CN105609736A - Preparation method for three-dimensional carbon nanotube/nitrogen-doped graphene/sulfur electrode slice - Google Patents
Preparation method for three-dimensional carbon nanotube/nitrogen-doped graphene/sulfur electrode slice Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention provides a preparation method for a three-dimensional carbon nanotube/nitrogen-doped graphene/sulfur electrode slice. The preparation method comprises the following steps of (1) adding the carbon nanotube, graphite oxide and polyacrylonitrile to N-methyl pyrrolidone, performing an ultrasonic reaction, coating an aluminium foil with mixed paste, and performing vacuum drying to obtain the electrode slice; (2) putting the obtained electrode slice into a muffle furnace under ammonia gas protection, heating to 400-500 DEG C, and naturally cooling; and (3) enabling the electrode slice obtained in the step (2) to be fully inserted into a Na2S2O3 solution, and slowly adding hydrochloric acid to the solution in a dropwise manner until the PH value of the solution reaches 6.5-7.5, taking out the electrode slice, and drying the electrode slice to obtain a positive plate. The electrode slice prepared by the invention can be directly used for the positive electrode of a lithium-sulfur battery without requiring a conductive agent and a binder, so that the cost of the electrode is greatly lowered.
Description
Technical field
The present invention relates to nano material synthetic, particularly a kind of preparation method of lithium sulfur battery anode material.
Background technology
Lithium-sulfur cell is taking lithium metal as negative pole, and elemental sulfur is anodal battery system. The thering are two and put of lithium-sulfur cellLevel platform (being about 2.4V and 2.1V), but its electrochemical reaction mechanism more complicated. It is high that lithium-sulfur cell has specific energy(2600Wh/kg), specific capacity high (1675mAh/g), low cost and other advantages, be considered to very promising a new generation's electricityPond. But there is at present that active material utilization is low, cycle life is low and the problem such as poor stability, this is seriously restricting lithiumThe development of sulphur battery. Cause the main cause of the problems referred to above to have the following aspects: (1) elemental sulfur is electronics and ion insulationBody, room-temperature conductivity is low by (5 × 10-30S·cm-1), owing to there is no the sulphur of ionic state, thus tired as positive electrode activationDifficult; (2) poly-many lithium sulfides of the state Li of height producing in electrode process2Sn(8 > n >=4) are soluble in electrolyte, positive and negativeBetween the utmost point, form concentration difference, under the effect of concentration gradient, move to negative pole, the high poly-many lithium sulfides of state are reduced into low by lithium metalThe poly-many lithium sulfides of state. Along with the carrying out of above reaction, the many lithium sulfides of oligomeric state are assembled at negative pole, finally between two electrodes, formConcentration difference, moves to again positive pole and is oxidized to the high poly-many lithium sulfides of state. This phenomenon is called as and flies shuttle effect, has reduced sulphur activityThe utilization rate of material. Insoluble Li simultaneously2S and Li2S2Be deposited on cathode of lithium surface, further worsened lithium-sulfur cellPerformance; (3) reaction end product Li2S is electronic body equally, can be deposited on sulfur electrode, and lithium ion is in solid-state sulfurationIn lithium, migration velocity is slow, makes electrochemical reaction dynamics speed slack-off; (4) sulphur and end product Li2The density difference of S, works as sulphurAbout 79% by volumetric expansion after lithiumation, easily cause Li2The efflorescence of S, causes the safety problem of lithium-sulfur cell. Above-mentioned not enough restrictionThe development of lithium-sulfur cell, this is also that current lithium-sulfur cell research needs the Important Problems solving.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of three-dimensional structure lithium sulfur battery anode material, simultaneously directly preparationBecome the method for lithium-sulphur cell positive electrode sheet, the method is prepared three-dimensional material with carbon element and is also comprised sulphur nano particle, CNT, partFormer nitrogen-doped graphene, nano-sulfur particles is deposited on the three dimensions surface of CNT and nitrogen-doped graphene formation, shouldDesign can improve the electric conductivity of sulphur, and can stop the dissolving of discharging product polysulfide.
The preparation technology's flow process that the invention provides a kind of three dimensional carbon nanotubes/nitrogen-doped graphene/sulfur electrode sheet is as follows:
(1) CNT, graphite oxide and polyacrylonitrile are joined to 1-METHYLPYRROLIDONE, ultrasonic reaction after stirring30-120 minute, then mixed slurry is coated on aluminium foil, and vacuum drying obtains electrode slice.
(2) electrode slice obtaining is put into the Muffle furnace of protection of ammonia, be slowly warmed up to the speed of 3-5 DEG C/min400-500 DEG C, reaction 0.5-5 hour, naturally cooling.
(3) electrode slice (2) being obtained inserts the Na of 0.5-2mol/L completely2S2O3In solution, static 30-60 minute,Then to the hydrochloric acid that drips slowly 1mol/L in solution, until solution PH=6.5-7.5 takes out electrode slice, just obtain after dryPole piece.
