CN108091837A - A kind of molybdenum disulfide/carbon composite and its preparation method and application - Google Patents
A kind of molybdenum disulfide/carbon composite and its preparation method and application Download PDFInfo
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Abstract
A kind of molybdenum disulfide/carbon composite and its preparation method and application, the preparation method adds in para-aminophenol, formaldehyde and ammonium hydroxide to prepare multi-layer C hollow ball, by regulating and controlling water first using water as solvent, the amount of 3 AP, formaldehyde and ammonium hydroxide regulates and controls the number of plies of C hollow balls；Using the C hollow balls of synthesis as skeleton, then using ammonium molybdate as molybdenum source, MoS is obtained by hydro-thermal method using thiocarbamide as sulphur source2/ C composite.And for the present invention during composite material is prepared, preparation method is simple, and safe preparation process, low energy consumption, workable.
Description
Technical field
The invention belongs to new energy materials fields, and in particular to molybdenum disulfide/carbon composite and preparation method thereof and use
On the way.
Background technology
Lithium ion battery (LIB) is considered as most promising energy storage device in portable electronic and electric vehicle, wherein
Electrode material is to its performance important.Although traditional graphite cathode has been commercialized, its capacity is very low
(372mA h g-1), greatly limit its practical application in portable electronic and electric vehicle.Further, since
LIB negative materials, with serious volume expansion, make material fragmentation serious in long-time charge and discharge process, cause irreversible
Capacitance loss and cyclical stability reduce.Therefore, the cycle performance of LIB, high rate performance and security performance need further to carry
It is high.
Molybdenum disulfide (MoS2) it is typical two-dimentional transient metal sulfide, in particular, MoS2Possess similar to graphene
Layer structure, wherein molybdenum atom is clipped between two layers of sulphur atom, this is structure most stable and common in stratified material family
One of.MoS2The characteristics of theoretical memory capacity is up to 670m Ah/g, layer structure is easy to lithium ion insertion-embedding.Although have
These advantages, but MoS2Still there is stability difference and capacity rapid decay, seriously hinder MoS2As lithium ion
The application of battery anode material.Some graphited carbon materials are because itself has preferable electric conductivity, in electrochemical field
Some other materials can be made up in terms of electric conductivity deficiency the shortcomings that, the two can realize structure by certain experimental method
On it is compound, can be made up mutually in performance each other so that original material obtains larger improvement on chemical property, and
The carbon materials such as graphene have preferable stability, can be still stabilized under the impact of a constant current with holding structure, no
It can cause the decline of chemical property.Simple MoS prepared by conventional hydrothermal method2Lithium storage content can reach 900m Ah/g,
But with very poor cyclical stability, cycle 20 times and be just reduced to less than 300m Ah/g under the current density of 0.1A/g, this
Any significantly limits MoS2Commercialized development in field of lithium ion battery.Therefore, to MoS2Related modification is carried out to have become
For main trend.
Nano-hollow carbon ball (HCN) in energy because with unique structure and excellent physicochemical property, having converted and having stored, urge
The various fields such as change, absorption and biological medicine show huge application prospect, are concerned in academia.In order to realize HCN
Performance optimization, generally require in preparation process to its structure, pattern and surface chemistry composition etc. regulate and control.However,
The preparation method of HCN relies primarily on template at present (including soft template and hard template)；Its face technique it is tediously long, it is seriously polluted,
And lack control and construct many bottlenecks such as labyrinth ability.Therefore, a kind of zero template, efficient, pollution-free and be easy to is opened up
The preparation method of regulation and control, and corresponding formation mechenism is furtherd investigate and discloses, there is highly important scientific meaning and using valency
Value.
