CN106450190A - Method for high-current density fast filling of microporous sulfur in lithium-sulfur battery - Google Patents
Method for high-current density fast filling of microporous sulfur in lithium-sulfur battery Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a method for high-current density fast filling of microporous sulfur in the lithium-sulfur battery. The method comprises the following steps of adding a microporous control material and elemental sulfur to carbon disulfide and carrying out uniform ultrasonic mixing to obtain a mixed material; drying the mixed material, evaporating the carbon disulfide and then obtaining a carbon-sulfur mixture of the microporous control material and the elemental sulfur; and preparing the battery by using the carbon-sulfur mixture, charging and discharging the battery for a certain number of turns at high current density and changing annular elemental sulfur into sulfur in a short-chain state to enter pores of the microporous control material. The method provided by the invention is simple in operation; the lithium-sulfur battery can be fast prepared; the cycling stability of the battery is more effectively improved after the lithium-sulfur battery is charged and discharged at relatively high current density; and the lithium-sulfur battery is closer to industrial application.
Description
Technical field
The invention belongs to lithium-sulfur cell technical field, be specifically related to high current density Fast Filling in a kind of lithium-sulfur cell micro-
The method of hole sulphur.
Background technology
The development of lithium battery receives more and more attention, and the capacity improving lithium battery is the key of high-end electronic product.
Lithium-sulfur cell is the one of lithium ion battery, and it is the positive electrode using element sulphur as lithium battery.Lithium-sulfur cell can obtain
Substantial amounts of research, because it has higher specific capacity (1673mAh/g) and specific energy (2600Whkg-1), it is lithium ion battery
5～10 times of capacity.In nature, element sulphur is very abundant, and the positive electrode as battery is environmentally friendly.But, lithium
Sulphur battery also faces a lot of technical barriers.First, the electric conductivity of elemental sulfur own is excessively poor, hinders the transmission of electronics, to electricity
The performance in pond produces impact；Second, elemental sulfur is in charge and discharge process, and positive electrode elemental sulfur can be from initial ring-type S8Become
The Li of solid-state short chain2S2And Li2S, it may occur that volumetric expansion, expansion rate reaches 80%；3rd, in battery charge and discharge process, in
Between product polysulfide can dissolve in the electrolytic solution, when polysulfide reaches negative pole, and lithium piece generation side reaction, and producing
" effect of shuttling back and forth " so that circulating battery stability reduces.
So far, it in order to solve three above problem, in prepared by the positive electrode of lithium-sulfur cell, is all to pass through simple substance
Sulphur preferably controls material and is combined with electric conductivity.In compound technique, elemental sulfur passes through chemical deposition and high-temperature process
When capillary absorption be combined, be finally reached control polysulfide diffusion.This combination process is too complicated, not only needs high temperature
Fill out sulphur, in addition it is also necessary to do surface treatment so that the cycle making battery is oversize.Meanwhile, when studying the electrical property of lithium-sulfur cell, test
During cycle life, the specific capacity of battery can gradually decay.Due to the decay of specific capacity, result in the unstability of battery, being difficult to should
It is used in reality industry.Therefore preparation method with low cost, that technique is simple, manufacturing cycle is short is found further, to lithium sulphur electricity
The application in pond has important actual application value.
Content of the invention
The present invention is directed to the deficiencies in the prior art, it is therefore intended that provide high current density in a kind of lithium-sulfur cell fast
Speed fills the method for micropore sulphur.
For achieving the above object, the technical solution adopted in the present invention is：
In a kind of lithium-sulfur cell, the method for high current density Fast Filling micropore sulphur, comprises the steps：
(1) by micropore control material and elemental sulfur join in carbon disulfide, ultrasonic mix after obtain mix material；
(2) the mixing material of step (1) gained is dried, after carbon disulfide evaporation, obtain micropore control material and elemental sulfur
Carbon sulphur mixture；
(3) step (2) gained carbon-sulfur compound is fabricated to positive level electrode slice, is prepared as battery again, then utilize high electricity
Current density carries out different number of turns discharge and recharge to battery, and the sulphur that ring-type elemental sulfur becomes short chain state is filled into micropore control material
In the duct of material.
