CN103198935B - The preparation method of a kind of graphene film modified spinelle type LiMn2O4 or α type manganese dioxide electrode - Google Patents
The preparation method of a kind of graphene film modified spinelle type LiMn2O4 or α type manganese dioxide electrode Download PDFInfo
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- CN103198935B CN103198935B CN201310136538.0A CN201310136538A CN103198935B CN 103198935 B CN103198935 B CN 103198935B CN 201310136538 A CN201310136538 A CN 201310136538A CN 103198935 B CN103198935 B CN 103198935B
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- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to the preparation method of a kind of graphene film modified spinelle type LiMn2O4 or α type manganese dioxide electrode, 80:15:5 takes containing manganese electrode material, conductive agent and PVDF adhesive powder in mass ratio, conductive agent is the mixture of graphene film or graphene film and acetylene black conductor, first each raw material is made into slurries, is then coated in aluminum foil current collector and nickel screen collector top roll is suppressed.Preparation technology of the present invention is comparatively easy, and the conductivity of the electrode obtained significantly improves, and rate capability significantly improves.
Description
Technical field
The present invention relates to a kind of improvement LiMn
2o
4with α-MnO
2the method of rate capability, is applied in anode material for lithium-ion batteries LiMn using graphene film as conductive additive
2o
4with electrochemical capacitor material α-MnO
2in electrode, improve above-mentioned material conductivity and rate capability, belong to lithium ion battery and electrochemical capacitor additive technology field.
Background technology
In recent years, along with the continuous consumption of fossil energy and the environmental pollution that brings day by day serious, research and development are effectively, the new forms of energy of environmental protection become the epoch problem of All Around The World.Not yet breaking away from the dependence of traditional energy, under background that the new energy is not yet used widely, energy storage becomes more and more important.How the existing energy stored effectively and discharge fast when needs to meet daily life demand, becoming the focus that obtains extensive concern.Lithium ion battery and electrochemical capacitor, because respective energy density is high, power density is high, obtain a large amount of concerns and application in energy storage system.But its main electrode material adopted is (as LiCoO
2and RuO
2) because the factor of the aspect such as cost, environmental protection limits, be difficult to widely use in Large Copacity energy storage system.Spinel-type LiMn
2o
4with α type MnO
2then there is the advantages such as capacity is high, cost is low, nontoxic, become the candidate material of anode material for lithium-ion batteries and electrochemical capacitor electrode material.But bi-material all exists the low shortcoming of electronic conductivity, result in its charge transfer process in big current situation comparatively slow, specific capacity is lower, and rate capability is poor.
Bi-material is carried out to the modification of conductivity, become major routes at present.Common way is as material with carbon element (comprising mesoporous carbon (mesoporouscarbon), carbon nano-tube (CNTs), Graphene (graphene) etc.), conducting metal etc. prepare composite material together with above-mentioned material by good for some conductivity material.The conductivity of the composite material of synthesis is more much better than pure electrode material, thus improves the low weakness of its electronic conductivity, improves its rate capability.But the method is complicated, wayward, and is difficult to realize suitability for industrialized production.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, and the preparation method of a kind of graphene film modified spinelle type LiMn2O4 or α type manganese dioxide electrode is provided, improve conductivity and the rate capability of bi-material.
The present invention is achieved by the following technical solutions:
A preparation method for graphene film modified spinelle type LiMn2O4 or α type manganese dioxide electrode, step is as follows:
(1) 80:15:5 takes manganese electrode material, conductive agent and Kynoar (PVDF) adhesive powder in mass ratio, and manganese electrode material is LiMn
2o
4or α-MnO
2, conductive agent is the mixture of graphene film or graphene film and acetylene black conductor, is dissolved in by PVDF adhesive powder in appropriate 1-METHYLPYRROLIDONE (NMP), forms the uniform solution that mass fraction is 0.77wt% ~ 0.94wt%;
(2) manganese electrode material and conductive agent are placed in absolute ethyl alcohol and form slurries, stir until ethanol vapors away completely, in the solution obtain the mixed-powder obtained immigration step (1), continue to stir 0.5-1 little of the uniform slurries of formation;
(3) slurries that step (2) obtains are coated on aluminum foil current collector or nickel screen collector, with roll squeezer pressure above-mentioned collector once after drying, make electrode material closely paste on a current collector, obtain LiMn
2o
4or α-MnO
2the modified electrode of material.
α-the MnO obtained
2the modified electrode of material can directly use, LiMn
2o
4electrode then needs to be assembled in button cell (CR2032) and goes, and its rate capability is by realizing the test of button cell.
