanosphere, then dopamine is in the auto polymerization of molybdenum disulfide interface, by obtaining core shell structure MoS after high temperature cabonization2@C nanos
Particle, finally obtains the adjustable yolk-shell structures MoS of intermediate gaps by hydrogen peroxide solution etching processing2@C nano materials
Material.When the concentration of hydrogen peroxide is 0.4 vol%, the yolk-shell structure molybdenum disulfide@carbon lithium ion batteries being prepared are born
Pole material is 1167 mAh g in the specific discharge capacity of the second circle-1, the specific discharge capacity after 200 circle circulations is 880mAh
g-1, capacity retention ratio 75.4%, and high rate performance protrudes, and is the best molybdenum-disulfide radical lithium-ion electric of current chemical property
One of pond negative material.
The present invention adopts the following technical scheme that realization：
A kind of preparation method of yolk-shell structures molybdenum disulfide@carbon electrode materials proposed by the present invention, comprises the following steps that：
（1）5 ~ 36mmol elemental sulfurs and 2 ~ 15mmol molybdenum trioxides are added in the solvent ethylene glycol solution of 300 ml, water-bath
Uniform solution is formed after 10 min of ultrasound；Then polytetrafluoroethylene (PTFE) high pressure that the uniform solution of formation is transferred to 500 ml is anti-
Answer in kettle, be put into the baking oven that temperature is 200 DEG C and react 12 h, obtain product molybdenum disulfide nano ball, its a diameter of 280nm；
（2）Take 800 mg steps（1）Obtained molybdenum disulfide nano ball is dispersed in the Tris buffer solutions of 200 ml（10 mM, pH
=8.5）In, add 200mg dopamines and stir 12 h, obtain molybdenum disulfide@poly-dopamines；Molybdenum disulfide@poly-dopamines are put into
It is 5 DEG C/min, protective gas N in heating rate in tube furnace2, temperature be carbonized 2 h under the conditions of being 800 DEG C, obtain nucleocapsid knot
Structure molybdenum disulfide@carbon；
（3）Hydrogen peroxide solution is configured, then adds 200mg steps（2）The core shell structure molybdenum disulfide@carbon of gained, is vigorously stirred 1
H, obtains final product yolk-shell structure molybdenum disulfide@carbon.
In the present invention, step（1）The molar ratio of middle sulphur and molybdenum trioxide is 12：5.
In the present invention, step（3）Described in hydrogen peroxide concentration be 0.05-3 vol %.
The beneficial effects of the present invention are：The molybdenum disulfide nano ball size uniformity that solvent heat is prepared, and particle ruler
Very little small, this can effectively improve the migration rate of lithium ion in the electrodes, be conducive to improve its high rate performance.Pass through dopamine
The mode of auto polymerization and then high temperature cabonization can improve material in one layer of carbon shell of molybdenum disulfide particles coated with uniform, carbon shell
Electric conductivity, and can be very good to prevent nanometer MOS 2 particle from reassociating.Finally hydrogen peroxide is innovatively used as etching agent
It is adjoint embedding when it can give battery discharge to prepare the adjustable yolk-shell structures molybdenum disulfide@carbon materials of intermediate gaps
Reason process provides space, so as to alleviate electrode dusting, capacity attenuation caused by volumetric expansion.Finally it is prepared with optimal
The yolk-shell structure molybdenum disulfide@carbon materials in gap, in the electric discharge specific volume of the second circle when it is as negative electrode of lithium ion battery
Amount is up to 1167 mAh g-1, the specific discharge capacity after 200 circle circulations is 880mAh g-1, capacity retention ratio is
75.4%, and high rate performance protrudes.
Brief description of the drawings
Fig. 1 (a), the Flied emission electron microscope that 1 (b) is molybdenum disulfide nano ball；Fig. 1 (c), 1 (d) are respectively molybdenum disulfide@
The Flied emission electron microscope and transmission electron microscope picture of poly-dopamine.
Fig. 2 (a), 2 (b) and 2 (c), 2 (d) are respectively MoS2The Flied emission electron microscope and transmission electron microscope picture of@C-0%；Fig. 2
(e), 2 (f) and 2 (g), 2 (h) are respectively MoS2The Flied emission electron microscope and transmission electron microscope picture of@C-0.2%；Fig. 2 (i), 2 (j) and
2 (k), 2 (l) are respectively MoS2The Flied emission electron microscope and transmission electron microscope picture of@C-0.4%；Fig. 2 (m), 2 (n) and 2 (o), 2 (p)
Respectively MoS2The Flied emission electron microscope and transmission electron microscope picture of@C-0.6%.