104934602 A of CN disclose a kind of molybdenum disulfide/carbon composite, including layer of molybdenum-disulfide and carbon hollow ball,
The layer of molybdenum-disulfide is located at the outside of the carbon hollow ball, and the carbon hollow ball has hollow-core construction.The invention also discloses
A kind of preparation method of above-mentioned molybdenum disulfide/carbon composite, including multiple steps, mould is done with amino modified silica spheres
Plate, then by being pyrolyzed organic carbon source coated die plate, then by it with four thio ammonium molybdate by solvent thermal reaction, in inert atmosphere
Lower high temperature cabonization, finally removes silica template, you can obtains molybdenum disulfide/carbon composite of the present invention.It is but this
Complex steps when method prepares composite material, and the number of plies of C shells can not be regulated and controled.105098151 A of CN disclose a kind of two sulphur
Change molybdenum-carbon hollow ball hybrid material, the molybdenum disulfide-carbon hollow ball hybrid material has the structure of hollow ball, individual layer or few layer
Molybdenum disulfide nano sheet is embedded in the shell that the hybrid material formed in carbon material is hollow ball.But the invention is also without examining
Consider influence of the number of plies of C shells to composite property.
The content of the invention
For this purpose, one of the objects of the present invention is to provide a kind of preparation methods of molybdenum disulfide/carbon composite.The present invention
Preparation method it is simple, safe preparation process, low energy consumption, workable.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of molybdenum disulfide/carbon (MoS2/ C) composite material preparation method, process is as follows：Using water as solvent, addition pair
Amino-phenol (3-AP), formaldehyde and ammonium hydroxide prepare C hollow balls, and by regulating and controlling water, 3-AP, the amount of formaldehyde and ammonium hydroxide regulates and controls C
The number of plies of hollow ball；Using the C hollow balls of synthesis as skeleton, then using ammonium molybdate as molybdenum source, obtained using thiocarbamide as sulphur source by hydro-thermal method
To MoS2/ C composite.
The preparation method of the present invention, can be by regulating and controlling water, 3-AP, and the amount of formaldehyde and ammonium hydroxide regulates and controls the number of plies of C hollow balls.
Preferably, the MoS of the present invention2The preparation method of/C composite, comprises the following steps：
1. para-aminophenol, formaldehyde and ammonium hydroxide are added to the water, clear solution is stirred to get；
2. by acetone be added to step 1. gained clear solution in, stir to get suspension；
3. 2. suspension that step is prepared carries out separation of solid and liquid, washing is dried to obtain precipitation；
4. 3. precipitation that step is prepared is ground to fine-powder, calcining is subsequently cooled to room temperature and obtains powder；
5. 4. powder and ammonium molybdate, thiocarbamide that step is obtained are added sequentially in deionized water, it is dispersed into uniform outstanding
Turbid；
6. 5. suspension that step is prepared heats reaction, after be cooled to room temperature, separation of solid and liquid, washing is dry
To the MoS2/ C composite.
Preferably, step 1. middle stirring when solution temperature be 25 DEG C, time of stirring is 0.5~1h, is preferably 0.5h.
0.1g 3-AP, 0.1mL formaldehyde and ammonium hydroxide can be used to be added to 30mLH220mL is added in O, after being sufficiently stirred to be made
Individual layer C hollow balls.
0.15g 3-AP, 0.15mL formaldehyde and ammonium hydroxide can be used to be added to 45mLH2In O, 30mL systems are added in after being sufficiently stirred
Obtain double-deck C hollow balls.
0.32g 3-AP, 0.32mL formaldehyde and ammonium hydroxide can be used to be added to 96mLH2In O, 64mL systems are added in after being sufficiently stirred
Obtain three layers of C hollow balls.
0.54g 3-AP, 0.54mL formaldehyde and ammonium hydroxide can be used to be added to 162mLH2In O, 108mL is added in after being sufficiently stirred
Four layers of C hollow balls are made.
0.6g 3-AP, 0.6mL formaldehyde and ammonium hydroxide can be used to be added to 180mLH2In O, 120mL systems are added in after being sufficiently stirred
Obtain five layers of C hollow balls.
