CN109449424A - A kind of compound carbon dots lithium ion battery anode material of cobalt molybdate and preparation method thereof - Google Patents
A kind of compound carbon dots lithium ion battery anode material of cobalt molybdate and preparation method thereof Download PDFInfo
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The present invention discloses a kind of compound carbon dots lithium ion battery anode material of cobalt molybdate and preparation method thereof, it is sintered using ammonium molybdate and cobalt chloride hexahydrate as raw material and generates molybdic acid cobalt precursor, it induces cobalt molybdate oriented growth to form raised nanoparticle structure using carbon dots by hydro-thermal method again, obtains the compound carbon dots lithium ion battery anode material of cobalt molybdate；This method has the characteristics that preparation process is simple, the period is short, low energy consumption, reproducible and yield is high, volume expansion can be alleviated using molybdic acid cobalt composite material prepared by the method, increase ion activation surface area, since the presence of carbon dots can produce certain fake capacitance, to improve the specific volume and energy density of material.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of compound carbon dots anode of lithium ion battery of cobalt molybdate
Material and preparation method thereof.
Background technique
Lithium ion battery is mainly used in electronic enterprises, and the energy-saving and environment-friendly lithium ion battery automobile of newest release
Due to its disadvantage of continuing a journey that stability is poor, capacity is low etc., us is promoted to look for the higher electrode material of capacity.Intercalation turns
Change reaction and alloying reaction, is three big mechanism of lithium ion battery reaction and the height for influencing materials theory capacity.And it is right
For possessing the material of conversion reaction, for the first time along with Li in process of intercalation2The generation of O, oxide become metal simple-substance, have
Multiple electronics participate in reaction, this kind of material often reversible specific capacity with higher and energy density.Cobalt molybdate, due to having height
Up to 980mAh g-1Capacity, and widely studied.[Sandhya,C.P.,John,B.,Gouri,C,
Sreemoolanadhan,H.,&Manwatkar,S.K.Promising anode material for lithium-ion
cells based on cobalt oxide synthesized by microwave heating.Ionics,2017.1-
9.][Wang,B.,Li,S.,Wu,X.,Liu,J.,Tian,W.,&Chen,J.Self-assembly of ultrathin
mesoporous CoMoO4nanosheet networks on flexible carbon fabric as a binder-
free anode for lithium-ion batteries.New Journal of Chemistry,2016.40(3),
2259-2267.] in charge and discharge process, due to lithium ion insertion and abjection so that material occur volume expansion, so as to cause
The decaying of capacity and the reduction of cycle life.Cobalt molybdate combination electrode material is prepared by the different preparation process of design to mention
The capacity and stability of high battery.[Xu,J.,Gu,S.,Fan,L.,Xu,P.,&Lu,B..Electrospun lotus root-
like CoMoO4@graphene nanofibers as high-performance anode for lithium ion
Batteries.Electrochimica Acta, 2016.196,125-130.] carbon dots, one of the new lover as carbon material,
Size is less than 10nm.Since it is with nontoxicity, excellent electric conductivity, photocatalytic and photoluminescence performance and by research
The great kindness of person.[Meng,X.,Chang,Q.,Xue,C.,Yang,J.,&Hu,S.Full-colour carbon dots:from
energy-efficient synthesis to concentration-dependent photoluminescence
properties.Chemical Communications,2017.53(21),3074.].
Summary of the invention
It, should present invention aims at a kind of compound carbon dots lithium ion battery anode material of cobalt molybdate and preparation method thereof is proposed
Method has preparation method simple, and process is easily-controllable, short preparation period, and the anode material cobalt molybdate purity is high prepared is used
Excellent electric conductivity, cyclical stability and high specific discharge capacity are shown in lithium ion battery.
Ion activation surface area is increased, the specific capacity and cyclical stability of lithium ion battery are improved.
To achieve the goals above, the present invention uses following technical scheme.