Fig. 3 (a), 3 (b) are respectively MoS2@C-0%、 MoS2@C-0.2%、 MoS2@C-0.4% 、MoS2@C-0.6% are in electricity
Current density is 200 mA g-1When specific discharge capacity cyclic curve and be 100 mA g in current density-1To 5 A g-1Times
Rate curve.
Embodiment
Following embodiments will the present invention is further illustrated with reference to attached drawing.It should be appreciated that these embodiments are only used for
Illustrate the present invention rather than limit the scope of the invention.Without prejudice to spirit of the invention and protected for those skilled in the art
The other changes and modifications made in the case of shield scope, are included within the scope of the present invention.
Embodiment 1
1）12 mmol elemental sulfurs and 5 mmol molybdenum trioxides are added in the ethylene glycol solution of 300 ml, water bath sonicator 10
Min forms uniform solution.Then above-mentioned solution is transferred in the polytetrafluoroethylene (PTFE) autoclave of 500 ml, is put into temperature
12 h are reacted for 200 DEG C of baking ovens, obtain molybdenum disulfide nano ball.
2）The above-mentioned molybdenum disulfide nano balls of 800 mg are taken to be dispersed in the Tris buffer solutions of 200 ml（10 mM, pH=8.5）
In, 200mg dopamines are added, 12 h is slowly stirred, obtains molybdenum disulfide@poly-dopamines.Molybdenum disulfide@poly-dopamines are put into
It is 5 DEG C/min, protective gas N in heating rate in tube furnace2, temperature be carbonized 2 h under the conditions of being 800 DEG C, obtain nucleocapsid
Structure molybdenum disulfide@carbon（It is named as MoS2@C-0%,）.
3 ）Configuration concentration is the hydrogen peroxide solution of 0.2 vol %, then adds the above-mentioned core shell structure molybdenum disulfide@of 200mg
Carbon, is vigorously stirred 1 h, obtains final product yolk-shell structure molybdenum disulfide@carbon（It is named as MoS2@C-0.2%,）.
From the Flied emission electron microscope of Fig. 1 (a), the different resolution of 1 (b) can be seen that solvent hot be it is a diameter of ~
The dispersed nano ball of 280 nm, its surface are smooth.Fig. 1 (c), the shape appearance figure of 1 (d) can see, and poly-dopamine is in curing
Molybdenum coated with uniform, its thickness about 30nm.Fig. 2 (a) -2 (d) is MoS2The Flied emission electron microscope and transmission electron microscope picture of@C-0%,
It can be seen that carbon thickness of the shell is uniform, about ~ 25nm.Fig. 2 (e) -2 (h) is MoS2The Flied emission electron microscope and transmission electron microscope of@C-0.2%
Figure, it can be seen that molybdenum disulfide（yolk）Diameter is varied down to ~ 225nm.MoS is seen in Fig. 3 (a)2The second circle electric discharge of@C-0.2%
Specific capacity is 910 mAh g-1, the specific discharge capacity after circulation 200 is enclosed is 652mAh g-1, capacity retention ratio 71.6%.Figure
See that in current density be 100 mAh g in 3 (b)-1When, the specific discharge capacity of MoS2@C-0.2% is 930mAh g-1, work as electric current
Density increases to 5 mAh g-1When, the specific discharge capacity of MoS2@C-0.2% is 320mAh g-1。
Embodiment 2
1）12 mmol elemental sulfurs and 5 mmol molybdenum trioxides are added in the ethylene glycol solution of 300 ml, water bath sonicator 10
Min forms uniform solution.Then above-mentioned solution is transferred in the polytetrafluoroethylene (PTFE) autoclave of 500 ml, is put into temperature
12 h are reacted for 200 DEG C of baking ovens, obtain molybdenum disulfide nano ball.
2）The above-mentioned molybdenum disulfide nano balls of 800 mg are taken to be dispersed in the Tris buffer solutions of 200 ml（10 mM, pH=8.5）
In, 200mg dopamines are added, 12 h is slowly stirred, obtains molybdenum disulfide@poly-dopamines.Molybdenum disulfide@poly-dopamines are put into
It is 5 DEG C/min, protective gas N in heating rate in tube furnace2, temperature be carbonized 2 h under the conditions of being 800 DEG C, obtain nucleocapsid
Structure molybdenum disulfide@carbon（It is named as MoS2@C-0%,）.
3）Configuration concentration is the hydrogen peroxide solution of 0.4 vol %, then adds the above-mentioned core shell structure molybdenum disulfide@of 200mg
Carbon, is vigorously stirred 1 h, obtains final product yolk-shell structure molybdenum disulfide@carbon（It is named as MoS2@C-0.4%,）.
