CN103985902A - Method for improving performance of lithium sulfur battery by utilizing desolvation colloidal electrolyte - Google Patents

Method for improving performance of lithium sulfur battery by utilizing desolvation colloidal electrolyte Download PDF

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Publication number
CN103985902A
CN103985902A CN201410240327.6A CN201410240327A CN103985902A CN 103985902 A CN103985902 A CN 103985902A CN 201410240327 A CN201410240327 A CN 201410240327A CN 103985902 A CN103985902 A CN 103985902A
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lithium
electrolyte
desolvation
sulfur cell
colloidal
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吴伯荣
穆道斌
刘琦
许洪亮
任永欢
王垒
吴振军
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Beijing Institute of Technology BIT
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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
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Dispersion Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention relates to a method for improving the performance of a lithium sulfur battery by utilizing desolvation colloidal electrolyte, which belongs to the technical field of electrochemistry and chemical power supply products. The desolvation colloidal electrolyte with high concentration is formed by carbonic ester solvent and lithium salt represented by LiPF6. The front step resistance of the electrode process can be reduced through the desolvation effect, and the electrochemical performance can be improved. Meanwhile, the dissolution of positive polysulfide can be inhibited through the electrolyte, so that the cycling stability of a positive electrode can be maintained. In addition, the growth of negative metal lithium dendritic crystals can be inhibited through the desolvation electrolyte, so that the safety performance of the battery can be improved, and the application prospect is good.

