CN110323424A - The preparation method of titania modified molybdenum disulfide lithium ion battery negative material - Google Patents
The preparation method of titania modified molybdenum disulfide lithium ion battery negative material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of titania modified molybdenum disulfide lithium ion battery negative material, comprising the following steps: sodium molybdate, thiocarbamide are added in deionized water, adds the mixing of oxalic acid uniform stirring, obtains mixed liquor；Mixed liquor reacts in water heating kettle, obtains MoS2；By MoS2It is dissolved in dehydrated alcohol, ammonia spirit ultrasonic treatment is added, is added dropwise after butyl titanate in 45~60 DEG C of 22~26h of reaction；After reacting gains centrifugation, washing, drying finally obtain titania modified molybdenum disulfide in 500~800 DEG C of heat treatment (4 ± 0.5) hours in an inert atmosphere.The titania modified molybdenum disulfide is used as lithium ion battery negative material, can get excellent storage lithium performance, enhances cyclical stability.
Description
Technical field
The present invention relates to material modifications and field of lithium ion battery, more particularly to a kind of titania modified molybdenum disulfide
The preparation method of lithium ion battery negative material.
Background technique
Molybdenum disulfide (MoS2) it is a kind of transition metal binary compound with graphene two-dimensional layered structure, You Liufang
The single-layer or multi-layer MoS of crystallographic system2It constitutes.Single layer MoS2Class " sandwich " knot is formed by sulphur atom layer-molybdenum atom layer-sulphur atom layer
Structure is connected in layer with covalent bond between S-Mo-S, is combined between layers by model ylid bloom action power.Layer structure is by several
A single layer MoS2It accumulates, interlamellar spacing is about 0.615nm.This biggish interlamellar spacing is conducive to the embedding de- of lithium ion, MoS2
Molecule carries out change type with lithium ion and reacts, and obtains 669mAh g-1High theoretical specific capacity.In addition, molybdenum source and sulphur source be located in it is rich
It is rich, cheap and easy to get, therefore, MoS2It is considered as a kind of very promising lithium ion battery negative material.However, six side 2H
Stable phase MoS2Material is a kind of semiconductor material, and relatively low conductivity causes the high rate performance of material bad.In addition, MoS2It is following
Polysulfide is generated during ring, is generated shuttle effect, is caused MoS2The loss of active material and the destruction of electrode structure, are caused
Capacity rapid decay.
Titanium dioxide (TiO2) there is at low cost, environmental-friendly, stable chemical performance, charge and discharge platform height (1.7V Li+/
Li), in cyclic process the advantages that volume change small (3-4%), it is considered to be a kind of important lithium ion battery negative material.Newly
Into studies have shown that constructing MoS2With TiO2Composite material can obtain good synergistic effect, realize mentioning for electrochemical lithium storage performance
It rises.Chinese invention patent CN201610013574 discloses a kind of TiO of stacked in layers as negative electrode of lithium ion battery2/MoS2
The preparation method of composite material of core-shell structure.Chinese invention patent CN201811240121 reports a kind of TiO2/C/MoS2It is hollow
The preparation method of hybrid microspheres, the material are used for lithium ion battery negative material, show high reversible capacity, excellent multiplying power
Performance.
Although mean disclosed above successfully obtains the improvement of electrochemical lithium storage performance, but be all with TiO2For matrix,
Do not solve MoS2The bad problem of more lithium sulfides dissolution in cyclic process, structural stability.Therefore, with MoS2For matrix, benefit
Use TiO2Modified MoS2It is the important channel alleviated more lithium sulfide dissolutions, promote material structure stability.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of titania modified molybdenum disulfide negative electrode of lithium ion battery materials
The preparation method of material, this method simple process and low cost, mild condition, the modification by titanium dioxide to molybdenum disulfide, enhancing
The cyclical stability of resulting materials.
The present invention provides a kind of preparation method of titania modified molybdenum disulfide lithium ion battery negative material, including with
Lower step:
1), sodium molybdate, thiocarbamide are added in deionized water, after stirring is dissolved to sodium molybdate, thiocarbamide, it is equal to add oxalic acid
It is even to be stirred, obtain mixed liquor；The sodium molybdate: thiocarbamide: oxalic acid=1:(1.6 ± 0.2): the weight ratio of (0.5 ± 0.05)；
The mixed liquor is transferred in water heating kettle (water heating kettle that liner is polytetrafluoroethylene (PTFE)), in 180~220 DEG C after sealing
React 22~26h；
Gains centrifugation is reacted, is centrifuged after resulting washing of precipitate dry (50~70 DEG C of 22~26h of drying), obtains MoS2
(powdered)；
2) MoS for, taking 0.1g step 1) to prepare2Material is dissolved in (120 ± 20) ml dehydrated alcohol, and mass concentration is added
For 25~28% ammonia spirit (0.4 ± 0.04) ml；Ultrasonic treatment 3~after five minutes, (time for adding is 3~10 points for dropwise addition
Clock) 1~3m of butyl titanate, the mixed solution is transferred to water bath device under 300~500rpm revolving speed in 45 after being added dropwise
~60 DEG C of 22~26h of reaction；
3), by step 2) reaction gains centrifugation, be centrifuged it is dry after the washing of resulting sediment (50~70 DEG C of drying 22~
26h), finally in inert atmosphere (such as argon atmosphere) in 500~800 DEG C of heat treatment (4 ± 0.5) hours, titanium dioxide is obtained
Titanium modified molybdenum disulfide material.