0.68g 3-AP, 0.68mL formaldehyde and ammonium hydroxide can be used to be added to 136mLH2In O, 204mL is added in after being sufficiently stirred
Six layers of C hollow balls are made.
0.7g 3-AP, 0.7mL formaldehyde and ammonium hydroxide can be used to be added to 140mLH2In O, 210mL systems are added in after being sufficiently stirred
Obtain seven layers of C hollow balls.
2. middle acetone is preferably to be added dropwise to step.
Preferably, the temperature of step 4. middle calcining is 1000-1500 DEG C, it is preferably 1200 DEG C, the time is more than 1h, excellent
Elect 2h as.Calcining preferably carries out in Ar gas shieldeds.
Calcining can carry out in tube furnace.
Preferably, 5. middle powder, ammonium molybdate and thiocarbamide mass ratio are 2 to step:1~4:1~4.
Preferably, the molar ratio of ammonium molybdate and thiocarbamide is 1:2.5-2.6.
Preferably, the volume of the deionized water of addition is 150-300 times of powder quality, is preferably 200 times.
Preferably, disperse to carry out by stirring, ultrasound, preferably stir 1h, ultrasonic 0.5h.
Preferably, the temperature of step 6. middle heating is 200 DEG C, the reaction time is for 24 hours.
Suspension, which can be put into be subsequently placed in insulating box in autoclave, to be reacted
Preferably, 3. and 6. middle wash is carried out step successively using deionized water, absolute ethyl alcohol.It is preferred that washing 3~6
It is secondary.
Preferably, first it is washed with deionized 3 times, then is washed 2 times with absolute ethyl alcohol.
Preferably, dry temperature is 50~60 DEG C, is preferably 50 DEG C, and the dry time is 10-15h, is preferably 12h.
Conventional method can be used to carry out for separation of solid and liquid in the present invention, such as；Centrifugation, filtering etc., preferably centrifuge.
An object of the present invention, which also resides in, provides MoS prepared by a kind of method of the present invention2/ C composite.
An object of the present invention, which also resides in, provides a kind of MoS of the present invention2/ C composite is in lithium ion battery
Application in negative material.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) preparation method using the present invention regulates and controls C hollow balls by the amount for regulating and controlling 3-AP, formaldehyde, ammonium hydroxide and acetone
The number of plies realizes the controllable regulation and control of the C hollow ball numbers of plies.
(2) in the present invention, the molar ratio of ammonium molybdate and thiocarbamide is 1:2.5-2.6, thiocarbamide are slightly excessive to ensure ammonium molybdate
The reaction was complete, while slows down MoS2Generating rate, reduce MoS2Size, for lithium ion insertion more active sites are provided, from
And cause material that there is good chemical property.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, is not construed as the concrete restriction to the present invention.
It is noted that described further below be all exemplary, it is intended to provide further instruction to the present invention.It is unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " bag
Include " when, indicate existing characteristics, step, operation and/or combination thereof.
Material made from example below and comparative example is prepared as follows electrode and is tested for the property.
The preparation of electrode：
Molybdenum disulfide/carbon composite that embodiment is obtained is with carbon black, polyvinylidene fluoride according to 7:1.5:1.5 weight
Amount is than mixing, then is mixed with N-methyl pyrrolidone solution, adjusts slurry viscosity with N-methyl pyrrolidones, then uses slurry
Scraper is uniformly applied on the copper foil by alcohol washes, when vacuum drying 12 is small at 120 DEG C, then by tabletting, is cut,
Electrode is made.
Electrode performance is tested
It is tested for the property in fastening lithium ionic cell.Battery assembling mode is as follows：
Using lithium piece as to electrode, Celgard2300 uses LiPF containing 1M as membrane, electrolyte6EC-DEC-EMC
(1:1:1) solution, LiPF6It is lithium hexafluoro phosphate, EC is ethylene carbonate, and EMC is methyl ethyl ester.During test, temperature
For room temperature, using constant current charge-discharge, current density 100mA/g, control reference voltage is 0~3V.
