CN107819152A - A kind of reference electrolyte and preparation method that can improve lithium-sulfur cell cycle performance - Google Patents
A kind of reference electrolyte and preparation method that can improve lithium-sulfur cell cycle performance Download PDFInfo
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- CN107819152A CN107819152A CN201711072813.1A CN201711072813A CN107819152A CN 107819152 A CN107819152 A CN 107819152A CN 201711072813 A CN201711072813 A CN 201711072813A CN 107819152 A CN107819152 A CN 107819152A
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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
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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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
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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
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0037—Mixture of solvents
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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 a kind of reference electrolyte and preparation method that can improve lithium-sulfur cell cycle performance;Including ether solvent, lithium salts, lithium nitrate and improve cycle performance additive;Ether solvent is the mixture of two kinds of solvents, and the first solvent is:Any one in 1,3 dioxolane or Isosorbide-5-Nitrae dioxane, second of solvent is:Any one in glycol dimethyl ether, diethylene glycol dimethyl ether, tetraethyleneglycol dimethyl ether;Lithium salts is LiPF6、LiBF4, any one in LiTFSi, LiFSi or LiBOB;It is any one in 3 aminopropyltriethoxywerene werenes, hexamethyldisilane or silicic acid tetrem fat to improve cycle performance additive;Simple with configuration process, solvent and additive are cheap, and materials are saved, and can play good negative pole lithium protecting effect, and lithium-sulfur cell electrolyte is used in lithium-sulfur cell, the advantages of can significantly improving the cycle performance of lithium-sulfur cell and security performance.
Description
Technical field
The invention belongs to electrolyte preparing technical field, and in particular to a kind of base that can improve lithium-sulfur cell cycle performance
Quasi- electrolyte and preparation method.
Background technology
In recent years, lithium rechargeable battery was with its larger energy density, higher operating voltage, longer cycle life
And the advantages that pollution-free, has turned into all kinds of digital and electric automobile product preferred power supplys.However as society rapid development,
The high expectation value and electric bicycle of digital product, electric automobile, the extensive development of intelligent grid and application, development quality
Specific energy density and the higher secondary cell of energy density per unit volume metric density, it is the only way which must be passed for meeting the needs of social fast development,
And the very big technological challenge that researcher is faced now.Therefore seeking a kind of brand-new, high energy battery system is always
The study hotspot in energy storage field.
Lithium-sulfur cell has been constantly subjected to the extensive concern of researcher since the seventies in last century.Elemental sulfur is as lithium sulphur two
Primary cell positive electrode, theoretical specific capacity 1675mAh/g, when being assembled into battery as negative pole using lithium metal, its theoretical ratio
Energy is up to 2600 Wh/kg, possesses and is widely applied and DEVELOPMENT PROSPECT.Moreover, elemental sulfur amount of storage it is big, it is cheap and
It is pollution-free, therefore lithium-sulfur cell is considered as the high-energy-density energy storage system of great exploitation potential.However, lithium-sulfur cell although
Possess the advantages of so many, elemental sulfur and discharging product Li2S has electrical insulating property, and conductive capability is poor, and sulphur in discharge process
Cubical expansivity be up to 80%, reduce electrode active the problems such as " the shuttle effect " of electrochemical reaction intermediate product polysulfide
The property utilization rate of material and the cycle life of battery, seriously hinder lithium-sulfur cell and march toward commercialization.
For above-mentioned lithium-sulfur cell weak point, countries in the world researchers have carried out a series of researchs, mainly around subtracting
Few polysulfide shuttle effect, improves electrode active material utilization rate, so as to improve battery cycle life, and set about mostly be a little
Start with from positive electrode, around heteroatom doping carbon-based material, carbon-based material and organic polymer is compound, carbon-based material and nothing
Machine Material cladding etc. conducts a research, such as:Wang Weikun of institute of Chemical Defence et al. starts with from high-performance positive electrode, from just
Lithium-sulfur cell cycle life is improved in terms of the material modification of pole.Metal Inst., Chinese Academy of Sciences Tang Xiao nanmus et al. are answered from lithium-sulfur cell
The interaction for closing guest materials and polysulfide in sulphur positive pole is set about, and improves the cycle life of battery.But these design sides
Method is cumbersome, and positive pole synthesis is cumbersome.
The content of the invention
There is provided that a kind of configuration process is simple, avoids it is an object of the invention to overcome the deficiencies in the prior art
Cumbersome positive electrode synthesis step, it is time saving and energy saving to operate, and can obtain lithium-sulfur cell cyclical stability and cycle period
To a kind of reference electrolyte and preparation method that can improve lithium-sulfur cell cycle performance being obviously improved.