Both the preferred 1-2:1 of mass ratio in graphene film described in above-mentioned steps (1) and the mixture of acetylene black conductor.
In aluminum foil current collector described in step (3), coating thickness is 150 ± 10 μm, and on nickel screen collector, (nickel screen is cut into 1cm × 2cm size, and the nickel screen specification of use is 60 orders), film area are 0.5 ± 0.1cm
2(the active material area namely each nickel screen is coated with is about 0.5cm
2, after film, nickel screen is covered by black active material completely).
Preferably be coated with containing LiMn in aluminum foil current collector in step (3)
2o
4slurries, nickel screen collector is coated with containing α-MnO
2slurries.
In order to better distinguish material of the present invention and unmodified material, according to the different quality mark of graphene film in the total material of each electrode, be LMO(not graphene-containing sheet respectively by electrode designations) and LMO-G(5wt%, 10wt% and 15wt%) and α-MnO
2(not graphene-containing sheet) and α-MnO
2-G(5wt%, 10wt% and 15wt%).
Because graphene film is a kind of high conductivity material with carbon element with layer structure, therefore it in the electrodes can by " face-point " conduction mode in conjunction with many LiMn
2o
4with α-MnO
2material granule (as Fig. 3).And acetylene black conductor is owing to being particulate material, therefore can only by " point-point " conduction mode in conjunction with above-mentioned electrode material granules.Clearly, " face-point " conduction mode is a kind of more effective conduction mode, and therefore the conductivity of above-mentioned electrode can be improved significantly.Stability during electrode material experience long circulating is also improved significantly by appropriate Graphene additive.
It should be noted that graphene film in conjunction with each electrode material granules, therefore always can not have some electrode materials and do not caused its performance to be difficult to be played by conductive agent connection.And when there being acetylene black conductor to exist in electrode, this part material can be combined by acetylene black particle.In addition, because the particle of acetylene black conductor combines with them in the space that can be filled into graphene film and electrode material, produce " filling " effect (as Fig. 3), therefore can there is a conductive network in whole electrode.Rely on the cooperative effect of " face-point " conduction mode and " filling " pattern, the conductivity of electrode is further enhanced.Therefore the rate capability of electrode material is significantly improved.
The realization of above-mentioned cooperative effect and the consumption of Graphene additive have direct relation.When Graphene is very few, " face-point " conduction mode in electrode is more weak; When Graphene is excessive, on the one hand, due to graphene planes structure, its Van der Waals force is comparatively large, and therefore Graphene sector-meeting produces clustering phenomena, and the efficiency in conjunction with electrode material reduces, and " face-point " conduction mode is died down; On the other hand, when not having acetylene black conductor in electrode, the synergy of " filling " pattern and two kinds of patterns has not existed, and the conductivity of electrode can be deteriorated, therefore LMO-G(15wt%) electrode capacity under high magnification is almost 0, and α-MnO
2-G(15wt%) ratio capacitance of electrode also has no than α-MnO
2exceed how many.
Compared with prior art, the present invention has the following advantages:
1. LMO and the α-MnO of not graphene-containing sheet
2the test result of electrode in fig. 1 and 2, can compare according to its result, and stability when finding out experience long circulating is improved significantly by appropriate Graphene additive.
As long as be added in electrode material by the graphene film of good dispersion in certain mass ratio, due to its distinctive planar structure and high conductivity, the conductivity of whole electrode can be improved significantly, and rate capability also can improve.
2. simple to operate, whole process, without complicated technology, is convenient to realize industrial applications, and the preparation technology of grapheme material is comparatively easy, can meet large-scale production needs.
Accompanying drawing explanation
Fig. 1 is the rate capability performance of Different L MO-G electrode, a: under the various multiplying power of 0.5-10C; Under b:20C multiplying power.
Fig. 2 is different α-MnO
2the rate capability performance of electrode;
Fig. 3 is the conduction schematic diagram of the electrode containing graphene conductive additive.
Embodiment
Further illustrate below in conjunction with embodiment.
Embodiment 1
(1) 80:15:5 takes LiMn in mass ratio
2o
4material, conductive agent and PVDF adhesive powder, conductive agent is graphene film, is dissolved in by PVDF adhesive powder in appropriate 1-METHYLPYRROLIDONE (NMP);
(2) by LiMn
2o
4material and conductive agent are placed in absolute ethyl alcohol and form slurries, stir until ethanol vapors away completely, now material again reverts to Powdered and mixes, and in the solution obtain, continues stirring 0.5 little of the uniform slurries of formation by the mixed-powder obtained immigration step (1);
(3) slurries that step (2) obtains are coated in (coating thickness is approximately 150 μm) in aluminum foil current collector, with roll squeezer pressure above-mentioned collector once after drying, make electrode material closely paste on a current collector, obtain LMO-G(15wt%) electrode.