Embodiment 1
0.1g 3-AP, 0.1mL formaldehyde and ammonium hydroxide are added to 30mLH2In O, it is sufficiently stirred.After stirring 0.5h, 20mL is taken
It in the solution that acetone is added to, is then centrifuged, is washed, dry, after grinding, 1200 DEG C of calcining 2h, obtain in Ar gas
To individual layer C hollow spherical powders.
Individual layer C hollow spherical powders prepared by 0.2g is taken to be dispersed in 40mL deionized waters, unit for uniform suspension are obtained, by 0.2g
In the suspension that ammonium molybdate, 0.2g thiocarbamides are added to, ultrasonic disperse 0.5h after 1h is stirred, suspension is transferred to reaction kettle
Afterwards, it is placed in 200 DEG C of insulating boxs hydro-thermal reaction for 24 hours；Suspension after hydro-thermal reaction is centrifuged, is washed, it is dry, after grinding
Obtain MoS2/ C powder.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1035mAh/g, and reversible de- lithium capacity is 887mAh/g, for the first time
Coulombic efficiency is 86%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 766mAh/g.
Embodiment 2
0.15g 3-AP, 0.15mL formaldehyde and ammonium hydroxide are added to 45mLH2In O, it is sufficiently stirred.After stirring 0.5h, take
It in the solution that 30mL acetone is added to, is then centrifuged, is washed, it is dry, after grinding, 1200 DEG C of calcinings in Ar gas
2h obtains double-deck C hollow spherical powders.
Double-deck C hollow spherical powders prepared by 0.2g is taken to be dispersed in 40mL deionized waters, unit for uniform suspension are obtained, by 0.2g
In the suspension that ammonium molybdate, 0.2g thiocarbamides are added to, ultrasonic disperse 0.5h after 1h is stirred, suspension is transferred to reaction kettle
Afterwards, it is placed in 200 DEG C of insulating boxs hydro-thermal reaction for 24 hours；Suspension after hydro-thermal reaction is centrifuged, is washed, it is dry, after grinding
Obtain MoS2/ C powder.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1045mAh/g, and reversible de- lithium capacity is 892mAh/g, for the first time
Coulombic efficiency is 85%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 778mAh/g.
Embodiment 3
0.32g 3-AP, 0.32mL formaldehyde and ammonium hydroxide are added to 96mLH2In O, it is sufficiently stirred.After stirring 0.5h, take
It in the solution that 64mL acetone is added to, is then centrifuged, is washed, it is dry, after grinding, 1200 DEG C of calcinings in Ar gas
2h obtains three layers of C hollow spherical powders.
Three layers of C hollow spherical powders prepared by 0.2g is taken to be dispersed in 40mL deionized waters, unit for uniform suspension are obtained, by 0.2g
In the suspension that ammonium molybdate, 0.2g thiocarbamides are added to, ultrasonic disperse 0.5h after 1h is stirred, suspension is transferred to reaction kettle
Afterwards, it is placed in 200 DEG C of insulating boxs hydro-thermal reaction for 24 hours；Suspension after hydro-thermal reaction is centrifuged, is washed, it is dry, after grinding
Obtain MoS2/ C powder.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1039mAh/g, and reversible de- lithium capacity is 893mAh/g, for the first time
Coulombic efficiency is 86%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 769mAh/g.
Embodiment 4
0.54g 3-AP, 0.54mL formaldehyde and ammonium hydroxide are added to 162mLH2In O, it is sufficiently stirred.After stirring 0.5h, take
It in the solution that 108mL acetone is added to, is then centrifuged, is washed, it is dry, after grinding, 1200 DEG C of calcinings in Ar gas
2h obtains four layers of C hollow spherical powders.