In such scheme, described micropore control material is the micro-pore carbon material being formed after ZIF-8 carbonization.
In such scheme, the mass ratio of described micropore control material and elemental sulfur is 85:15.
In such scheme, the described ultrasonic power of step (1) is 99kHz, and ultrasonic time is 30min.
In such scheme, the temperature of the described drying of step (2) is 60 DEG C, and the time is 20～24h.
In such scheme, the preparation of the described battery of step (3) needs anode electrode piece, lithium piece and barrier film, and electrolyte is
LiNO3.
In such scheme, the described high current density of step (3) is the current density of 2C～5C.
In such scheme, the number of turns of the described discharge and recharge of step (3) is 10～50 circles.
The principle of the present invention is：By micropore control material and elemental sulfur physical mixed in carbon disulfide, steam in 60 DEG C
Send out carbon disulfide, obtain elemental sulfur and control the mixed uniformly carbon-sulfur compound of material with micropore；Carbon sulphur mixture is fabricated to positive pole
Electrode slice, with anode electrode piece, lithium piece and barrier film, electrolyte is LiNO3It is prepared as battery, to electricity under higher current density
Pond carries out the discharge and recharge of a fixing turn, and the purpose of do so is the sulphur making elemental sulfur become chain rupture state, is finally filled in a subtle way
In the duct of Porous materials, reach to limit the diffusion of polysulfide, strengthened the cyclical stability of battery.
Beneficial effects of the present invention：The present invention uses the method for high current density repeated charge to be filled into elemental sulfur micro-
In the duct of hole control material, in preparation cell process, do not use high-temperature process, fill out the side of sulphur with chemical deposition and steam
Method is compared, and decreases the absorption process of amount of heat in course of reaction, reduces energy ezpenditure；And the method for the invention simply holds
Easily operation, it is possible to achieve quickly prepare lithium-sulfur cell, and lithium-sulfur cell is after higher current density discharge and recharge, following of battery
Ring stability has obtained significantly more efficient improvement so that lithium-sulfur cell is closer to the application of industry.
Brief description
Fig. 1 is Sulfur in the embodiment of the present invention 1, micro-pore carbon material MC, the wide-angle diffraction XRD of carbon-sulfur compound (MC/S)
Figure.
Fig. 2 is that in the embodiment of the present invention 2, ZIF-8 low power (a) high power (b) and micro-pore carbon material MC low power (c) high power (d) are swept
Retouch Electronic Speculum figure.
Fig. 3 is micro-pore carbon material MC (a) nitrogen adsorption curve in the embodiment of the present invention 3, (b) micropore size distribution map.
Fig. 4 is the cycle performance figure preparing battery in the embodiment of the present invention 4.
Fig. 5 is the charge and discharge electrograph preparing battery in the embodiment of the present invention 4.
Detailed description of the invention
It in order to be more fully understood that the present invention, is further elucidated with present disclosure below in conjunction with embodiment, but the present invention
Content is not limited solely to the following examples.
In following example, as no specific instructions, described reagent is commercially available chemical reagent.
Described positive electrode is made up of micro-pore carbon material MC (Microporous) and elemental sulfur：By elemental sulfur and microporous carbon
Material MC dispersion with carbon disulfide in, at 60 DEG C be vacuum dried 24h obtain micropore control material mix with the carbon sulphur of elemental sulfur
Thing；This carbon sulphur mixture is cathode material.
The synthesis step of described micro-pore carbon material MC includes：Zinc nitrate hexahydrate is dissolved in methyl alcohol, simultaneously by 2-methyl
Imidazoles is dissolved in methyl alcohol, after stirring 30min, by molten for the methyl alcohol that the methanol solution dissolved with 2-methylimidazole pours zinc nitrate hexahydrate into
In liquid, continuing stirring 5h, suction filtration is simultaneously dried, and obtains ZIF-8；The carbonization in tube furnace by ZIF-8, is raised to 800 DEG C from room temperature, and 5
DEG C/programming rate of min, it is incubated 3h, after cooling, obtain micro-pore carbon material MC；Described zinc nitrate hexahydrate：The matter of 2-methylimidazole
Amount ratio is 4：9.