The improvement of preparation method as titania modified molybdenum disulfide lithium ion battery negative material of the invention: institute
It states in step 1), the deionized water of every 1g sodium molybdate adapted (80 ± 20) ml.
Preparation method as titania modified molybdenum disulfide lithium ion battery negative material of the invention it is further
It improves: being carried out under 180~360w ultrasonic power in the step 2) ultrasonic treatment 3~5 minutes.
Preparation method as titania modified molybdenum disulfide lithium ion battery negative material of the invention it is further
It improves:
In the step 2), the dosage of butyl titanate is 2ml, for 24 hours in 45 DEG C of reactions；
In the step 3), it is heat-treated 4 hours in 600 DEG C.
The present invention has equally distributed MoS first using sodium molybdate and thiocarbamide as molybdenum source and sulphur source, by hydro-thermal method synthesis2
Material；Then with prepared MoS2It is synthesized by immersion method in MoS for matrix using butyl titanate as titanium source2Shape on matrix
At the presoma of titanium, i.e., using dynamics Controlling immersion method in MoS2Material surface carries out titanizing processing.Finally in inert atmosphere
It is heat-treated to obtain titania modified molybdenum disulfide material (TiO in (such as argon atmosphere)2Modified MoS2Material).By
After titania modified, molybdenum disulfide material morphology structure is kept very well；It is combined between titanium dioxide and molybdenum disulfide tight
It is close, the interface of stable structure is obtained, the transmission for enhancing electronics and ion is conducive to.In addition, titanium dioxide is able to suppress shuttle effect
It answers.
The present invention is with MoS2For matrix, by immersion method in MoS2TiO is plated on matrix2Clad, immersion method can be controlled very well
TiO processed2The thickness and MoS of clad2Bonding state, TiO2Clad can alleviate MoS2More vulcanizations in charge and discharge process
Lithium problems of dissolution keeps the stability of material structure, obtains excellent storage lithium performance.
In conclusion preparation method mild condition of the invention, simple process and cheap；Pass through TiO2Modified MoS2,
More lithium sulfides can be effectively adsorbed, its dissolution is alleviated, promote the structural stability of material, therefore, this titania modified two
Material molybdenum sulfide is used as lithium ion battery negative material, can get excellent storage lithium performance, enhances cyclical stability.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 is MoS prepared by embodiment 12XRD diagram；
Fig. 2 is MoS prepared by embodiment 1210000 times of scanning electron microscopic picture；
Fig. 3 is that different embodiments prepare resulting TiO2Modified MoS2Material XRD diagram；
It (a) is embodiment 2；(b) embodiment 6；It (c) is embodiment 12；
Fig. 4 is TiO prepared by embodiment 62Modified MoS210000 times of scanning electron microscopic picture of material；
Fig. 5 is MoS prepared by embodiment 12Cycle performance figure；
Fig. 6 is TiO prepared by embodiment 62Modified MoS2The cycle performance figure of material.
Specific embodiment
In conjunction with the following specific embodiments technical solution that the present invention is furture elucidated, but the present invention is not limited in detail below
Embodiment, all equivalent transformations made on the basis of the technical solutions of the present application each fall within protection scope of the present invention.Below with reference to reality
Example is applied to be described in further details the present invention.
Embodiment 1, MoS2The preparation of material:
It weighs 1g (4.85mmol) sodium molybdate and 1.6g (21.05mmol) thiocarbamide is added in 80ml deionized water, stirring is extremely
Sodium molybdate, thiocarbamide dissolve, and 0.5g oxalic acid is then added, and uniform stirring mixing obtains mixed liquor；Above-mentioned mixed liquor is transferred to poly- four
In vinyl fluoride water heating kettle liner, reacted for 24 hours in 200 DEG C after sealing；
Reaction gains are centrifuged (being centrifuged 5 minutes under the revolving speed of 8000rpm), the resulting sediment of centrifugation after being cooled to room temperature
(washing is until eluent is neutrality), dry (60 DEG C of drying are for 24 hours) are successively washed, MoS is obtained2Material.