In step (1), the mass ratio of CNT, Graphene and polyacrylonitrile is 1:1.6-2.4:0.8-1.2, ultrasonic anti-Between seasonable, be 30-120 minute, the diameter of CNT is 20-100nm, and length is 1-20um;
In step (2) reaction, to pass into gas be ammonia in reaction, and the programming rate of Muffle furnace is 3-5 DEG C/min; Reaction temperature is400-500 DEG C; Reaction time 0.5-5 hour; React rear naturally cooling.
Na in step (3)2S2O3The concentration of solution is 0.5-2mol/L; Electrode slice inserts Na2S2O3Solution is quiescent time30-60 minute; The addition of hydrochloric acid just makes the PH=6.5-7.5 of solution.
The present invention adopts above technical scheme, and its advantage is, graphite oxide is at high temperature reduced to Graphene, nitrogen dopingTime go back residual fraction oxygen atom on Graphene, the existence of this part oxygen atom on the one hand can be in charge and discharge process and lithiumIonic reaction provides energy, and oxygen atom can attract the movement of polysulfide on the other hand, reduces and flies shuttle effect.
The present invention has following beneficial effect: (1) this preparation method is by graphite oxide reduction, nitrogen doping and polyacrylonitrileAnnulation one step completes, and improves reaction efficiency; (2) polyacrylonitrile at Graphene between layers and Graphene and carbon nanometerBetween pipe, there is annulation and crosslinked together, make the CNT of one dimension and two-dimentional Graphene form a three-dimensional spaceBetween, then by in-situ reducing, sulphur is stored in this three dimensions; (3) CNT of high conductivity and grapheme material energyEffectively improve the electrical conductivity of electrode slice; (4), in charge and discharge process, being configured with of three-dimensional structure is beneficial to lithium ion and electronics manyIn dimension conducting path, shuttle back and forth, improve ion and electron conductivity; (5) for the nitrogen-doped graphene of fully reduction contains part nitrogenAtom and oxygen atom, have suction-operated to sulphur, can effectively reduce and fly shuttle effect, improves the cycle life of lithium-sulfur cell; (6) thisThe electrode slice of bright preparation can be directly used in the positive pole of lithium-sulfur cell, does not need to add conductive agent and binding agent again, greatly reducesThe cost of electrode.
Brief description of the drawings
Fig. 1 is the SEM figure of three dimensional carbon nanotubes/nitrogen-doped graphene/sulfur electrode sheet of preparing of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, preferably embodiment of the present invention is described in further detail:
Embodiment 1
(1) be that 20nm length is the N-first that 1um CNT, 1g graphite oxide, 1g polyacrylonitrile join 100mL by 1g diameterBase pyrrolidones, ultrasonic reaction 30 minutes after stirring, then mixed slurry is coated on aluminium foil, and vacuum drying obtains electrodeSheet.
(2) electrode slice obtaining is put into the Muffle furnace of protection of ammonia, be slowly warmed up to 400 with the speed of 3 DEG C/minDEG C, react 5 hours, naturally cooling.
(3) electrode slice (2) being obtained inserts the Na of 2mol/L completely2S2O3In solution, static 30 minutes, then to moltenIn liquid, drip slowly the hydrochloric acid of 1mol/L, until electrode slice is taken out in solution PH=7.5, after being dried, obtain positive plate.
Embodiment 2
(1) be that 100nm length is that 20um CNT, 0.8g graphite oxide, 1.2g polyacrylonitrile join 100mL by 1g diameter1-METHYLPYRROLIDONE, ultrasonic reaction 120 minutes after stirring, then mixed slurry is coated on aluminium foil, vacuum dryingObtain electrode slice.
(2) electrode slice obtaining is put into the Muffle furnace of inert gas shielding, be slowly warmed up to the speed of 5 DEG C/min500 DEG C, react 0.5 hour, naturally cooling.
(3) electrode slice (2) being obtained inserts the Na of 0.5mol/L completely2S2O3In solution, static 60 minutes, then toIn solution, drip slowly the hydrochloric acid of 1mol/L, until electrode slice is taken out in solution PH=6.5, after being dried, obtain positive plate.
Embodiment 3
(1) be that 30nm length is that 10um CNT, 1.2g graphite oxide, 0.8g polyacrylonitrile join 100mL by 1g diameter1-METHYLPYRROLIDONE, ultrasonic reaction 60 minutes after stirring, then mixed slurry is coated on aluminium foil, vacuum drying obtainsTo electrode slice.
(2) electrode slice obtaining is put into the Muffle furnace of protection of ammonia, be slowly warmed up to 450 with the speed of 4 DEG C/minDEG C, react 1 hour, naturally cooling.