A kind of compound carbon dots lithium ion battery anode material preparation method of cobalt molybdate is with ammonium molybdate and cobalt chloride hexahydrate
Raw material is sintered by solid phase method and generates molybdic acid cobalt raw material；Cobalt molybdate is induced to grow along different crystal faces with carbon dots by hydro-thermal method again
Raised out, synthesis has the compound carbon dots nanostructure of the cobalt molybdate of small protrusion to get the compound carbon dots anode of lithium ion battery of cobalt molybdate
Material.
Further, include the following steps:
1) it, is added to using performic acid as oxide in coal tar pitch and stirs centrifugation, taking supernatant is then carbon dots solution；
2) it, takes the analytically pure ammonium molybdate of 0.15~1.15g to be put into mortar, adds 0.35~1.85mg, six chloride hydrate
Cobalt is put into crucible after being fully ground and is sintered in Muffle furnace, and Muffle furnace is heated up with the speed of 5~10 DEG C/min, from room temperature
80~120 DEG C are warming up to, 1~3h is kept the temperature；；300~450 DEG C are warming up to the speed of 1~5 DEG C/min again, keeps the temperature 1~3h；
3) product obtained is filtered respectively using water and ethyl alcohol, is cleaned repeatedly by, cooled to room temperature, dry, before obtaining
Drive body molybdic acid cobalt dust；It filters, clean repeatedly,
4) carbon dots solution of molybdic acid cobalt dust and the preparation of 5~45ml step 1), is obtained, after mixing, 10ml is added and goes
Ionized water is put into hydrothermal reaction kettle, is heated to 120~180 DEG C, keeps the temperature 6~12h；
5) it, after insulation reaction, is cooled to room temperature, after addition deionized water staticly settles, outwells upper layer supernatant, then
Deionized water is added, is so repeated as many times；Then products therefrom is repeatedly filtered with ethyl alcohol and deionized water, vacuum is dry
It is dry to get the compound carbon dots lithium ion battery anode material of cobalt molybdate.
Further, performic acid is added in coal tar pitch to stir in the step 1) and is centrifuged afterwards for 24 hours, taking supernatant is then carbon
Point solution.
Further, filter paper aperture is used to clean for 0.224 μm of suction filtration, 60~80 product obtained in the step 3)
It is dry at a temperature of DEG C to obtain presoma molybdic acid cobalt dust for 24 hours.
Further, it is cooled to room temperature after insulation reaction in the step 5), 10~50ml deionized water is added and stands
After one day, upper layer supernatant is outwelled, adds 10~50ml deionized water, so in triplicate；With ethyl alcohol and deionized water pair
Products therefrom filter 3-5 times, is put into vacuum drying oven and is dried to get the compound carbon dots anode of lithium ion battery of cobalt molybdate
Material.
A kind of compound carbon dots lithium ion battery anode material of cobalt molybdate, to have the nano junction of small protrusion along different crystal faces
Structure.
The compound carbon dots lithium ion battery anode material preparation method of cobalt molybdate of the invention, with ammonium molybdate and six chloride hydrates
Cobalt is raw material sintering generation molybdic acid cobalt precursor, then induces cobalt molybdate oriented growth to be formed with convex using carbon dots by hydro-thermal method
The nanoparticle structure risen obtains the compound carbon dots lithium ion battery anode material of cobalt molybdate；This method have preparation process it is simple,
The features such as period is short, low energy consumption, reproducible and yield is high, can be delayed using molybdic acid cobalt composite material prepared by the method
Volume expansion is solved, increases ion activation surface area, since the presence of carbon dots can produce certain fake capacitance, to improve material
Specific volume and energy density.
Preparation method of the present invention is simple, and process is easily-controllable, short preparation period, and the repeatability of product is high, and homogeneity is good, is conducive to
Large-scale production.The purity is high of cobalt molybdate made from the method for the present invention, is used for showing excellent conduction in lithium ion battery
Property, cyclical stability and high specific discharge capacity, can be as the application in terms of cathode material for high capacity lithium ion battery.