Fig. 2 (i) -2 (l) is MoS2The Flied emission electron microscope and transmission electron microscope picture of@C-0.4%, it can be seen that molybdenum disulfide
（yolk）Diameter is varied down to ~ 190nm.MoS is seen in Fig. 3 (a)2The second circle specific discharge capacity of@C-0.4% is 1167 mAh g-1, the specific discharge capacity after circulation 200 is enclosed is 880mAh g-1, capacity retention ratio 75.4%.See in Fig. 3 (b) in electric current
Density is 100 mAh g-1When, the specific discharge capacity of MoS2@C-0.4% is 1100mAh g-1, when current density increases to 5 mAh
g-1When, the specific discharge capacity of MoS2@C-0.4% is 450mAh g-1。MoS2The chemical property of@C-0.4% is optimal, this is because
In-between pore size is optimal.
Embodiment 3
1）12 mmol elemental sulfurs and 5 mmol molybdenum trioxides are added in the ethylene glycol solution of 300 ml, water bath sonicator 10
Min forms uniform solution.Then above-mentioned solution is transferred in the polytetrafluoroethylene (PTFE) autoclave of 500 ml, is put into temperature
12 h are reacted for 200 DEG C of baking ovens, obtain molybdenum disulfide nano ball.
2）The above-mentioned molybdenum disulfide nano balls of 800 mg are taken to be dispersed in the Tris buffer solutions of 200 ml（10 mM, pH=8.5）
In, 200mg dopamines are added, 12 h is slowly stirred, obtains molybdenum disulfide@poly-dopamines.Molybdenum disulfide@poly-dopamines are put into
It is 5 DEG C/min, protective gas N in heating rate in tube furnace2, temperature be carbonized 2 h under the conditions of being 800 DEG C, obtain nucleocapsid
Structure molybdenum disulfide@carbon（It is named as MoS2@C-0%,）.
3）Configuration concentration is the hydrogen peroxide solution of 0.6 vol %, then adds the above-mentioned core shell structure molybdenum disulfide@of 200mg
Carbon, is vigorously stirred 1 h, obtains final product yolk-shell structure molybdenum disulfide@carbon（It is named as MoS2@C-0.6%,）.
Fig. 2 (m) -2 (p) is MoS2The Flied emission electron microscope and transmission electron microscope picture of@C-0.6%, it can be seen that molybdenum disulfide
（yolk）Diameter is varied down to ~ 100nm.The second circle specific discharge capacity that MoS2@C-0.6% are seen in Fig. 3 (a) is 1034mAh g-1,
Specific discharge capacity after the circle of circulation 200 is 703 mAh g-1, capacity retention ratio 70.0%.See in Fig. 3 (b) close in electric current
Spend for 100 mAh g-1When, the specific discharge capacity of MoS2@C-0.6% is 940mAh g-1, when current density increases to 5 mAh g-1
When, the specific discharge capacity of MoS2@C-0.6% is 335mAh g-1。
Claims (3)
1. a kind of preparation method of yolk-shell structures molybdenum disulfide@carbon electrode materials, it is characterised in that specific steps are such as
Under：
（1）5 ~ 36mmol elemental sulfurs and 2 ~ 15mmol molybdenum trioxides are added in the solvent ethylene glycol solution of 300 ml, water-bath
Uniform solution is formed after 10 min of ultrasound；Then polytetrafluoroethylene (PTFE) high pressure that the uniform solution of formation is transferred to 500 ml is anti-
Answer in kettle, be put into the baking oven that temperature is 200 DEG C and react 12 h, obtain product molybdenum disulfide nano ball, its a diameter of 280nm；
（2）Take 800 mg steps（1）Obtained molybdenum disulfide nano ball is dispersed in the Tris buffer solutions of 200 ml（10 mM, pH
=8.5）In, add 200mg dopamines and stir 12 h, obtain molybdenum disulfide@poly-dopamines；Molybdenum disulfide@poly-dopamines are put into
It is 5 DEG C/min, protective gas N in heating rate in tube furnace2, temperature be carbonized 2 h under the conditions of being 800 DEG C, obtain nucleocapsid knot
Structure molybdenum disulfide@carbon；
（3）Hydrogen peroxide solution is configured, then adds 200mg steps（2）The core shell structure molybdenum disulfide@carbon of gained, is vigorously stirred 1
H, obtains final product yolk-shell structure molybdenum disulfide@carbon.
2. according to the method described in claim 1, it is characterized in that step（1）The molar ratio of middle sulphur and molybdenum trioxide is 12：5.
3. according to the method described in claim 1, it is characterized in that step（3）Described in hydrogen peroxide concentration be 0.05-3 vol
%。
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| CN109735200B (en) * | 2018-12-10 | 2020-12-22 | 华南理工大学 | Epoxy anticorrosive coating composition and preparation method and application thereof |
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