By MoS obtained2Material, acetylene black and PVDF are that 7:2:1 carries out being mixed to get cementitious slurry with mass ratio, by it
It is coated uniformly on round copper foil (diameter 1.4cm), is to electrode, 1mol/L LiPF with metal lithium sheet6/ DMC+EC (volume
Than being electrolyte for 1:1), Celgard 2300 is diaphragm, button cell is assembled into glove box, in 0~3.0V voltage model
Enclose interior carry out electrochemical property test.In 0.3A g-1Its reversible capacity is 282mAh g after circulation 100 times-1。
Following embodiment is all made of the embodiment 1 and prepares resulting MoS2Material.
Embodiment 2 prepares titania modified molybdenum disulfide
Weigh the MoS of the above-mentioned preparation of 0.1g2Material is dissolved in 120ml dehydrated alcohol, and 0.4ml ammonia spirit (matter is added
Measuring concentration is 26%), to be ultrasonically treated and (handled 3 minutes under 40KHZ, 360w ultrasonic power), is then slowly added dropwise into 1ml
Butyl titanate (the addition time is 3 minutes), is transferred to water bath device in 300~500rpm revolving speed for mixed solution after being added dropwise
Under in 45 DEG C reaction for 24 hours.
It will reaction gains centrifugation (being centrifuged 5 minutes under the revolving speed of 8000rpm), the resulting sediment washing (washing of centrifugation
Up to eluent is neutrality) and it is dry (60 DEG C of drying are for 24 hours), finally 500 DEG C heat treatment 4 hours in argon atmosphere, obtain two
Titanium oxide modified molybdenum disulfide material.
" 500 DEG C are heat-treated 4 hours " of embodiment 2 is changed to " 800 DEG C are heat-treated 4 hours " by embodiment 3；Remaining is equivalent
In embodiment 2.
" 45 DEG C of water-baths are for 24 hours " of embodiment 2 is changed to " 60 DEG C of water-baths are for 24 hours " by embodiment 4；Remaining is equal to implementation
Example 2.
The dosage of the butyl titanate of embodiment 2 is changed to " 2ml " by " 1ml " by embodiment 5；Remaining is equal to embodiment
2。
The dosage of the butyl titanate of embodiment 2 is changed to " 2ml " by embodiment 6 by " 1ml ", and will " 500 DEG C of heat treatments 4
Hour " it is changed to " 600 DEG C are heat-treated 4 hours "；Remaining is equal to embodiment 2.
The dosage of the butyl titanate of embodiment 2 is changed to " 2ml " by embodiment 7 by " 1ml ", and will " 500 DEG C of heat treatments 4
Hour " it is changed to " 800 DEG C are heat-treated 4 hours "；Remaining is equal to embodiment 2.
The dosage of the butyl titanate of embodiment 2 is changed to " 2ml " by embodiment 8 by " 1ml ", and by " 45 DEG C of water-baths
It is changed to " 60 DEG C of water-baths are for 24 hours " for 24 hours "；Remaining is equal to embodiment 2.
The dosage of the butyl titanate of embodiment 2 is changed to " 3ml " by " 1ml " by embodiment 9, remaining is equal to embodiment
2。
The dosage of the butyl titanate of embodiment 2 is changed to " 3ml " by embodiment 10 by " 1ml ", will " 500 DEG C of heat treatments 4
Hour " being changed to " 800 DEG C are heat-treated 4 hours ", remaining is equal to embodiment 2.
The dosage of the butyl titanate of embodiment 2 is changed to " 3ml " by embodiment 11 by " 1ml ", and " 45 DEG C of water-baths
It is changed to that " 60 DEG C of water-baths are for 24 hours for 24 hours "；Remaining is equal to embodiment 2.
The dosage of the butyl titanate of embodiment 2 is changed to " 3ml " by embodiment 12 by " 1ml ", and " 45 DEG C of water-baths
Be changed to for 24 hours " " 60 DEG C of reactions for 24 hours ", " 500 DEG C be heat-treated 4 hours " are changed to " 800 DEG C are heat-treated 4 hours "；Remaining is equal to reality
Apply example 2.
Experiment one,
By titania modified molybdenum disulfide material, acetylene black and PVDF made from 2~embodiment of above-described embodiment 12 with
Mass ratio is that 7:2:1 carries out being mixed to get cementitious slurry, is coated uniformly on round copper foil (diameter 1.4cm), with gold
Belonging to lithium piece is to electrode, and 1mol/L LiPF6/DMC+EC (volume ratio 1:1) is electrolyte, and Celgard 2300 is diaphragm,
Button cell is assembled into glove box, in carrying out electrochemical property test in 0~3.0V voltage range.In 0.3A g-1Circulation 100
Its reversible capacity is described in table 1 below after secondary.
