CN109950509A - A kind of MoO2/MoS2Combination electrode material and preparation method thereof - Google Patents
A kind of MoO2/MoS2Combination electrode material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of MoO2/MoS2Combination electrode material and preparation method thereof.Then uniformly mixed solid powder is calcined, obtains MoO after cooling the following steps are included: S1. mixes ammonium molybdate powder and oxalic acid powder by the preparation method3Presoma；S2. by the MoO3Presoma and sulphur powder are uniformly mixed, and then uniformly mixed solid powder is placed in closed reactor, 0.5-100h is reacted under the conditions of 170~230 DEG C, cools down after reaction；Wherein, the MoO3The weight ratio of presoma and the sulphur powder is 1:0.5-5；S3. reaction product after cooling in step S2 is warming up to 500-800 DEG C of heat preservation 1-3h under inert gas protection, then cools down, obtains MoS2/MoO2Composite material.Method of the invention is easy to operate, securely and reliably, is conducive to industrialized production, and each component content is controllable in the composite material.
Description
Technical field
The invention belongs to field of batteries, more particularly, to a kind of MoO2/MoS2Combination electrode material and preparation method thereof.
Background technique
With the fast development of all kinds of electric cars, the demand to battery high capacity high-energy electrode material sharply increases
Add.Molybdenum dioxide (MoO2) due to specific capacity height (880mAh g-1), it is at low cost, toxicity is low, natural abundant, in lithium ion battery
It is attracted wide attention with the field SCs.But MoO2In charge and discharge process violent volume change make its cyclical stability and
High rate capability is poor, affects its practical application.The MoO that document report is prepared by two-step method2/Au/MnO2Composite construction table
Reveal excellent chemical property (X.Zhang, Y.Xu, Y.Ma, M.Yang, Y.Qi, A hierarchical MoO2/Au/
MnO2heterostructure with enhanced electrochemical performance for application
as supercapacitor,Eur.J.Inorg.Chem.2015(2015)3764–3768).It is compound compared with single compound
Material shows excellent chemical property.Therefore, by MoO2With other electroactive materials are compound becomes so as to improve its performance
Research hotspot.In these Mo based compounds, MoS2Because of higher ionic conductivity (being higher than oxide) and higher theoretical appearance
Amount (being higher than graphite) becomes preferably selection.
Currently, MoO2/MoS2There are mainly three types of methods for the synthesis of composite material.One is traditional hydro-thermal methods.Hydro-thermal method master
Will using molybdenum salt, perhaps molybdenum source and various sulphur sources are dissolved in water or organic solvent as molybdenum source by molybdenum oxide, add some auxiliary and try
Agent controls certain acid-base property, and 200 DEG C or so reactions synthesize target product in a sealed container.This method simple process is controllable,
Product morphology is uniform, is current synthesis MoO2/MoS2The main method of composite material, but solvent usage is big, cost for wastewater treatment
Height limits its large-scale production.
Second is in situ synthesis.CN106410150A is disclosed MoO3Presoma and S powder according to 0.5:(1.0~
5.0) mass ratio, after grinding uniformly, under inert conditions, from room temperature to 400~600 DEG C, 0.5~2h of insulation reaction,
It then proceedes to be warming up to 600~800 DEG C, 0.5~2h of insulation reaction is cooled to room temperature, and reaction product is cleaned, is dry, is made
MoO with core-shell structure2-MoS2Anode material of lithium-ion battery.CN105514403B discloses similar with CN103367713A
Method, by MoO3Presoma and S powder are blended, then high-temperature calcination.This method simple possible is relatively suitble to small lot raw
It produces.But the composition of synthetic product composite material is affected by gas flow rate, calcination temperature and presoma ratio.Flow velocity is big,
Temperature height results in sulphur and largely evaporates, loss.In order to improve the content of molybdenum sulfide in compound, need to increase S powder dosage, S powder
With MoO3Forerunner's body mass ratio is up to 5:0.5, if that is, molar ratio is up to 40:1. large-scale production, excessive sulphur steams
Gas deposits to the cold in tube furnace, it is easy to block gas passage, lead to safety problem.