Embodiment 1
In a kind of lithium-sulfur cell, the method for high current density Fast Filling micropore sulphur, comprises the steps：
(1) synthesis of micro-pore carbon material MC：It is dissolved in 1.2g zinc nitrate hexahydrate in the methyl alcohol of 80mL, simultaneously by 2.7g2-
Methylimidazole is dissolved in the methyl alcohol of 80mL, after stirring 30min, the methanol solution dissolved with 2-methylimidazole is poured six water nitric acid into
In the methanol solution of zinc, stirring 5h, suction filtration is simultaneously dried, and obtains ZIF-8；By ZIF-8, carbonization in tube furnace, is raised to from room temperature
800 DEG C, the programming rate of 5 DEG C/min, it is incubated 3h, after cooling, obtain micro-pore carbon material MC；
(2) it is 85 in mass ratio by micro-pore carbon material MC and elemental sulfur:The ratio of 15 joins in carbon disulfide, ultrasonic work(
Rate 99kHz, time 30min, after mixing, obtain mixing material；
(3) it is placed in step (2) gained mixing material at 60 DEG C vacuum drying 24h, after carbon disulfide evaporation, obtain micropore
Control material MC and the carbon sulphur mixture of elemental sulfur；
(4) by step (3) gained carbon sulphur mixture according to mass ratio PVDF：Conductive carbon：Carbon sulphur mixture=10：15：75
Ratio mixing be fabricated to anode electrode piece, further with lithium piece, barrier film, electrolyte LiNO3Composition battery, at high current density
The 30th, the 10th, lower 2C discharge and recharge 50 enclose respectively, makes ring-type elemental sulfur become the sulphur of short chain state the hole entering micropore control material MC
In road.
Fig. 1 is that the present embodiment prepares Sulfur, micro-pore carbon material MC, the XRD of carbon-sulfur compound (MC/S).Permissible by figure
Find out that Sulfur has a lot of characteristic peak, be because that sublimed sulfur has three kinds of crystal formations, demonstrate a lot of characteristic peak.And ZIF-8 carbonization
After the micro-pore carbon material MC that obtains be two bulges of an agraphitic carbon, micro-pore carbon material MC is dissolved in two sulphur with elemental sulfur
Change in carbon, after being dried, measure the XRD of carbon sulphur mixture (MC/S), figure shows, the feature containing sulphur in carbon sulphur mixture
Peak.
Embodiment 2
In a kind of lithium-sulfur cell, the method for high current density Fast Filling micropore sulphur, comprises the steps：
(1) synthesis of micro-pore carbon material MC：It is dissolved in 2.4g zinc nitrate hexahydrate in the methyl alcohol of 80mL, simultaneously by 5.4g
2-methylimidazole is dissolved in the methyl alcohol of 80mL, after stirring 30min, the methanol solution dissolved with 2-methylimidazole is poured six water nitre into
In the methanol solution of acid zinc, stirring 5h, suction filtration is simultaneously dried, and obtains ZIF-8；By ZIF-8, carbonization in tube furnace, is raised to from room temperature
800 DEG C, the programming rate of 5 DEG C/min, it is incubated 3h, after cooling, obtain micro-pore carbon material MC；
(2) it is 85 in mass ratio by micro-pore carbon material MC and elemental sulfur:The ratio of 15 joins in carbon disulfide, ultrasonic work(
Rate 99kHz, time 30min, after mixing, obtain mixing material；
(3) it is placed in step (2) gained mixing material at 60 DEG C vacuum drying 24h, after carbon disulfide evaporation, obtain micropore
Control material MC and the carbon sulphur mixture of elemental sulfur；
(4) by step (3) gained carbon sulphur mixture according to mass ratio PVDF：Conductive carbon：Carbon sulphur mixture=10：15：75
Ratio mixing be fabricated to anode electrode piece, further with lithium piece, barrier film, electrolyte LiNO3Composition battery, at high current density
Under 2C, carry out discharge and recharge respectively to battery and the 10th, the 30th, 50 enclose, make ring-type elemental sulfur become the sulphur of short chain state and enter micropore control
In the duct of prepared material MC.