Table 1
Comparative example 1-1, the dosage of ammonia spirit in embodiment 6 is changed to 0.3ml by 0.4ml；Remaining is equal to embodiment
6。
Comparative example 1-2, the dosage of ammonia spirit in embodiment 6 is changed to 0.5ml by 0.4ml；Remaining is equal to embodiment
6。
Comparative example 2, MoS2Material the preparation method comprises the following steps: use the molybdenum trioxide of 4.85mmol for molybdenum source, use
The hydrogen sulfide of 21.05mmol be sulphur source, in argon atmosphere at 650 DEG C 5 hours synthesis of carbon/molybdenum disulfide materials of high-temperature calcination.
The MoS that the molybdenum disulfide material substitution embodiment 1 being in the above way prepared is prepared2Material, remaining etc.
It is same as embodiment 6.
Comparative example 3, MoS2Material the preparation method comprises the following steps: use the molybdenum trioxide of 4.85mmol for molybdenum source, use
The elemental sulfur of 21.05mmol be sulphur source, in argon atmosphere at 650 DEG C 5 hours synthesis of carbon/molybdenum disulfide materials of high-temperature calcination.
The MoS that the molybdenum disulfide material substitution embodiment 1 being in the above way prepared is prepared2Material, remaining etc.
It is same as embodiment 6.
Comparative example 4, using sulphur sodium molybdate as raw material 400 DEG C of pyrolysis 4h in argon atmosphere, obtain curing molybdenum materials
Material.The MoS that the molybdenum disulfide material substitution embodiment 1 being in the above way prepared is prepared2Material, remaining is equal to reality
Apply example 6.
Comparative example 5, using sulphur sodium molybdate as raw material 400 DEG C of pyrolysis 4h in hydrogen reducing atmosphere, obtain curing
Molybdenum material.The MoS that the molybdenum disulfide material substitution embodiment 1 being in the above way prepared is prepared2Material, remaining is equivalent
In embodiment 6.
Above-mentioned all comparative examples are detected according to above-mentioned one the method for experiment, acquired results and embodiment 6
Comparison is described in table 2 below.
Table 2
The above list is only a few specific embodiments of the present invention for finally, it should also be noted that.Obviously, this hair
Bright to be not limited to above embodiments, acceptable there are many deformations.Those skilled in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
Claims (4)
1. the preparation method of titania modified molybdenum disulfide lithium ion battery negative material, it is characterised in that including following step
It is rapid:
1), sodium molybdate, thiocarbamide are added in deionized water, after stirring is dissolved to sodium molybdate, thiocarbamide, oxalic acid is added and uniformly stirs
Mixing is mixed, mixed liquor is obtained；The sodium molybdate: thiocarbamide: oxalic acid=1:(1.6 ± 0.2): the weight ratio of (0.5 ± 0.05)；
The mixed liquor is transferred in water heating kettle, in 180~220 DEG C of 22~26h of reaction after sealing；It is washed after reaction gains centrifugation
It washs, dry, obtain MoS2；
2) MoS for, taking 0.1g step 1) to prepare2Be dissolved in (120 ± 20) ml dehydrated alcohol, be added mass concentration be 25~
28% ammonia spirit (0.4 ± 0.04) ml；Ultrasonic treatment 3~after five minutes, 1~3m of butyl titanate is added dropwise, after being added dropwise
By the mixed solution in 45~60 DEG C of 22~26h of reaction under 300~500rpm revolving speed；
3), by step 2) reaction gains centrifugation, be centrifuged it is dry after the washing of resulting sediment, finally in an inert atmosphere in
500~800 DEG C of heat treatment (4 ± 0.5) hours, obtain titania modified molybdenum disulfide.
2. the preparation method of titania modified molybdenum disulfide lithium ion battery negative material according to claim 1,
It is characterized in that:
In the step 1), the deionized water of every 1g sodium molybdate adapted (80 ± 20) ml.
3. the preparation method of titania modified molybdenum disulfide lithium ion battery negative material according to claim 1 or 2,
It is characterized by: being carried out under 180~360w ultrasonic power in the step 2) ultrasonic treatment 3~5 minutes.
4. the preparation method of titania modified molybdenum disulfide lithium ion battery negative material according to claim 3,
It is characterized in that:
In the step 2), the dosage of butyl titanate is 2ml, for 24 hours in 45 DEG C of reactions；
In the step 3), it is heat-treated 4 hours in 600 DEG C.
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