Embodiment 2
Step is with embodiment 1, and difference is the mixture that the conductive agent used is graphene film and acetylene black, and quality proportioning is 10:5, obtains LMO-G(10wt%) electrode.
Embodiment 3
Step is with embodiment 1, and difference is the mixture that the conductive agent used is graphene film and acetylene black, and quality proportioning is 5:10, obtains LMO-G(5wt%) electrode.
Embodiment 4
(1) 80:15:5 takes α-MnO in mass ratio
2material, conductive agent and PVDF adhesive powder, conductive agent is graphene film, is dissolved in by PVDF adhesive powder in appropriate 1-METHYLPYRROLIDONE (NMP);
(2) by α-MnO
2material and conductive agent are placed in absolute ethyl alcohol and form slurries, stir until ethanol vapors away completely, now material again reverts to Powdered and mixes, and in the solution obtain, continues stirring 0.5 little of the uniform slurries of formation by the mixed-powder obtained immigration step (1);
(3) be coated on nickel screen collector by the slurries that step (2) obtains, nickel screen is cut into 1cm × 2cm size, and the nickel screen specification of use is 60 orders, and film area is 0.5 ± 0.1cm
2(the active material area namely each nickel screen is coated with is about 0.5cm
2, after film, nickel screen is covered by black active material completely), with roll squeezer pressure above-mentioned collector once after drying, make electrode material closely paste on a current collector, obtain α-MnO
2-G(15wt%) electrode.
Embodiment 5
Step is with embodiment 4, and difference is the mixture that the conductive agent used is graphene film and acetylene black, and quality proportioning is 10:5, obtains α-MnO
2-G(10wt%) electrode.
Embodiment 6
Step is with embodiment 4, and difference is the mixture that the conductive agent used is graphene film and acetylene black, and quality proportioning is 5:10, obtains α-MnO
2-G(5wt%) electrode.
Performance test
Test the rate capability that Graphene mass fraction in electrode is each electrode in 5wt%, 10wt% and 15wt% tri-kinds of situations in the present invention respectively, graphene film is by using hydrazine hydrate (N
2h
4h
2o) method of redox graphene (GrapheneOxide, GO) obtains.GO is then by adopting the Hummers method improved to prepare [Q.Cheng, J.Tang, J.Ma, H.Zhang, N.Shinya, L.C.Qin, GrapheneandnanostructuredMnO by graphite powder
2compositeelectrodesforsupercapacitors.Carbon, 2011,49,2917-2925].
The preparation process of graphene film is:
(1) take 0.05gGO powder, joined in 60mL ultra-pure water, then ultrasonic process 2h is carried out to it, make GO powder to be distributed in ultra-pure water equably, form GO dispersion liquid.
(2) in above-mentioned dispersion liquid, NH is dripped
3h
2o, uses magnetic stirring apparatus to stir it simultaneously, regulates the pH value of this dispersion liquid to approximate 10, continue to stir 0.5h.
(3) under constantly stirring, in dispersion liquid, 250 μ LN are slowly added dropwise to
2h
4h
2o(85wt%), be then placed in water-bath by dispersion liquid, setting heating-up temperature is 90 ° of C, after carrying out agitating heating 15h, stops heating, treats that it cools naturally, obtain the aqueous dispersions of graphene film it.
(4) use centrifuge, the grapheme material obtained is separated from liquid, and respectively cleans three times with ultra-pure water and absolute ethyl alcohol, be then placed on 80 ° of dry 12h of C in drying box.
The Different electrodes prepared containing above-described embodiment is designated as LMO-G(5wt%, 10wt%, 15wt% respectively) and α-MnO
2-G(5wt%, 10wt%, 15wt%).
(1) rate capability of various electrode is tested
The rate capability of LMO and various LMO-G electrode realizes by carrying out constant current charge-discharge test to the button cell (CR2032) of its assembling, being assembled in glove box of battery is carried out, LMO and LMO-G electrode is as anode, lithium sheet (purity is more than 99.9%) as battery cathode, 1molL
-1liPF
6solution [ethylenecarbonate(EC of solvent to be volume ratio be 1:1) and dimethylcarbonate(DMC)] be electrolyte.Charge-discharge test uses Land charge-discharge test instrument to realize, and charge and discharge potential interval is 3.5-4.3V(vs.Li/Li
+), charge-discharge magnification is respectively 0.5,2,5,10 and 20C(1C=148mAg
-1).α-MnO
2with various α-MnO
2the rate capability of-G electrode is undertaken by carrying out constant current charge-discharge test to its three-electrode system as work electrode, Pt sheet (1 × 2cm) as to electrode, saturated calomel electrode (SCE) as reference electrode, 0.5molL
-1na
2sO
4the aqueous solution is as electrolyte.Charge-discharge test uses CHI760C electrochemical workstation to realize, and charge and discharge potential interval is-0.2-0.8V(vs.SCE), charging and discharging currents density is 1000mAg
-1.