The third method is vapour deposition process.CN109207957A is disclosed with solid-state S and MoO3For presoma, sulphur powder is put
Steam is flashed in tube furnace low-temperature space, molybdenum dioxide is placed on high-temperature region and flashes to steam, drive of two kinds of steams in carrier gas
Under meet, MoS is synthesized in target substrate after chemical gas phase reaction2/MoO2, wherein S steam is dense in tube furnace warm area
Degree can be adjusted by the size of carrier gas flux.This method utilizes gas phase reaction, reacts more thorough, is more advantageous to preparation pure phase
MoS2, pure MoS is obtained using this method as CN106757361A is disclosed2.But this method needs higher reaction temperature, up to 800
DEG C or more, sulfur vapor is even more significantly excessive, S and MoO3The mass ratio of powder is up to 100:3, and it is stifled that this method equally exists sulfur vapor
Safety problem caused by plug instrument.And use instead logical hydrogen sulfide gas instead of sulphur powder method (1.Dingbin Xiao,
Jinying Zhang,Xin Li,Dan Zhao,Hongyang Huang,Jialiang Huang,Daxian Cao,Zhihui
Li, and Chunming Niu, ACS Nano 2016,10,9509-9515.2.Prabhat Kumar,Megha Singh,
178 (2016) 6e11 of Rabindar K.Sharma, G.B.Reddy, Materials Chemistry and Physics) because
Hydrogen sulfide severe toxicity is also not suitable for promoting.
Summary of the invention
The purpose of the present invention is more complex, composite material content poor controllabilities and safety difference etc. for prior art processes
Problem provides a kind of improved MoO2/MoS2The preparation method of combination electrode material, this method is easy to operate, securely and reliably, has
Conducive to industrialized production, and each component content is controllable in the composite material.
To achieve the goals above, the first aspect of the present invention provides a kind of MoO2/MoS2The preparation side of combination electrode material
Method, the preparation method the following steps are included:
S1. ammonium molybdate powder and oxalic acid powder are mixed, then calcines uniformly mixed solid powder, after cooling
Obtain MoO3Presoma；
S2. by the MoO3Presoma and sulphur powder are uniformly mixed, and are then placed in uniformly mixed solid powder closed anti-
It answers in kettle, reacts 0.5-100h under the conditions of 170~230 DEG C, cool down after reaction；Wherein, the MoO3Presoma and institute
The weight ratio for stating sulphur powder is 1:0.5-5；
S3. reaction product after cooling in step S2 is warming up to 500-800 DEG C of heat preservation 1-3h under inert gas protection,
Then cool down, obtain MoS2/MoO2Composite material.
Key problem in technology of the invention is: using the hydrothermal reaction kettle of sealing as reactor, by MoO3Presoma and sulphur powder
It is blended, sulphur powder is allowed to become sulfur vapor at a certain temperature, steam generates certain pressure in the container of sealing, promotes oxide
Vulcanization reaction.
Pass through control sulphur powder and MoO3Ratio, vulcanization reaction temperature and time between presoma are realized to MoO2/
MoS2The controllability of composite material composition, obtains required composite material.Through MoO made from this method2/MoS2Lithium ion battery
Negative electrode material specific discharge capacity with higher and preferable cyclical stability.
Further, in step S1, the condition of the calcining includes: that temperature is 450-550 DEG C, and the time is 1-4 hours.
According to the present invention, in step S1, the dosage of ammonium molybdate and oxalic acid can determine as needed, it is preferable that ammonium molybdate and
The molar ratio of oxalic acid is 1:2-4.
In accordance with the present invention it is preferred that the time of reaction is 1-60h, further preferably 4-48h in step S2.