Detailed description of the invention
Fig. 1 is the TEM photo of prepared carbon dots
Fig. 2 is the XRD spectrum of prepared composite material
Fig. 3 is that the SEM of prepared composite material schemes
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
Embodiment 1
1) it, is added in coal tar pitch to stir using performic acid as oxide and be centrifuged afterwards for 24 hours, take supernatant, supernatant is then
For using performic acid as the carbon dots solution of solvent；
2) analytically pure the ammonium molybdate ((NH of 0.35g, is taken4)Mo7O24·4H2O it) is put into mortar, adds six water of 0.45mg
Close cobalt chloride (CoCl2·6H2O it) is ground, is fully ground half an hour；Mixture after grinding is put into crucible in Muffle furnace
Middle sintering；120 DEG C are warming up to the heating rate of 5 DEG C/min, keeps the temperature a hour；It is heated up again with the heating rate of 1 DEG C/min
To 450 DEG C, two hours are kept the temperature；
3), naturally cool to room temperature, by product obtained using 0.224 μm of aperture filter paper water and ethyl alcohol filter and it is clear
It washes 3-6 times, is put into vacuum oven and is dried for 24 hours for 70 DEG C；
4) product after, taking drying, which is added in 30ml deionized water, to be sufficiently mixed uniformly, and polytetrafluoroethyllining lining is put into
In, 180 DEG C of hydro-thermal reaction, 12h；
5), after water heating kettle naturally cools to room temperature, 10~50ml deionized water standing is added after one day, outwells on upper layer
Clear liquid adds 10~50ml deionized water, so in triplicate；Suction filtration 3- is carried out to products therefrom with ethyl alcohol and deionized water
It 5 times, is put into vacuum drying oven and is dried to get the compound carbon dots lithium ion battery anode material of cobalt molybdate.
Fig. 1 is the transmission plot of carbon quantum dot, and the carbon dots solution size prepared as can be seen from Figure 1 and distribution are all relatively more equal
One.
Fig. 2 is the XRD diagram of composite material, and corresponding pdf card 21-0868 can be seen that the composite material of preparation is monocline
The cobalt molybdate of phase.
Fig. 3 is composite material scanning figure, in figure it can be seen that material particle size prepared by the present invention Nano grade with
Under, it helps to improve material and obtains chemical property.
Embodiment 2
1) it, is added in coal tar pitch to stir using performic acid as oxide and be centrifuged afterwards for 24 hours, take supernatant, supernatant is then
For using performic acid as the carbon dots solution of solvent；
2) analytically pure the ammonium molybdate ((NH of 0.15g, is taken4)Mo7O24·4H2O it) is put into mortar, adds six water of 0.35mg
Close cobalt chloride (CoCl2·6H2O it) is ground, is fully ground half an hour；Mixture after grinding is put into crucible in Muffle furnace
Middle sintering；100 DEG C are warming up to the heating rate of 10 DEG C/min, keeps the temperature 3 hours；It is warming up to again with the heating rate of 3 DEG C/min
350 DEG C, keep the temperature 3 hours；
3) room temperature, is naturally cooled to, product water obtained and ethyl alcohol are filtered and cleaned 3-6 times, vacuum drying is put into
It is dried for 24 hours for 60 DEG C in case；
4) product after, taking drying, which is added in 5ml carbon dots solution, to be sufficiently mixed uniformly, and polytetrafluoroethyllining lining is put into
In, 150 DEG C of hydro-thermal reaction, 10h；
5), after water heating kettle naturally cools to room temperature, 10~50ml deionized water standing is added after one day, outwells on upper layer
Clear liquid adds 10~50ml deionized water, so in triplicate；Suction filtration 3- is carried out to products therefrom with ethyl alcohol and deionized water
It 5 times, is put into vacuum drying oven and is dried to get the compound carbon dots lithium ion battery anode material of cobalt molybdate.