Description

A kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte
Technical field
The present invention relates to a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte, be particularly useful for the secondary lithium-sulfur cell taking sulfurized polyacrylonitrile as anodal lithium metal as negative pole, belong to the technical field of chemical products.
Background technology
Along with the continuous consumption of the non-renewable energy resources such as oil and fire coal, and the continuous increase of the mankind to energy demand; The exploitation of new forms of energy and storage have great importance to the mankind's sustainable development.Thereby the motorized of automobile can reduce the consumption of oil and reduce motor vehicle exhaust emission amount and improve atmosphere quality.Lithium ion battery replaces oil to have in practice application as the power of electric automobile.But the energy density of traditional lithium ion battery is limited, make the distance travelled of electric automobile and vehicle traction power compare and still have very large gap with traditional automobile taking oil as power; This has just limited the extensive use of electric automobile.Therefore, the green secondary cell of research and development high-energy-density high power density is extremely urgent.In addition, the fast development of information technology and the arrival in mobile Internet 4G epoch and the more functional requirement of digital product also propose very large challenge to the capacity of battery.But lithium-sulfur cell has prospect as follow-on high-energy-density secondary cell very much.The anodal theoretical specific energy of typical sulphur can reach 1672mAh/g, and theoretical energy density can reach 2600Wh/kg.The theoretical specific energy of lithium an-ode also can reach 3860mAh/g simultaneously, and normal potential that the more important thing is lithium metal is minimum (3.040Vvs standard hydrogen electrode) in all metals.But the subject matter of lithium-sulfur cell is the quick decay that the dissolving of the poly-sulphur lithium compound of electric discharge intermediate product in electrolyte causes positive electrode capacity, and the growth that another main problem is exactly negative pole Li dendrite causes battery short circuit to cause safety problem.
Because elemental sulfur is electronic body, for lithium sulfur battery anode material, a lot of focus is all on carbon sulphur composite material, and various mesoporous carbon such as Graphene, carbon nano-tube etc. are all used for doing the carrier of sulphur.Polymer at high temperature becomes key formation polymer sulphur composite material to be also used as lithium sulfur battery anode material with elemental sulfur in addition.Thereby mesoporous carbon can be wrapped up the dissolving of polysulfides intermediate product restriction intermediate product in electrolyte.Simultaneously polymer dielectric and fast-ionic conductor etc. are also used for the fail safe of the cyclical stability and the battery that improve lithium-sulphur cell positive electrode.Researcher also suppresses the dendritic growth of lithium anode with some electrolysis additives.But these methods fundamentally do not solve these problems of lithium-sulfur cell yet.
Summary of the invention
The object of the invention is dissolving in order to overcome polysulfides in lithium-sulfur cell and suppress the growth of Li dendrite, a kind of method of improving lithium-sulfur cell cyclical stability and fail safe with desolvation colloidal state electrolyte is provided.
The object of the invention is to be achieved through the following technical solutions.
A kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte, solute is joined in solvent, within 3-48 hour, obtain the high viscosity solution that range of viscosities is 10-100cp by stirring, control the mass ratio of solute and solvent between 0.4-0.8, obtain desolvation colloidal state electrolyte; Then used for electrolyte in lithium-sulfur cell by gained, can improve the chemical property of lithium-sulfur cell by this method.
Described solute is lithium hexafluoro phosphate (LiPF 6), lithium perchlorate (LiCIO 4), LiBF4 (LiBF 4), hexafluoroarsenate lithium (LiAsF 6) at least one.
Described solvent is carbonates solvent;
To be ethylene carbonate (EC) mix with one or more in dimethyl carbonate (DMC), diethyl carbonate (DEC), Merlon (PC), methyl ethyl carbonate (EMC) described solvent; Proportion requirement is arbitrary proportion.
The positive electrode mating with desolvation colloidal electrolyte consist of active material, conductive agent and binding agent, wherein the proportion requirement scope of positive electrode active materials and conductive agent is between 1-8, active material adds conductive agent composite material and binding agent proportion requirement scope is between 2-19, and described ratio is mass ratio; Wherein active material is sulfurized polyacrylonitrile or carbon sulphur composite material; Conductive agent is acetylene black or electrically conductive graphite; Binding agent is Kynoar (PVDF) or polyacrylonitrile (PAN); Barrier film is polyethylene (PE) or glass fibre; The negative material mating with desolvated colloidal electrolyte is lithium metal.
