CN109309198A - A kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method - Google Patents
A kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention discloses a kind of preparation methods of negative electrode of lithium ion battery red phosphorus/graphene composite material.The method is fully dispersed in a solvent by red phosphorus and graphene by low temperature liquid polymerization process, and by red phosphorus and graphene surface electrical behavior difference in a solvent, makes red phosphorus nanometer sheet uniform load on the surface of graphene, obtain uniform red phosphorus/graphene composite material.The method includes purification red phosphorus, preparation mixed dispersion liquid, centrifugal treating and freeze-dryings.Preparation method of the present invention is simple, environmental-friendly, low in cost；In obtained red phosphorus/graphene composite material, red phosphorus is amorphous nano-sheet pattern, and is uniformly adhered on the surface of graphene, utilization rate with higher, improves the specific capacity and cycle charge discharge electrical stability of lithium ion battery significantly.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of that unbodied red phosphorus nanometer sheet is supported on graphite
The preparation method on alkene surface, and the negative electrode material by red phosphorus/graphene composite material obtained as lithium ion battery.
Background technique
Lithium ion battery is concerned with the advantages that its high-energy-density, high voltage and long-life.Commercial li-ion battery is adopted
Use graphite material as cathode, LiFePO4, cobalt acid lithium, LiMn2O4 etc., as anode, utilize lithium ion containing lithium metal oxide
" rocking chair effect " between positive and negative anodes contributes capacity.However, the specific capacity of graphite cathode is lower, high rate performance is limited, it is difficult to
Meet today's society for energy-storage system increasingly higher demands, thus the negative electrode material for finding new high capacity density becomes lithium
The key of ion battery raising energy density.
It is elemental phosphorous with its height ratio capacity (2595mAh g in numerous potential electrode materials-1) obtain more concern.
Elemental phosphorous there are three types of allotropes: white phosphorus, black phosphorus and red phosphorus.Wherein, white phosphorus is inflammable, from a security point of view, is not suitable for
As electrode material.Black phosphorus has obtained extensive research because of its high conductivity, need to be however, its preparation process is complicated harsh
It under conditions of high temperature and pressure and inert gas shielding, is synthesized by dedicated equipment, considerably increases its cost.In comparison,
The advantages such as red phosphorus has height ratio capacity, low in cost, Environmental compatibility is good, are expected to as lower-cost, alternative graphite
Negative electrode material.Currently, red phosphorus as lithium ion battery negative material there are the problem of essentially consist in it after embedding lithium there are larger
Volume expansion (490%), and electric conductivity is poor.It is then desired to which itself and other carbon materials are especially had abundant hole knot
The carbon material of structure carries out compound.On the one hand, the electron-transport efficiency of composite material can be improved in the high conductivity of carbon material；It is another
Aspect, a large amount of pore structures in carbon material, can sufficiently accommodate volume expansion of the red phosphorus in electrochemical reaction, to keep
Stable electrode structure.Based on considerations above, the graphene with high conductivity, high strength and high-flexibility is considered
It is ideal carbon support material.After graphene is fully dispersed in a solvent, continuous three-dimensional network can be formed, is the liquid phase of red phosphorus
Synthesis provides a possibility that more.The flexibility of graphene can also effectively accommodate the volume expansion of red phosphorus, answering in buffer electrode
Power, to obtain red phosphorus/graphene composite material of high stability.
Red phosphorus is being higher than 450 degree of temperature generally by high-temperature process by existing red phosphorus and the compound technique of graphene
Degree distillation, so that red phosphorus steam uniform deposition is in the hole of graphene network.During the disadvantages of this method is cooling
The white phosphorus of formation is inflammable, there is certain risk, and the removal of white phosphorus then needs to use the toxic reagents such as carbon disulfide, and safety is hidden
Suffer from larger.And since red phosphorus is introduced by steam, so the percentage of red phosphorus in the composite is difficult to control.And high warm
Processing can also expend a large amount of energy, increase cost.
The present invention passes through low temperature liquid polymerization process, and graphene is fully dispersed in a solvent, and by red phosphorus and graphene molten
Surface electrical behavior difference in agent makes red phosphorus nanometer sheet uniform load on the surface of graphene, obtains uniform red phosphorus/graphene composite wood
Material.Prepared composite material is in the negative electrode material as lithium ion battery, specific capacity with higher and superior circulation
Performance.
Summary of the invention
In order to solve the problems, such as that existing red phosphorus exists with graphene combination process, the present invention provides a kind of lithium ion battery
Cathode red phosphorus/graphene composite material preparation method.The method is by low temperature liquid polymerization process, in a solvent by red phosphorus and graphene
It is fully dispersed, and by red phosphorus and graphene surface electrical behavior difference in a solvent, make red phosphorus nanometer sheet uniform load in graphene
Surface obtains uniform red phosphorus/graphene composite material.The composite material prepared by the method is as lithium ion battery
Negative electrode material when, specific capacity with higher and superior cycle performance.