Fig. 2 (a) and (b) are the scanning electron microscope (SEM) photograph that the present embodiment prepares ZIF-8, as can be seen from the figure：ZIF-8 is at methyl alcohol
Under system highly uniform；Fig. 2 (c) and (d) are the scanning electron microscope (SEM) photograph that the present embodiment prepares micro-pore carbon material MC, can from figure
Going out, micro-pore carbon material MC is the structure of a kind of hexagonal prism, its a size of 100nm.
Embodiment 3
In a kind of lithium-sulfur cell, the method for high current density Fast Filling micropore sulphur, comprises the steps：
(1) synthesis of micro-pore carbon material MC：It is dissolved in 3.6g zinc nitrate hexahydrate in the methyl alcohol of 80mL, simultaneously by 8.1g
2-methylimidazole is dissolved in the methyl alcohol of 80mL, after stirring 30min, the methanol solution dissolved with 2-methylimidazole is poured six water nitre into
In the methanol solution of acid zinc, stirring 5h, suction filtration is simultaneously dried, and obtains ZIF-8；By ZIF-8, carbonization in tube furnace, is raised to from room temperature
800 DEG C, the programming rate of 5 DEG C/min, it is incubated 3h, after cooling, obtain micro-pore carbon material MC；
(2) it is 85 in mass ratio by micro-pore carbon material MC and elemental sulfur:The ratio of 15 joins in carbon disulfide, ultrasonic work(
Rate 99kHz, time 30min, after mixing, obtain mixing material；
(3) it is placed in step (2) gained mixing raw material at 60 DEG C vacuum drying 24h, after carbon disulfide evaporation, obtain micropore
Control material MC and the carbon sulphur mixture of elemental sulfur；
(4) by step (3) gained carbon sulphur mixture according to mass ratio PVDF：Conductive carbon：Carbon sulphur mixture=10：15：75
Ratio mixing be fabricated to anode electrode piece, further with lithium piece, barrier film, electrolyte LiNO3Composition battery, at high current density
Under 2C, respectively the 30th, the 10th, battery charging and discharging 50 is enclosed, make ring-type elemental sulfur become the sulphur of short chain state and enter micropore control material
In the duct of material MC.
Fig. 3 (a) is the nitrogen adsorption isotherm that the present embodiment prepares micro-pore carbon material MC, and in figure, shape is divided according to IUPAC
Class is I type, and micro-pore carbon material MC adsorption isothermal curve exists very big absorption when relative pressure is less than 0.02, and microporous carbon is described
There is substantial amounts of micropore canals structure in material ZIF-8, nearly levelling bench subsequently shows, micropore fills with, almost without
Further absorption occurs；Fig. 3 (b) is the micropore size distribution map that the present embodiment prepares micro-pore carbon material MC.In conjunction with Fig. 3 (a)
(b) understanding that the micropore size of micro-pore carbon material MC is concentrated mainly on about 0.6nm, micropore specific area reaches 2564m2/g.
Embodiment 4
In a kind of lithium-sulfur cell, the method for high current density Fast Filling micropore sulphur, comprises the steps：
(1) synthesis of micro-pore carbon material MC：It is dissolved in 4.8g zinc nitrate hexahydrate in the methyl alcohol of 80mL, will simultaneously
10.8g2-methylimidazole is dissolved in the methyl alcohol of 80mL, after stirring 30min, pours the methanol solution dissolved with 2-methylimidazole into
In the methanol solution of zinc nitrate hexahydrate, stirring 5h, suction filtration is simultaneously dried, and obtains ZIF-8；The carbonization in tube furnace by ZIF-8, from room
Temperature rise to 800 DEG C, the programming rate of 5 DEG C/min, it is incubated 3h, after cooling, obtain micro-pore carbon material MC；
(2) it is 85 in mass ratio by micro-pore carbon material MC and elemental sulfur:The ratio of 15 joins in carbon disulfide, ultrasonic work(
Rate 99kHz, time 30min, after mixing, obtain mixing material；
(3) it is placed in step (2) gained mixing raw material at 60 DEG C vacuum drying 24h, after carbon disulfide evaporation, obtain micropore
Control material MC and the carbon sulphur mixture of elemental sulfur；
(4) by step (3) gained carbon sulphur mixture according to mass ratio PVDF：Conductive carbon：Carbon sulphur mixture=10：15：75
Ratio mixing be fabricated to anode electrode piece, further with lithium piece, barrier film, electrolyte LiNO3Composition battery, at high current density
Under 2C, respectively the 30th, the 10th, battery charging and discharging 50 is enclosed, make ring-type elemental sulfur become the sulphur of short chain state and enter micropore control material
In the duct of material MC.