(3) electrode slice (2) being obtained inserts the Na of 1mol/L completely2S2O3In solution, static 50 minutes, then to moltenIn liquid, drip slowly the hydrochloric acid of 1mol/L, until electrode slice is taken out in solution PH=7, after being dried, obtain positive plate.
Embodiment 4
(1) be that 50nm length is that 5um CNT, 0.9g graphite oxide, 1.1g polyacrylonitrile join 100mL by 1g diameter1-METHYLPYRROLIDONE, ultrasonic reaction 90 minutes after stirring, then mixed slurry is coated on aluminium foil, vacuum drying obtainsTo electrode slice.
(2) electrode slice obtaining is put into the Muffle furnace of protection of ammonia, be slowly warmed up to the speed of 3.5 DEG C/min420 DEG C, react 2 hours, naturally cooling.
(3) electrode slice (2) being obtained inserts the Na of 1.5mol/L completely2S2O3In solution, static 40 minutes, then toIn solution, drip slowly the hydrochloric acid of 1mol/L, until electrode slice is taken out in solution PH=7.3, after being dried, obtain positive plate.
Embodiment 5
(1) be that 70nm length is that 15um CNT, 1.1g graphite oxide, 0.9g polyacrylonitrile join 100mL by 1g diameter1-METHYLPYRROLIDONE, ultrasonic reaction 100 minutes after stirring, then mixed slurry is coated on aluminium foil, vacuum dryingObtain electrode slice.
(2) electrode slice obtaining is put into the Muffle furnace of protection of ammonia, be slowly warmed up to the speed of 4.5 DEG C/min470 DEG C, react 3 hours, naturally cooling.
(3) electrode slice (2) being obtained inserts the Na of 1.2mol/L completely2S2O3In solution, static 35 minutes, then toIn solution, drip slowly the hydrochloric acid of 1mol/L, until electrode slice is taken out in solution PH=6.7, after being dried, obtain positive plate.
The preparation and property test of electrode; Using the electrode slice of preparation as positive pole, metal lithium sheet is to electrode, CELGARD2400 is barrier film, and the LiTFSI/DOL-DME (volume ratio 1:1) of 1mol/L is electrolyte, and the LiNO3 of 1mol/L is additive,Be full of in Ar glove box and be assembled into button cell, adopt Land battery test system to carry out constant current charge-discharge test. Discharge and recharge electricityPressure scope is 1-3V, and current density is 1C, and performance is as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Specific discharge capacity after circulation first | 960mAh/g | 990mAh/g | 940mAh/g | 980mAh/g | 960mAh/g |
| Specific discharge capacity after 100 circulations | 650mAh/g | 720mAh/g | 690mAh/g | 700mAh/g | 660mAh/g |
Fig. 1 is the SEM figure that the present invention prepares positive electrode, as can be seen from the figure this positive electrode toolStandby a large amount of open three-dimensional cavernous structure, can be good at providing ion transfer passage, improves the chemical property of material.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assertSpecific embodiment of the invention is confined to these explanations. For general technical staff of the technical field of the invention,Do not depart under the prerequisite of the present invention's design, can also make some simple deduction or replace, all should be considered as belonging to of the present inventionProtection domain.
Claims (5)
1. a preparation method for three dimensional carbon nanotubes/nitrogen-doped graphene/sulfur electrode sheet, is characterized in that, comprises following severalIndividual step:
Step (1): CNT, graphite oxide and polyacrylonitrile are joined to 1-METHYLPYRROLIDONE, ultrasonic after stirringReaction 30-120 minute, then mixed slurry is coated on aluminium foil, and vacuum drying obtains electrode slice;
Step (2): the electrode slice obtaining is put into the Muffle furnace of protection of ammonia, be slowly warmed up to the speed of 3-5 DEG C/min400-500 DEG C, reaction 0.5-5 hour, naturally cooling;
Step (3): the electrode slice that step (2) is obtained inserts Na completely2S2O3In solution, static 30-60 minute, then to moltenIn liquid, drip slowly hydrochloric acid, until solution PH=6.5-7.5 takes out electrode slice, after being dried, obtain positive plate.
2. the method for claim 1, is characterized in that, CNT, Graphene and polyacrylonitrile in described step (1)Mass ratio be 1:1.6-2.4:0.8-1.2, the diameter of CNT is 20-100nm, length is 1-20um.
3. the method for claim 1, is characterized in that, described step (2) reaction temperature is 400-500 DEG C.
4. the method for claim 1, is characterized in that, described Na2S2O3The concentration of solution is 0.5-2mol/L.
5. the method for claim 1, is characterized in that, in described step (3), the concentration of hydrochloric acid is 1mol/L.
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| CN106158421A (en) * | 2016-08-16 | 2016-11-23 | 肖丽芳 | A kind of preparation method of pre-lithium intercalated graphite alkene positive plate |
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