To realize above-mentioned target, the invention adopts the following technical scheme:
A kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method, the method pass through low temperature liquid polymerization process,
Red phosphorus and graphene is fully dispersed in a solvent, and by red phosphorus and graphene surface electrical behavior difference in a solvent, make red phosphorus
Nanometer sheet uniform load on the surface of graphene, obtains uniform red phosphorus/graphene composite material.
It the described method comprises the following steps:
1) red phosphorus is purified: by commercial red phosphorus ball milling in deionized water, the vacuum drying after hydro-thermal process 12h at 200 DEG C；
2) prepare mixed dispersion liquid: by after purification red phosphorus and graphene dispersion in ethyl alcohol/deionized water mixed solvent
In, 5~120min of ultrasonic disperse obtains uniform mixed dispersion liquid；
3) centrifugal treating: by step 2) mixed dispersion liquid obtained by multiple centrifugal treating, exchange solvent be go from
Sub- water obtains pure mixture；
4) it is freeze-dried: step 3) mixture obtained being freezed at -80 DEG C, is lyophilized, is obtained by freeze drier
Red phosphorus/graphene composite material.
Preferably, mixed solvent described in step 2) is the mixed solvent of alcohol-water, and wherein the volume ratio of ethyl alcohol and water is
1:5-1:1。
Preferably, concentration of the graphene in mixed dispersion liquid is 0.1~10g/L.
Preferably, the mass ratio of red phosphorus and graphene in mixed dispersion liquid is 1:2~4:1.
Red phosphorus is negative in the zeta current potential of in the mixed solvent, and graphene is positive in the zeta current potential of in the mixed solvent, from
And make the two that mutually absorption occur in the solution, form stable composite construction.
The advantages and benefits of the present invention are: preparation method of the invention is simple, environmental-friendly；Obtained red phosphorus/
In graphene composite material, red phosphorus is amorphous nano-sheet pattern, and is uniformly adhered on the surface of graphene, benefit with higher
With rate, the specific capacity and cycle charge discharge electrical stability of lithium ion battery are improved significantly.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is red phosphorus/graphene composite material XRD diagram of the embodiment 1 preparation.
Fig. 2 is that red phosphorus/graphene composite material SEM figure of the embodiment 1 preparation and corresponding phosphorus, carbon are distributed
Figure.
Fig. 3 is that red phosphorus/graphene composite material of the embodiment 1 preparation and the TEM of grapheme material scheme.
Fig. 4 is red phosphorus/graphene composite material high power TEM figure of the embodiment 1 preparation.
Fig. 5 is red phosphorus/graphene composite material of the embodiment 1 preparation and the cyclic curve of red phosphor material.
Specific embodiment
Embodiment 1
1) purify red phosphorus: by commercial red phosphorus, ball milling 6h, revolving speed 300rpm are then lauched at 200 DEG C in deionized water
It is heat-treated 12h, then vacuum drying, the red phosphorus powder purified；
2) mixed dispersion liquid is prepared: by 80mg red phosphorus powder, 20mg graphene in 50mL ethyl alcohol/deionized water (volume ratio
Ultrasonic disperse 30min in mixed solution 1:3) obtains graphene-red phosphorus mixed dispersion liquid；
3) centrifugal treating: for several times by mixed dispersion liquid centrifugation, exchange solvent is deionized water, obtains pure mixture；
4) it is freeze-dried: step 3) mixture obtained being freezed at -80 DEG C, is lyophilized, is obtained by freeze drier
Red phosphorus/graphene composite material.
Referring to attached drawing 1, this figure is the XRD diagram of red phosphorus/graphene composite material manufactured in the present embodiment, can from figure
Red phosphorus is amorphous structure out.
Referring to attached drawing 2, this figure is the SEM figure and corresponding phosphorus, carbon of red phosphorus/graphene composite material manufactured in the present embodiment
Distribution diagram of element, the red phosphorus/graphene composite material as can be seen from the figure prepared form uniform composite structure.
Referring to attached drawing 3, this figure is the TEM figure of red phosphorus/graphene composite material and grapheme material manufactured in the present embodiment,
As can be seen from the figure in the red phosphorus/graphene composite material prepared, red phosphorus is evenly affixed to the surface of graphene.
Referring to attached drawing 4, this figure is the high power of red phosphorus/graphene composite material and grapheme material manufactured in the present embodiment
TEM schemes, and in the red phosphorus/graphene composite material as can be seen from the figure prepared, red phosphorus is laminated structure.
Referring to attached drawing 5, this figure is that the circulation of red phosphorus/graphene composite material and red phosphor material manufactured in the present embodiment is bent
Line, the red phosphorus/graphene composite material as can be seen from the figure prepared show good cycle performance.Prepared red phosphorus/
Graphene composite material still keeps 1286mAh g under the electric current of 200mA/g, by 100 circulations-1Specific capacity, hence it is evident that it is high
In the specific capacity of red phosphor material.