Four layers of C hollow spherical powders prepared by 0.2g is taken to be dispersed in 40mL deionized waters, unit for uniform suspension are obtained, by 0.2g
In the suspension that ammonium molybdate, 0.2g thiocarbamides are added to, ultrasonic disperse 0.5h after 1h is stirred, suspension is transferred to reaction kettle
Afterwards, it is placed in 200 DEG C of insulating boxs hydro-thermal reaction for 24 hours；Suspension after hydro-thermal reaction is centrifuged, is washed, it is dry, after grinding
Obtain MoS2/ C powder.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1041mAh/g, and reversible de- lithium capacity is 878mAh/g, for the first time
Coulombic efficiency is 84%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 763mAh/g.
Embodiment 5
0.6g 3-AP, 0.6mL formaldehyde and ammonium hydroxide are added to 180mLH2In O, it is sufficiently stirred.After stirring 0.5h, take
It in the solution that 120mL acetone is added to, is then centrifuged, is washed, it is dry, after grinding, 1200 DEG C of calcinings in Ar gas
2h obtains five layers of C hollow spherical powders.
Five layers of C hollow spherical powders prepared by 0.2g is taken to be dispersed in 40mL deionized waters, unit for uniform suspension are obtained, by 0.2g
In the suspension that ammonium molybdate, 0.2g thiocarbamides are added to, ultrasonic disperse 0.5h after 1h is stirred, suspension is transferred to reaction kettle
Afterwards, it is placed in 200 DEG C of insulating boxs hydro-thermal reaction for 24 hours；Suspension after hydro-thermal reaction is centrifuged, is washed, it is dry, after grinding
Obtain MoS2/ C powder.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1045mAh/g, and reversible de- lithium capacity is 889mAh/g, for the first time
Coulombic efficiency is 85%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 768mAh/g.
Embodiment 6
0.68g 3-AP, 0.68mL formaldehyde and ammonium hydroxide are added to 136mLH2In O, it is sufficiently stirred.After stirring 0.5h, take
It in the solution that 204mL acetone is added to, is then centrifuged, is washed, it is dry, after grinding, 1200 DEG C of calcinings in Ar gas
2h obtains six layers of C hollow spherical powders.
Six layers of C hollow spherical powders prepared by 0.2g is taken to be dispersed in 40mL deionized waters, unit for uniform suspension are obtained, by 0.2g
In the suspension that ammonium molybdate, 0.2g thiocarbamides are added to, ultrasonic disperse 0.5h after 1h is stirred, suspension is transferred to reaction kettle
Afterwards, it is placed in 200 DEG C of insulating boxs hydro-thermal reaction for 24 hours；Suspension after hydro-thermal reaction is centrifuged, is washed, it is dry, after grinding
Obtain MoS2/ C powder.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1030mAh/g, and reversible de- lithium capacity is 881mAh/g, for the first time
Coulombic efficiency is 85.5%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 755mAh/g.
Embodiment 7
0.7g 3-AP, 0.7mL formaldehyde and ammonium hydroxide are added to 140mLH2In O, it is sufficiently stirred.After stirring 0.5h, take
It in the solution that 210mL acetone is added to, is then centrifuged, is washed, it is dry, after grinding, 1200 DEG C of calcinings in Ar gas
2h obtains seven layers of C hollow spherical powders.
Seven layers of C hollow spherical powders prepared by 0.2g is taken to be dispersed in 40mL deionized waters, unit for uniform suspension are obtained, by 0.2g
In the suspension that ammonium molybdate, 0.2g thiocarbamides are added to, ultrasonic disperse 0.5h after 1h is stirred, suspension is transferred to reaction kettle
Afterwards, it is placed in 200 DEG C of insulating boxs hydro-thermal reaction for 24 hours；Suspension after hydro-thermal reaction is centrifuged, is washed, it is dry, after grinding
Obtain MoS2/ C powder.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1033mAh/g, and reversible de- lithium capacity is 882mAh/g, for the first time
Coulombic efficiency is 85%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 777mAh/g.
Comparative example 1
It is same as Example 1, except using 0.2g ammonium molybdates, 0.15g thiocarbamides.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 1020mAh/g, and reversible de- lithium capacity is 668mAh/g, for the first time
Coulombic efficiency is 65%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 534mAh/g.