Embodiment 3
1) it, is added in coal tar pitch to stir using performic acid as oxide and be centrifuged afterwards for 24 hours, take supernatant, supernatant is then
For using performic acid as the carbon dots solution of solvent；
2) analytically pure the ammonium molybdate ((NH of 0.65g, is taken4)Mo7O24·4H2O it) is put into mortar, adds six water of 0.85mg
Close cobalt chloride (CoCl2·6H2O it) is ground, is fully ground half an hour；Mixture after grinding is put into crucible in Muffle furnace
Middle sintering；80 DEG C are warming up to the heating rate of 8 DEG C/min, keeps the temperature 2 hours；300 are warming up to again with the heating rate of 5 DEG C/min
DEG C, keep the temperature 2 hours；
3) room temperature, is naturally cooled to, product water obtained and ethyl alcohol are filtered and cleaned 3-6 times, vacuum drying is put into
It is dried for 24 hours for 80 DEG C in case；
4) product after, taking drying, which is added in 30ml carbon dots solution, to be sufficiently mixed uniformly, and polytetrafluoroethyllining lining is put into
In, 180 DEG C of hydro-thermal reaction, 6h；
5), after water heating kettle naturally cools to room temperature, 10~50ml deionized water standing is added after one day, outwells on upper layer
Clear liquid adds 10~50ml deionized water, so in triplicate；Suction filtration 3- is carried out to products therefrom with ethyl alcohol and deionized water
It 5 times, is put into vacuum drying oven and is dried to get the compound carbon dots lithium ion battery anode material of cobalt molybdate.
Embodiment 4
1) it, is added in coal tar pitch to stir using performic acid as oxide and be centrifuged afterwards for 24 hours, take supernatant, supernatant is then
For using performic acid as the carbon dots solution of solvent；
2) analytically pure the ammonium molybdate ((NH of 1.15g, is taken4)Mo7O24·4H2O it) is put into mortar, adds six water of 1.85mg
Close cobalt chloride (CoCl2·6H2O it) is ground, is fully ground half an hour；Mixture after grinding is put into crucible in Muffle furnace
In；120 DEG C are warming up to the heating rate of 2 DEG C/min, keeps the temperature 2 hours；400 DEG C are warming up to the heating rate of 2 DEG C/min again,
Heat preservation 1 hour；
3) room temperature, is naturally cooled to, product water obtained and ethyl alcohol are filtered and cleaned 3-6 times, vacuum drying is put into
It is dried for 24 hours for 60 DEG C in case；
4) product after, taking drying, which is added in 45ml carbon dots solution, to be sufficiently mixed uniformly, and polytetrafluoroethyllining lining is put into
In, 120 DEG C of hydro-thermal reaction, 12h；
5), after water heating kettle naturally cools to room temperature, 10~50ml deionized water standing is added after one day, outwells on upper layer
Clear liquid adds 10~50ml deionized water, so in triplicate；Suction filtration 3- is carried out to products therefrom with ethyl alcohol and deionized water
It 5 times, is put into vacuum drying oven and is dried to get the compound carbon dots lithium ion battery anode material of cobalt molybdate.
The present invention first generates cobalt molybdate raw material using ammonium molybdate and cobalt chloride hexahydrate as raw material, by solid phase method sintering；Again
Protrusion, the synthetic and synthesis technology of the method for the present invention are grown along different crystal faces with carbon dots induction cobalt molybdate using hydro-thermal method
The special construction for having synthesized the cobalt molybdate with small protrusion can further improve the capacity of lithium ion battery and forthright again
Energy.