(2) the rate capability performance of various electrode
When containing appropriate graphene conductive additive, the rate capability of bi-material has had obvious lifting.With LiMn
2o
4, be example (as shown in Figure 1), LMO-G(5wt%) specific discharge capacity of electrode under the various multiplying power of 0.5-20C be all far away higher than LMO electrode.Especially under the large multiplying power of 10C and 20C, LMO-G(5wt%) the initial discharge specific capacity of electrode is respectively 88 and 78mAhg
-1, far away higher than 70 and 60mAhg of LMO electrode
-1.Again with α-MnO
2material is example (as Fig. 2), α-MnO
2-G(10wt%) electrode is at 1000mAg
-1through 1000 charge and discharge cycles under current density, its electric discharge ratio capacitance maintains 80Fg all the time
-1above, α-MnO is better than far away
2electrode.Stability during this bi-material experience long circulating is also improved significantly by appropriate Graphene additive.
The rate capability of bi-material is significantly improved, and is caused by above-mentioned " synergy that graphene film ' face-point ' conduction mode produces with ' filling ' pattern of AB particle ".First, graphene film is by the higher face-point of electrical efficiency " conduction mode improves the conductivity of electrode; Secondly, AB particle relies on its " filling " pattern, is connected to those not by the isolated electrode material granules that graphene film combines, the material in whole electrode is combined, forms an effective conductive network, further increase the conductivity of electrode.Given this, bi-material rate capability be improved significantly.
Claims (3)
1. a preparation method for graphene film modified spinelle type LiMn2O4 or α type manganese dioxide electrode, is characterized in that, comprise step as follows:
(1) 80:15:5 takes manganese electrode material, conductive agent and Kynoar PVDF adhesive powder in mass ratio, and manganese electrode material is LiMn
2o
4or α-MnO
2, conductive agent is the mixture of graphene film and acetylene black conductor, is dissolved in by PVDF adhesive powder in appropriate 1-METHYLPYRROLIDONE, forms the uniform solution that mass fraction is 0.77wt% ~ 0.94wt%; Described conductive agent, when manganese electrode material is LiMn
2o
4time, the quality proportioning of graphene film and acetylene black is 5:10, when manganese electrode material is α-MnO
2time, the quality proportioning of graphene film and acetylene black is 10:5;
(2) manganese electrode material and conductive agent are placed in absolute ethyl alcohol and form slurries, stir until ethanol vapors away completely, in the solution obtain the mixed-powder obtained immigration step (1), continue to stir 0.5-1 little of the uniform slurries of formation;
(3) slurries that step (2) obtains are coated on aluminum foil current collector or nickel screen collector, with roll squeezer pressure above-mentioned collector once after drying, make electrode material closely paste on a current collector, obtain LiMn
2o
4or α-MnO
2the modified electrode of material.
2. the preparation method of a kind of graphene film modified spinelle type LiMn2O4 according to claim 1 or α type manganese dioxide electrode, it is characterized in that, in aluminum foil current collector described in step (3), coating thickness is 150 ± 10 μm, on nickel screen collector, nickel screen is cut into 1cm × 2cm size, and film area is 0.5 ± 0.1cm
2.
3. the preparation method of a kind of graphene film modified spinelle type LiMn2O4 according to claim 1 or α type manganese dioxide electrode, is characterized in that, is coated with containing LiMn in step (3) in aluminum foil current collector
2o
4slurries, nickel screen collector is coated with containing α-MnO
2slurries.
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| CN103730655A (en) * | 2014-01-21 | 2014-04-16 | 中国计量学院 | Preparation method of LiMn2O4-graphene composite positive electrode material |
| WO2016005590A1 (en) * | 2014-07-10 | 2016-01-14 | Repsol, S.A. | Cathode for lithium batteries |
| WO2016092263A1 (en) * | 2014-12-11 | 2016-06-16 | The University Of Liverpool | Electrode composition |
| CN110474099A (en) * | 2019-07-12 | 2019-11-19 | 大连恒超锂业科技有限公司 | A kind of preparation method of lithium ion battery anode glue size |
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