Beneficial effect
1, a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte of the present invention, because electrolytical high viscosity and colloidal state and electrolytical desolvation, this desolvation colloidal electrolyte can suppress the dissolving of anodal polysulfide, increases cyclical stability and the multiplying power cyclical stability of positive electrode.
2, a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte of the present invention, because viscosity increase has reduced the diffusion current density of electrolyte intermediate ion, increase the invertibity of electrode reaction, and the electric field strength that has reduced electrode surface due to the increase of ion concentration makes this desolvation colloidal electrolyte can suppress the growth of negative pole Li dendrite, increase the security performance of battery.
3, reduced the transfer reaction activity of lithium ion simultaneously due to the solvation of general electrolyte, battery performance is reduced; And desolvation colloidal electrolyte can reduce the impedance of electrode reaction, strengthen the chemical property of battery.In the secondary lithium-sulfur cell taking sulfurized polyacrylonitrile as anodal lithium metal as negative pole, show good chemical property by used for electrolyte this kind of desolvation colloidal state.This kind of method simple possible, operating procedure is controlled, is conducive to advance lithium-sulfur cell application.
Brief description of the drawings
Fig. 1 is the illustraton of model that common electrolyte solvent turns the desolvation (right side) of use (left side) and desolvation colloidal state electrolyte into, wherein common electrolyte consists of: EC and DMC are as solvent, wherein the mass ratio of EC and DMC is 1:1, and the mass ratio of LiPF6 and EC+DMC is 0.12;
Fig. 2 is the AC impedance figure that sulfurized polyacrylonitrile/electrolyte/lithium metal battery circulates after 3 times;
Fig. 3 is the SEM figure on smooth Cu paper tinsel surface;
Fig. 4 is for forming Li/ electrolyte/Cu battery with desolvation colloidal state electrolyte, and lithium deposits to the SEM figure on Cu paper tinsel surface; Depositing current density is 0.1mA/cm -2;
Fig. 5 is for forming Li/ electrolyte/Li battery with desolvation colloidal state electrolyte, and lithium deposits to the SEM figure on lithium paper tinsel surface; Deposition current is 0.1mA/cm -2;
Fig. 6 is the cycle performance figure of desolvation colloidal state electrolyte and common electrolyte;
Fig. 7 is the multiplying power cycle performance figure of desolvation colloidal state electrolyte and common electrolyte.
Fig. 8 is for forming Li/ electrolyte/Cu battery with common electrolyte, lithium deposits to the SEM figure on Cu paper tinsel surface;
Wherein depositing current density is 0.1mA/cm -2;
Fig. 9 is for forming Li/ electrolyte/Li battery with common electrolyte, lithium deposits to the SEM figure on lithium paper tinsel surface;
Wherein deposition current is 0.1mA/cm -2.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is further described.
Embodiment 1
With LiPF 6as solute, EC and DMC are as solvent, and wherein the mass ratio of EC and DMC is 1:1, by LiPF 6slowly join in the mixture of EC and DMC, and stir 24h, obtain high viscosity and gluey electrolyte solution; Now LiPF 6dissolving reach LiPF 6with the mass ratio of EC+DMC be 0.72; Fig. 1 has illustrated the solvation of general electrolyte and the desolvation of desolvation colloidal state electrolyte.In common electrolyte, lithium salt content is low, and the C=O group in carbonates solvent and lithium ion effect form complex compound, has reduced the activity of lithium ion.In desolvation colloidal electrolyte, lithium salt content is far above general electrolyte, and this makes the content of lithium ion more.Therefore the active force of lithium ion and C=O group reduces, and has reached the desolvated effect of lithium ion.Fig. 2 be with sulfurized polyacrylonitrile be the anode AC impedance figure after circulation 3 times with the battery of the desolvation colloidal state electrolyte after common electrolyte and modification and lithium metal composition respectively, experimental study the impact of desolvation on electrode and electrolyte liquor interface.The semicircle that can obviously find out the representative Charge-transfer resistance that uses desolvated colloidal electrolyte from figure obviously diminishes, and has illustrated that the desolvation colloidal state electrolyte after modification has reduced the Charge-transfer resistance at electrode and electrolyte liquor interface.This is because the desolvation of lithium ion has reduced the preposition step of converting impedance of electrode process, and has illustrated that lithium ion is to control step in the exchange at electrode and electrolyte liquor interface.And as can be seen from the figure the ohmage of the desolvation colloidal state electrolyte after modification is greater than common electrolyte, this electrolyte being mainly attributed to after modification has high viscosity feature.