Further, in step S2, the MoO3The weight ratio of presoma and the sulphur powder is 1:1-3.
By further controlling sulphur powder and MoO3Ratio, vulcanization reaction temperature and time between presoma, can obtain
Obtain the more excellent MoO of performance2/MoS2Combination electrode material.
According to the present invention, in step S2, the closed reactor can be conventional various hydrothermal reaction kettles, for example, have
There is the hydrothermal reaction kettle of polytetrafluoroethyllining lining.
According to the present invention, in step S3, the temperature is preferably risen with slower speed, particularly preferably, the heating
Rate be 3-8 DEG C/min.
In the present invention, in three steps, cooling mode is both preferably natural cooling, specifically,
In step S1, cooled to room temperature after calcining obtains MoO3Presoma；
In step S2, after reaction by reaction product cooled to room temperature；
In step S3, after heat preservation, room temperature is cooled to furnace.
According to the present invention, in step S1 and S2, this field routine is can be used into the method that solid powder is uniformly mixed
Various methods, for example, polishing.
A kind of specific embodiment according to the present invention, the preparation method include the following steps:
The first step, presoma MoO3Synthesis: weigh a certain amount of Ammonium Molybdate Tetrahydrate and oxalic acid, use mortar grinder respectively
It after powder, remixes and grinds together, be sufficiently mixed two kinds of solid powders.Then uniformly mixed solid powder is placed
It is calcined 2 hours under the conditions of 500 DEG C in Muffle furnace in crucible, is taken out after cooled to room temperature, obtain MoO3Presoma.
Second step, difference composition MoO2/MoS2Composite material synthesis: a certain amount of sulphur powder and above-mentioned synthesis MoO are weighed3In
It is ground in mortar, is uniformly mixed two kinds of solid powders, hybrid solid powder is then transferred to village's high temperature in polytetrafluoroethylene (PTFE)
In reaction kettle, in air dry oven, a period of time is reacted under the conditions of 180~220 DEG C, makes its natural cooling after reaction
To room temperature, MoO is obtained2/MoS2Product.
Third step, in order to improve the crystallinity of product, the product of synthesis in tube furnace under argon gas protection environment with 5 DEG C/
The heating rate of min is warming up to 700-800 DEG C of heat preservation 2h, is subsequently reduced to room temperature, obtains MoS2/MoO2Composite material.
The second aspect of the present invention provides the MoO as made from above-mentioned preparation method2/MoS2Combination electrode material.
The beneficial technical effect of the present invention lies in:
Method of the invention is with sulphur powder and MoO3For presoma, is reacted by water heating kettle sealing, synthesized MoO2/
MoS2Composite material.This method simple process, safe operation are suitble to industrialized production, and material composition is controllable.By in height
Temperature is lower to carry out isothermal holding, can be further improved the crystallinity of product.
The composite material that the present invention synthesizes can be used as lithium ion battery negative material, in chemical property and compound
MoS2Content it is related, content is too low, and conductivity of composite material is poor, and discharge capacity is lower；Content is too high, in MoO2Surface
Arranged type changes, and composite material surface property is caused also to change therewith, therefore, using preparation method of the invention,
The component for regulating and controlling composite material, make full use of the coordinating effect in composite material between different component, available to have excellent performance
Lithium ion battery negative material.
Other features and advantages of the present invention will then part of the detailed description can be specified.
Detailed description of the invention
Exemplary embodiment of the invention is described in more detail in conjunction with the accompanying drawings, it is of the invention above-mentioned and its
Its purpose, feature and advantage will be apparent.
Fig. 1 is MoO made from 1-4 of the embodiment of the present invention2-MoS2The XRD diagram of product.
Fig. 2A -2D is respectively MoO made from 1-4 of the embodiment of the present invention2-MoS2The SEM of product schemes.
Fig. 3 is MoO made from 1-4 of the embodiment of the present invention2-MoS2The impedance diagram of product.