Fig. 4 is the cycle performance of battery figure that the present embodiment prepares.Fig. 4 left side is corresponding is to carry out under different current densities
Obtained specific discharge capacity is enclosed in discharge and recharge 200, and current density is 0.2C, 0.5C, 1C, 2C respectively, corresponding first circle electric discharge specific volume
Amount is 1074mA h g-1、968mA h g-1、845mA h g-1、746mA h g-1, after circulation 200 is enclosed, retain respectively puts
Electricity specific capacity is about 630mA h g-1、580mA h g-1、490mA h g-1、330mA h g-1.Fig. 4 right side is corresponding is relatively
Carry out the discharge and recharge of the different number of turns under high current density (2C), be then return to 0.2C.The left contrast with Fig. 4, at high current density
After lower discharge and recharge, the then same current density at 0.2C, specific capacity increases, and after circulation 200 circle, battery specific capacity declines
Relatively slow, illustrate that circulating battery stability improves, this is the effect that elemental sulfur enters micropore canals.
Fig. 5 is the charge and discharge electrograph that the present embodiment prepares battery, and before circulating battery, 50 circles are in higher current density
(2C) discharge and recharge under, it can be seen that have two discharge platforms and a charging platform, two discharge platform corresponding initial shapes respectively
The high-order ring-type S of state8Short chain S with low level2～S4.When, after the 51st encloses, only one of which discharge platform, voltage platform exists
About 1.7V, illustrates the short chain S of only low level2～S4.Illustrate, under higher current density, to be capable of the filling of micropore sulphur
In micropore canals.
Obviously, above-described embodiment is only by clearly demonstrating made example, and the not restriction to embodiment.Right
For those of ordinary skill in the field, can also make on the basis of the above description other multi-forms change or
Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change therefore amplified or change
Move within still in the protection domain of the invention.
Claims (8)
1. the method for high current density Fast Filling micropore sulphur in a lithium-sulfur cell, it is characterised in that comprise the steps：
（1）By micropore control material and elemental sulfur join in carbon disulfide, ultrasonic mix after obtain mix material；
（2）By step（1）Gained mixing material is dried, and obtains the carbon sulphur of micropore control material and elemental sulfur after carbon disulfide evaporation
Mixture；
（3）By step（2）Gained carbon-sulfur compound is fabricated to anode electrode piece, is prepared as battery again, then utilizes high electric current close
Degree carries out a fixing turn discharge and recharge to battery, and the sulphur that ring-type elemental sulfur becomes short chain state enters the duct that micropore controls material
In.
2. method according to claim 1, it is characterised in that described micropore control material is formation after ZIF-8 carbonization
Micro-pore carbon material.
3. method according to claim 1, it is characterised in that the mass ratio of described micropore control material and elemental sulfur is
85：15.
4. method according to claim 1, it is characterised in that step（1）Described ultrasonic power is 99 kHz, when ultrasonic
Between be 30 min.
5. method according to claim 1, it is characterised in that step（2）The temperature of described drying is 60 DEG C, and the time is
20~24h.
6. method according to claim 1, it is characterised in that step（3）The preparation of described battery need anode electrode piece,
Lithium piece and barrier film, electrolyte is LiNO3.
7. method according to claim 1, it is characterised in that step（3）Described high current density is the electric current of 2C ~ 5C
Density.
8. method according to claim 1, it is characterised in that step（3）The number of turns of described discharge and recharge is 10 ~ 50 circles.
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- 2016-10-11 CN CN201610888847.7A patent/CN106450190B/en not_active Expired - Fee Related
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| US20050042503A1 (en) * | 2003-08-23 | 2005-02-24 | Kim Ju-Yup | Lithium-sulfur battery |
| CN101728538A (en) * | 2009-11-26 | 2010-06-09 | 上海大学 | Ordered nanostructure sulphur/mesoporous carbon composite material for anode of lithium ion battery |
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