Fig. 3 is the SEM figure of smooth copper surface, and as can be seen from the figure the copper surface of deposition is very smoothless.Electrolyte is assembled to Li/ electrolyte/Cu battery, taking current density as 0.1mA/cm -2the growth of Li dendrite can be found significantly to suppress in the surface that lithium is deposited to copper, as shown in Figure 4, only has a small amount of dendritic growth, and surface is comparatively level and smooth.
Electrolyte is assembled to Li/ electrolyte/Li battery, and the surface that as shown in Figure 5 lithium is deposited to lithium also can obviously find out that desolvation colloidal electrolyte can suppress the growth of Li dendrite.
Taking sulfurized polyacrylonitrile as positive electrode, lithium metal as negative pole, polyethylene as barrier film, desolvation colloidal electrolyte is electrolyte composition battery, press 60mA/g current density constant-current discharge to 1V, then constant current charge is to 3V, and as shown in Figure 6, after circulating 50 weeks, reversible capacity is 1276mAh/g.Same with above-mentioned battery testing the high rate performance of battery.Carry out charge and discharge cycles by 60mA/g, 120mA/g, 360mA/g, 600mA/g, 60mA/g respectively, circulate respectively to as shown in Figure 7 a different current density 10 times, and corresponding capacity is respectively 1575mAh/g, 1455mAh/g, 1261mAh/g, 610mAh/g, 1426mAh/g.These data have reflected that desolvation colloidal state electrolyte has improved cyclical stability and the multiplying power cyclical stability of battery.
Embodiment 2
With LiPF 6as solute, EC and DMC are as solvent, and wherein the mass ratio of EC and DMC is 1:1, by LiPF 6slowly join in the mixture of EC and DMC, and constantly stir, until obtain high viscosity and gluey electrolyte solution; Now LiPF 6dissolving reach LiPF 6with the mass ratio of EC+DMC be 0.8; Electrolyte is assembled to Li/ electrolyte/Cu battery, taking current density as 0.1mA/cm -2the growth of Li dendrite can be found significantly to suppress in the surface that lithium is deposited to copper, and electrolyte is assembled to Li/ electrolyte/Li battery, and the surface that lithium is deposited to lithium also can obtain the result that desolvation colloidal electrolyte can suppress the growth of Li dendrite.Taking sulfurized polyacrylonitrile as positive electrode, lithium metal is negative pole, taking polyethylene as barrier film, desolvation colloidal electrolyte is electrolyte composition battery, press 60mA/g current density constant-current discharge to 1V, then constant current charge is to 3V, and after circulating 50 weeks, reversible capacity is 1325mAh/g, demonstrates good chemical property.
Embodiment 3
With LiPF 6as solute, EC and DMC are as solvent, and wherein the mass ratio of EC and DMC is 1:1, prepare common binary electrolyte, wherein LiPF 6with the mass ratio of EC+DMC be 0.12.Electrolyte is assembled to Li/ electrolyte/Cu battery, taking current density as 0.1mA/cm -2lithium is deposited to the surface of copper.Obviously find out as shown in Figure 8 after deposition to such an extent that copper surface is relatively coarse, Li dendrite growth obviously.Then electrolyte is assembled to Li/ electrolyte/Li battery, the growth of a large amount of Li dendrites also can be obviously found out on the surface that as shown in Figure 9 lithium is deposited to lithium.Taking sulfurized polyacrylonitrile as positive electrode active materials, lithium metal be negative pole taking polyethylene as barrier film, common electrolyte composition battery, with 60mA/g current density constant-current discharge, to 1V, then constant current charge is to 3V, circulate 50 weeks afterwards reversible capacity be 851mAh/g.Same with above-mentioned battery testing the high rate performance of battery, carry out charge and discharge cycles with 60mA/g, 120mA/g, 360mA/g, 600mA/g, 60mA/g, the high rate performance after circulation is starkly lower than desolvation colloidal electrolyte.
Contrast common electrolyte and desolvation colloidal state electrolyte the growth that uses the method for desolvation colloidal state electrolyte to be conducive to suppress Li dendrite can be obviously described; And illustrated in real lithium electrode surface, the desolvation colloidal electrolyte after modification has also played the effect that suppresses Li dendrite growth, improves the security performance of battery.Use the method for desolvation colloidal state electrolyte not only can suppress the growth of Li dendrite simultaneously, can reduce the preposition step of converting impedance of anodal and electrolyte interface simultaneously, improve the chemical property of battery.Sulfurized polyacrylonitrile is that the comparative studies result of the chemical property of anodal lithium-sulfur cell shows to make by the method that desolvation colloidal state electrolyte improves performance that anodal cyclical stability is relative with multiplying power stability to be all improved.