Fig. 4 is MoO made from 1-4 of the embodiment of the present invention2-MoS2The electrochemistry cycle performance figure of product.
Specific embodiment
The preferred embodiment of the present invention is described in more detail below.Although the following describe preferred implementations of the invention
Mode, however, it is to be appreciated that may be realized in various forms the present invention without that should be limited by the embodiments set forth herein.
Embodiment 1
The present embodiment is for illustrating MoO of the invention2/MoS2Composite material and preparation, it is described preparation in accordance with the following steps into
Row:
(1) it weighs in the balance and accurately takes 0.01mol Ammonium Molybdate Tetrahydrate (1.7654g), 0.03mol oxalic acid (3.78g), with grinding
Alms bowl grinding is sufficiently mixed two kinds of solid powders.It solid powder will then be mixed will be placed in Muffle furnace and be forged under the conditions of 500 DEG C
It burns 2 hours, is taken out after being then cooled to room temperature, obtain MoO3Presoma.
(2) MoO described in 0.5g is weighed3Two kinds of powder are sufficiently mixed by presoma and 1g sulphur powder, and it is poly- to be subsequently transferred to 50mL
In tetrafluoroethene in village's pyroreaction kettle, 4h is reacted under the conditions of 220 DEG C in air dry oven, then it is made to naturally cool to room
Obtained powder is finally warming up to 800 DEG C of heat preservations under argon gas protection environment in tube furnace with the heating rate of 5 DEG C/min by temperature
2h is down to room temperature with furnace, obtains MoS2/MoO2Composite material.
Embodiment 2
The present embodiment is for illustrating MoO of the invention2/MoS2Composite material and preparation, it is described preparation in accordance with the following steps into
Row:
(1) experimental procedure is identical with embodiment 1 step (1).
(2) MoO described in 0.5g is weighed3Presoma and 0.8g sulphur powder are fully ground in mortar, then by hybrid solid powder
End is transferred in 50mL polytetrafluoroethylene (PTFE) in village's pyroreaction kettle, is reacted 8h under the conditions of being sealed in 220 DEG C, is obtained MoO2/MoS2It is multiple
Condensation material initial product is finally warming up to 750 DEG C of heat preservations under argon gas protection environment in tube furnace with the heating rate of 5 DEG C/min
2h is down to room temperature with furnace, obtains MoS2/MoO2Composite material.
Embodiment 3
The present embodiment is for illustrating MoO of the invention2/MoS2Composite material and preparation, it is described preparation in accordance with the following steps into
Row:
(1) experimental procedure is identical with embodiment 1 step (1).
(2) MoO described in 0.5g is weighed3Presoma and 0.6g sulphur powder are sufficiently mixed in mortar, then by hybrid solid powder
End is transferred in polytetrafluoroethylene (PTFE) in village's pyroreaction kettle, is reacted for 24 hours under the conditions of 200 DEG C, is made it naturally cold after reaction
But to room temperature, primary product is obtained, finally primary product is placed in tube furnace under argon gas protection environment with the heating of 5 DEG C/min
Rate is warming up to 700 DEG C of heat preservation 2h and obtains MoS with the near room temperature of furnace2/MoO2Composite material.
Embodiment 4
The present embodiment is for illustrating MoO of the invention2/MoS2Composite material and preparation, it is described preparation in accordance with the following steps into
Row:
(1) experimental procedure is identical with embodiment 1 step (1).
(2) MoO described in 0.5g is weighed3Presoma and 0.5g sulphur powder are ground in mortar, keep two kinds of solid powder mixing equal
It is even, then hybrid solid powder is transferred in reaction kettle, 48h is reacted under the conditions of 200 DEG C, makes it naturally cold after reaction
But, solid powder after cooling is placed in tube furnace and is warming up to 700 DEG C of heat preservation 2h under argon gas protection, is down to room temperature with furnace, obtains
MoS2/MoO2Composite material.