Comparative example 2
It is same as Example 1, except using 0.2g ammonium molybdates, 0.39g thiocarbamides.
After testing, the lithium capacity embedding for the first time of products obtained therefrom is 935mAh/g, and reversible de- lithium capacity is 502mAh/g, for the first time storehouse
Logical sequence efficiency is 53%.
Reversible lithium insertion capacity after 30 Xun Huans before the lithium ion battery of the molybdenum disulfide of the present embodiment/carbon composite assembling
For 437mAh/g.
The amount that can be seen that ammonium molybdate and thiocarbamide from the comparison of comparative example 1 and 2 and embodiment 1 compares obtained material property
Important is 1 in the molar ratio of ammonium molybdate and thiocarbamide:It is optimal that material property is made during 2.5-2.6.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of preparation method of molybdenum disulfide/carbon composite, process are as follows：Using water as solvent, para-aminophenol (3- is added in
AP), formaldehyde and ammonium hydroxide prepare C hollow balls, and by regulating and controlling water, 3-AP, the amount of formaldehyde and ammonium hydroxide regulates and controls the layer of C hollow balls
Number；Using the C hollow balls of synthesis as skeleton, then using ammonium molybdate as molybdenum source, MoS is obtained by hydro-thermal method using thiocarbamide as sulphur source2/ C is multiple
Condensation material.
2. preparation method according to claim 1, comprises the following steps：
1. para-aminophenol, formaldehyde and ammonium hydroxide are added to the water, clear solution is stirred to get；
2. by acetone be added to step 1. gained clear solution in, stir to get suspension；
3. 2. suspension that step is prepared carries out separation of solid and liquid, washing is dried to obtain precipitation；
4. 3. precipitation that step is prepared is ground to fine-powder, calcining is subsequently cooled to room temperature and obtains powder；
5. 4. powder and ammonium molybdate, thiocarbamide that step is obtained are added sequentially in deionized water, uniform suspension is dispersed into；
6. 5. suspension that step is prepared heats reaction, after be cooled to room temperature, separation of solid and liquid, washing is dried to obtain institute
State molybdenum disulfide/carbon composite.
3. preparation method according to claim 2, which is characterized in that step 1. middle stirring when solution temperature be 25 DEG C, stir
The time mixed is 0.5~1h, is preferably 0.5h.
4. the preparation method according to Claims 2 or 3, which is characterized in that step 4. middle calcining temperature be 1000-1500
DEG C, it is preferably 1200 DEG C, the time is more than 1h, is preferably 2h.
5. according to claim 2-4 any one of them preparation methods, which is characterized in that step 5. middle powder, ammonium molybdate and sulphur
Urea mass ratio is 2:1~4:1~4；
Preferably, the molar ratio of ammonium molybdate and thiocarbamide is 1:2.5-2.6.
6. according to claim 2-5 any one of them preparation methods, which is characterized in that the step 5. deionized water of middle addition
Volume is 150-300 times of powder quality；
Preferably, disperse to carry out by stirring, ultrasound, preferably stir 1h, ultrasonic 0.5h.
7. according to claim 2-6 any one of them preparation methods, which is characterized in that step 6. middle heating temperature be 200
DEG C, the reaction time is for 24 hours.
8. according to claim 2-7 any one of them preparation methods, which is characterized in that step 3. and 6. middle washing use go from
Sub- water, absolute ethyl alcohol carry out successively；
Preferably, first it is washed with deionized 3 times, then is washed 2 times with absolute ethyl alcohol；
Preferably, dry temperature is 50~60 DEG C, is preferably 50 DEG C, and the dry time is 10-15h, is preferably 12h.
9. a kind of molybdenum disulfide/carbon composite prepared by claim 1-8 any one of them method.
10. a kind of application of the molybdenum disulfide/carbon composite in lithium ion battery negative material described in claim 9.
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