Embodiment 2
1) purify red phosphorus: by commercial red phosphorus, ball milling 6h, revolving speed 300rpm are then lauched at 200 DEG C in deionized water
It is heat-treated 12h, vacuum drying after washing, the red phosphorus powder purified；
2) mixed dispersion liquid is prepared: by 10mg red phosphorus powder, 20mg graphene in 50mL ethyl alcohol/deionized water (volume ratio
Ultrasonic disperse 30min in mixed solution 1:3) obtains graphene-red phosphorus mixed dispersion liquid；
3) centrifugal treating: for several times by mixed dispersion liquid centrifugation, exchange solvent is deionized water, obtains pure mixture；
4) it is freeze-dried: step 3) mixture obtained being freezed at -80 DEG C, is lyophilized, is obtained by freeze drier
Red phosphorus/graphene composite material.
Embodiment 3
1) purify red phosphorus: by commercial red phosphorus, ball milling 6h, revolving speed 300rpm are then lauched at 200 DEG C in deionized water
It is heat-treated 12h, then vacuum drying after washing, the red phosphorus powder purified；
2) mixed dispersion liquid is prepared: by 60mg red phosphorus powder, 20mg graphene in 50mL ethyl alcohol/deionized water (volume ratio
Ultrasonic disperse 30min in mixed solution 1:3) obtains graphene-red phosphorus mixed dispersion liquid；
3) centrifugal treating: for several times by mixed dispersion liquid centrifugation, exchange solvent is deionized water, obtains pure mixture；
4) it is freeze-dried: step 3) mixture obtained being freezed at -80 DEG C, is lyophilized, is obtained by freeze drier
Red phosphorus/graphene composite material.
It finally, it should be noted that the above embodiment is merely an example for clearly illustrating the present invention, and is not pair
The restriction of embodiment.For the those of ordinary skill in the field, it can also be made on the basis of the above description
Its various forms of variation or variation.There is no necessity and possibility to exhaust all the enbodiments.And it thus extends out
Obvious changes or variations be still in the protection scope of this invention.
Claims (6)
1. a kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method, it is characterised in that: the method passes through low
Warm liquid phase method, red phosphorus and graphene is fully dispersed in a solvent, and surface electrical behavior is poor in a solvent by red phosphorus and graphene
It is different, make red phosphorus nanometer sheet uniform load on the surface of graphene, obtains uniform red phosphorus/graphene composite material.
2. a kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method as described in claim 1, feature exist
In the described method comprises the following steps:
1) red phosphorus is purified: by commercial red phosphorus ball milling in deionized water, the vacuum drying after hydro-thermal process 12h at 200 DEG C；
2) prepare mixed dispersion liquid: by after purification red phosphorus and graphene dispersion in ethyl alcohol/deionized water in the mixed solvent, surpass
Sound disperses 5~120min, obtains uniform mixed dispersion liquid；
3) centrifugal treating: by step 2) mixed dispersion liquid obtained by multiple centrifugal treating, exchange solvent is deionized water,
Obtain pure mixture；
4) be freeze-dried: by step 3) mixture obtained -80 DEG C freeze, be lyophilized by freeze drier, obtain red phosphorus/
Graphene composite material.
3. a kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method as claimed in claim 2, feature exist
In: mixed solvent described in the step 2) is the mixed solvent of alcohol-water, and wherein the volume ratio of ethyl alcohol and water is 1:5-1:1.
4. a kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method as claimed in claim 2, feature exist
In: concentration of the graphene in mixed dispersion liquid is 0.1~10g/L.
5. a kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method as described in claim 1,2 or 4,
Be characterized in that: the mass ratio of red phosphorus and graphene in mixed dispersion liquid is 1:2~4:1.
6. a kind of negative electrode of lithium ion battery red phosphorus/graphene composite material preparation method as claimed in claim 2, feature exist
In: red phosphorus is negative in the zeta current potential of in the mixed solvent, and graphene is positive in the zeta current potential of in the mixed solvent, to make two
Person occurs mutually to adsorb in the solution, forms stable composite construction.
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Cited By (4)
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| CN110212185A (en) * | 2019-06-04 | 2019-09-06 | 中国地质大学（北京） | A kind of Sn-P-CNT composite material and its purposes for preparing lithium ion battery negative material |
| CN113023713A (en) * | 2021-02-02 | 2021-06-25 | 厦门大学 | Preparation method of red phosphorus/graphene composite roll |
| CN116111223A (en) * | 2023-02-20 | 2023-05-12 | 东莞理工学院 | Method for preparing ternary composite material by recycling waste lithium battery negative electrode and application |
| CN117334849A (en) * | 2023-11-20 | 2024-01-02 | 浙江大学 | Red phosphorus anode, preparation method thereof and application thereof in lithium ion battery |
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