In conclusion the method for the present invention mentality of designing is novel, it is simple to operate.Three generated with the direct step of hydro-thermal method
Molybdenum oxide is that bulk material be easy to cause body when bulk material is applied to lithium ion battery negative material in charge and discharge process
Structure collapses, so that the capacity of material reduces and cyclical stability is deteriorated.The present invention can not only expand as after the dry distillation of coal
Waste residue coal tar pitch purposes, can more improve the specific capacity of lithium ion battery.In addition, preparation process of the present invention is simply easy to control
System, and low energy consumption, the repeatability of product is also preferable, is conducive to be mass produced.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (6)
1. a kind of compound carbon dots lithium ion battery anode material preparation method of cobalt molybdate, it is characterised in that: with ammonium molybdate and six water
Conjunction cobalt chloride is raw material, is sintered by solid phase method and generates molybdic acid cobalt raw material；Induce cobalt molybdate along not with carbon dots by hydro-thermal method again
The isomorphous, which is looked unfamiliar, grows protrusion, synthesis have the compound carbon dots nanostructure of the cobalt molybdate of small protrusion to get the compound carbon dots lithium of cobalt molybdate from
Sub- battery anode material.
2. preparation method as described in claim 1, it is characterised in that include the following steps:
1) it, is added to using performic acid as oxide in coal tar pitch and stirs centrifugation, taking supernatant is then carbon dots solution；
2) it, takes the analytically pure ammonium molybdate of 0.15~1.15g to be put into mortar, adds 0.35~1.85mg cobalt chloride hexahydrate and fill
It is put into crucible after point grinding and is sintered in Muffle furnace, Muffle furnace is heated up with the speed of 5~10 DEG C/min, is heated up from room temperature
To 80~120 DEG C, 1~3h is kept the temperature；300~450 DEG C are warming up to the speed of 1~5 DEG C/min again, keeps the temperature 1~3h；
3) product obtained is filtered respectively using water and ethyl alcohol, is cleaned repeatedly by, cooled to room temperature, dry, obtains presoma
Molybdic acid cobalt dust；
4) carbon dots solution of molybdic acid cobalt dust and the preparation of 5~45ml step 1), is obtained, after mixing, 10ml deionization is added
Water is put into hydrothermal reaction kettle, is heated to 120~180 DEG C, keeps the temperature 6~12h；
5) it, after insulation reaction, is cooled to room temperature, after addition deionized water staticly settles, outwells upper layer supernatant, add
Deionized water is so repeated as many times；Then products therefrom is repeatedly filtered with ethyl alcohol and deionized water, is dried in vacuo, i.e.,
Obtain the compound carbon dots lithium ion battery anode material of cobalt molybdate.
3. preparation method as claimed in claim 2, it is characterised in that: performic acid is added in coal tar pitch in the step 1)
Stirring is centrifuged afterwards for 24 hours, and taking supernatant is then carbon dots solution.
4. preparation method as claimed in claim 2, it is characterised in that: product obtained is used filter paper hole in the step 3)
Diameter is 0.224 μm of suction filtration cleaning, drying obtains presoma molybdic acid cobalt dust for 24 hours at a temperature of 60~80 DEG C.
5. preparation method as claimed in claim 2, it is characterised in that: in the step 5) after insulation reaction, be cooled to
Room temperature is added 10~50ml deionized water standing after one day, outwells upper layer supernatant, add 10~50ml deionized water, such as
This is in triplicate；Products therefrom filter 3-5 times with ethyl alcohol and deionized water, is put into vacuum drying oven and is dried, i.e.,
Obtain the compound carbon dots lithium ion battery anode material of cobalt molybdate.
6. a kind of compound carbon dots anode of lithium ion battery material of cobalt molybdate based on the preparation of any one of claim 1-5 the method
Material, to have the nanostructure of small protrusion along different crystal faces.
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| WO2022268055A1 (en) * | 2021-06-22 | 2022-12-29 | 重庆文理学院 | Method for preparing nio@comoo4/nf capacitor electrode |
| CN115490307A (en) * | 2022-09-01 | 2022-12-20 | 同济大学 | Sodium ion removal material CoMoO 4 @ CQDs-NCNTs and preparation method and application thereof |
| CN115490307B (en) * | 2022-09-01 | 2023-08-29 | 同济大学 | Sodium ion removing material CoMoO 4 @CQDs-NCNTs and preparation method and application thereof |
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