Claims (6)

1. one kind is improved the method for lithium-sulfur cell performance with desolvation colloidal state electrolyte, it is characterized in that: just solute joins in solvent, within 3-48 hour, obtain the high viscosity solution that range of viscosities is 10-100cp by stirring, control the mass ratio of solute and solvent between 0.4-0.8; Then the electrolyte solution of gained is used for to lithium-sulfur cell, can improves the chemical property of lithium-sulfur cell.
2. a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte as claimed in claim 1, is characterized in that: described solute is lithium hexafluoro phosphate lithium perchlorate, LiBF4, at least one in hexafluoroarsenate lithium.
3. a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte as claimed in claim 1, is characterized in that: described solvent is carbonates solvent.
4. a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte as described in claim 1 or 3, is characterized in that: to be ethylene carbonate mix with one or more in dimethyl carbonate, diethyl carbonate, Merlon, methyl ethyl carbonate described solvent.
5. a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte as claimed in claim 1, it is characterized in that: the positive electrode mating with desolvated colloidal electrolyte consist of active material, conductive agent and binding agent, described positive electrode active materials is sulfurized polyacrylonitrile or carbon sulphur composite material; Described barrier film is polyethylene or glass fibre, and described conductive agent is acetylene black or electrically conductive graphite, and described binding agent is Kynoar or polyacrylonitrile; The negative material mating with desolvated colloidal electrolyte is lithium metal.
6. a kind of method of improving lithium-sulfur cell performance with desolvation colloidal state electrolyte as described in claim 1 or 5, it is characterized in that: the proportion requirement scope of positive electrode active materials and conductive agent is between 1-8, active material adds conductive agent composite material and binding agent proportion requirement scope is between 2-19, and described ratio is mass ratio.
CN201410240327.6A 2014-05-30 2014-05-30 Method for improving performance of lithium sulfur battery by utilizing desolvation colloidal electrolyte Pending CN103985902A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107069093A (en) * 2017-03-10 2017-08-18 中国计量大学 A kind of high concentration esters electrolyte for lithium-sulfur cell
CN109786842A (en) * 2018-12-26 2019-05-21 中国电子科技集团公司第十八研究所 A kind of high safety high-energy-density lithium/fluorocarbons battery preparation method
CN111781253A (en) * 2020-06-19 2020-10-16 国联汽车动力电池研究院有限责任公司 Device and method for measuring desolvation activation energy of lithium ions in electrolyte
US11581571B2 (en) 2020-04-29 2023-02-14 Wuhan Rikomay New Energy Co., Ltd. Method for improving performance of layered electrode materials
CN115799504A (en) * 2022-12-20 2023-03-14 北京化工大学 Vulcanized polyacrylonitrile anode and preparation method and application thereof

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CN1335653A (en) * 2000-07-25 2002-02-13 三星Sdi株式会社 Electrolyte for lithium sulphur cell and lithium sulphur cell containing the same electrolyte
CN1389948A (en) * 2001-06-01 2003-01-08 三星Sdi株式会社 Lithium-sulfur cell
CN101667640A (en) * 2008-09-01 2010-03-10 索尼株式会社 Positive electrode active material, positive electrode using the same and non-aqueous electrolyte secondary battery
CN102598390A (en) * 2009-10-27 2012-07-18 旭硝子株式会社 Nonaqueous electrolyte solution for secondary battery, and secondary battery
CN103682361A (en) * 2013-11-28 2014-03-26 四川大学 Adhesive for anode of lithium sulfur battery and application of adhesive to preparation of lithium sulfur battery

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1335653A (en) * 2000-07-25 2002-02-13 三星Sdi株式会社 Electrolyte for lithium sulphur cell and lithium sulphur cell containing the same electrolyte
CN1389948A (en) * 2001-06-01 2003-01-08 三星Sdi株式会社 Lithium-sulfur cell
CN101667640A (en) * 2008-09-01 2010-03-10 索尼株式会社 Positive electrode active material, positive electrode using the same and non-aqueous electrolyte secondary battery
CN102598390A (en) * 2009-10-27 2012-07-18 旭硝子株式会社 Nonaqueous electrolyte solution for secondary battery, and secondary battery
CN103682361A (en) * 2013-11-28 2014-03-26 四川大学 Adhesive for anode of lithium sulfur battery and application of adhesive to preparation of lithium sulfur battery

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107069093A (en) * 2017-03-10 2017-08-18 中国计量大学 A kind of high concentration esters electrolyte for lithium-sulfur cell
CN107069093B (en) * 2017-03-10 2020-04-24 中国计量大学 High-concentration ester electrolyte for lithium-sulfur battery
CN109786842A (en) * 2018-12-26 2019-05-21 中国电子科技集团公司第十八研究所 A kind of high safety high-energy-density lithium/fluorocarbons battery preparation method
US11581571B2 (en) 2020-04-29 2023-02-14 Wuhan Rikomay New Energy Co., Ltd. Method for improving performance of layered electrode materials
CN111781253A (en) * 2020-06-19 2020-10-16 国联汽车动力电池研究院有限责任公司 Device and method for measuring desolvation activation energy of lithium ions in electrolyte
CN115799504A (en) * 2022-12-20 2023-03-14 北京化工大学 Vulcanized polyacrylonitrile anode and preparation method and application thereof

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Application publication date: 20140813