Test case 1
MoS is synthesized under the different sealing reaction time that Fig. 1 is embodiment 1-42/MoO2The XRD diagram of composite material, by Fig. 1
As can be seen that the MoS of water heating kettle sealing reaction synthesis in 4 hours2/MoO2In composite material, MoO2Characteristic peak has higher strong
Degree, and MoS2Characteristic peak it is weaker；With the extension in sealing reaction time, MoO in composite material2The intensity of characteristic peak is gradually
It reduces, and MoS2Diffraction maximum peak intensity gradually increases.It is possible thereby to infer MoS in composite material2Content is prolonged with the sealing reaction time
It grows and increases.
Test case 2
The MoS of the different sealing reaction time synthesis of embodiment 1-4 is followed successively by shown in Fig. 2A-D2/MoO2Scanning electron microscope (SEM) photograph,
It can be seen that synthesized sample appearance pattern difference is little.The main reason for difference of composite property is not that pattern causes
's.
Test case 3
MoS is synthesized under the different sealing time conditions that Fig. 3 is embodiment 1-42/MoO2The ac impedance spectroscopy of composite material.
As seen from Figure 3,8 hours sample radius minimums are reacted in sealing, show its charge transfer resistance minimum, indication sealing reaction 8
Hour sample has better chemical property.
Test case 4
The MoS synthesized under the different sealing reaction time that Fig. 4 show embodiment 1-42/MoO2Composite material is in 100mA/g
50 weeks cycle performance curves under current density.Sealing reacts 4h, 8h, for 24 hours with 48h's it can be seen from discharge curve in Fig. 4
Sample, its specific discharge capacity is followed successively by 573.1mAh/g, 824.8mAh/g, 574.2mAh/g, 411mAh/g after recycling within 50 weeks,
Sealing 8 hours sample charge-discharge performances of reaction are best.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes are obvious for the those of ordinary skill in art field.
Claims (10)
1. a kind of MoO2/MoS2The preparation method of combination electrode material, which is characterized in that the preparation method the following steps are included:
S1. ammonium molybdate powder and oxalic acid powder are mixed, then calcines uniformly mixed solid powder, obtained after cooling
MoO3Presoma；
S2. by the MoO3Presoma and sulphur powder are uniformly mixed, and uniformly mixed solid powder is then placed in closed reactor
In, 0.5-100h is reacted under the conditions of 170~230 DEG C, is cooled down after reaction；Wherein, the MoO3Presoma and the sulphur
The weight ratio of powder is 1:0.5-5；
S3. reaction product after cooling in step S2 is warming up to 500-800 DEG C of heat preservation 1-3h under inert gas protection, then
Cooling, obtains MoS2/MoO2Composite material.
2. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that in step S1,
The condition of the calcining includes: that temperature is 450-550 DEG C, and the time is 1-4 hours.
3. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that in step S1,
The molar ratio of ammonium molybdate and oxalic acid is 1:2-4.
4. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that in step S2,
The time of reaction is 1-60h.
5. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that in step S2,
The MoO3The weight ratio of presoma and the sulphur powder is 1:1-3.
6. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that in step S2,
The closed reactor is hydrothermal reaction kettle.
7. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that in step S3,
The rate of the heating is 3-8 DEG C/min.
8. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that
In step S1, cooled to room temperature after calcining obtains MoO3Presoma；
In step S2, after reaction by reaction product cooled to room temperature；
In step S3, after heat preservation, room temperature is cooled to furnace.
9. MoO according to claim 12/MoS2The preparation method of combination electrode material, which is characterized in that step S1 and S2
In, the method that solid powder is uniformly mixed is polishing.
10. MoO made from the preparation method as described in any one of claim 1-92/MoS2Combination electrode material.
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Cited By (1)
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|---|---|---|---|---|
| CN111468144A (en) * | 2020-05-19 | 2020-07-31 | 郑州大学 | MoS2/MoO2Ru composite material and preparation method and application thereof |
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