The object of the present invention is achieved like this:The reference electrolyte includes ether solvent, lithium salts, lithium nitrate and improvement
Cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,3- dioxolane or
Any one in 1,4- dioxane, second of solvent is:Glycol dimethyl ether, diethylene glycol dimethyl ether or tetraethylene glycol
Any one in dimethyl ether;Described lithium salts is LiPF6、LiBF4, any one in LiTFSi, LiFSi or LiBOB;Institute
It is appointing in APTES, hexamethyldisilane or silicic acid tetrem fat that stating, which improves cycle performance with additive,
Meaning is a kind of.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take two kinds it is molten
Agent uniformly mixes, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than 1ppm;
Step 2:Lithium salts is taken, and lithium salts is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixing
Liquid;The molar concentration of the lithium salts is 0.8~1.5mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 0.1%~3% in the semi-finished product electrolyte;
Step 4:Taking improves cycle performance additive, and the improvement cycle performance is slowly added in step 3 with additive
Described semi-finished product electrolyte, is made reference electrolyte;Improve the quality of cycle performance additive in the reference electrolyte
Fraction is 1%~10%.
Preferably, the mass ratio of two kinds of solvents in the step 1 is 1:1.
The present invention is simple with configuration process, and solvent for use and additive are cheap, and materials save, and can play good bear
Pole lithium protecting effect, the lithium-sulfur cell electrolyte of configuration are used in lithium-sulfur cell, can make the cycle performance and peace of lithium-sulfur cell
The advantages of full performance significantly improves.
Embodiment
The present invention is a kind of reference electrolyte and preparation method that can improve lithium-sulfur cell cycle performance, wherein, the base
Quasi- electrolyte includes ether solvent, lithium salts, lithium nitrate and improves cycle performance additive;Described ether solvent is two kinds
The mixture of solvent, the first solvent are:Any one in 1,3- dioxolane or 1,4- dioxane, second of solvent
For:Any one in glycol dimethyl ether, diethylene glycol dimethyl ether or tetraethyleneglycol dimethyl ether;Described lithium salts is LiPF6、
LiBF4, any one in LiTFSi, LiFSi or LiBOB;The improvement cycle performance is 3- aminopropyls three with additive
Any one in Ethoxysilane, hexamethyldisilane or silicic acid tetrem fat.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take two kinds it is molten
Agent uniformly mixes, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than 1ppm;
Step 2:Lithium salts is taken, and lithium salts is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixing
Liquid;The molar concentration of the lithium salts is 0.8~1.5mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 0.1%~3% in the semi-finished product electrolyte;
Step 4:Taking improves cycle performance additive, and the improvement cycle performance is slowly added in step 3 with additive
Described semi-finished product electrolyte, is made reference electrolyte;Improve the quality of cycle performance additive in the reference electrolyte
Fraction is 1%~10%.The mass ratio of two kinds of solvents in the step 1 is 1:1.
In order to more clearly explain the present invention, it is further described in conjunction with specific embodiment.It is specific real
Under applying for example:
Embodiment one
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, including ether solvent, lithium salts, lithium nitrate and improvement
Cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,3- dioxolane,
Second of solvent be:Glycol dimethyl ether;Described lithium salts is LiTFSi;The improvement cycle performance is 3- amino with additive
Propyl-triethoxysilicane.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take 1,3- bis-
Oxygen five rings and glycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:LiTFSi is taken, and LiTFSi is slowly added in the ether solvent described in step 1, uniformly mixing, is made
Mixed liquor;The molar concentration of the LiTFSi is 1.5mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 1.5% in the semi-finished product electrolyte;
Step 4:APTES is taken, and APTES is slowly added to step 3
Described in semi-finished product electrolyte, reference electrolyte is made;APTES in the reference electrolyte
Mass fraction is 5%.The mass ratio of two kinds of solvents in the step 1 is 1:1.
Embodiment two
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is: 1
, 4- dioxane, second of solvent be:Diethylene glycol dimethyl ether;Described lithium salts is LiFSi;The improvement cycle performance is used
Additive is hexamethyldisilane.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take Isosorbide-5-Nitrae-two
The ring of oxygen six and diethylene glycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:LiFSi is taken, and LiFSi is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixed
Close liquid;The molar concentration of the LiFSi is 1.15mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 3% in the semi-finished product electrolyte;
Step 4:Hexamethyldisilane is taken, and hexamethyldisilane is slowly added to the semi-finished product electrolyte described in step 3,
Reference electrolyte is made;The mass fraction of hexamethyldisilane is 10% in the reference electrolyte.Two kinds in the step 1
The mass ratio of solvent is 1:1.
Embodiment three
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,
3- dioxolanes, second of solvent are:Tetraethyleneglycol dimethyl ether;Described lithium salts is LiFSi;The improvement cycle performance is with adding
It is silicic acid tetrem fat to add agent.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take 1,3- bis-
Oxygen five rings and tetraethyleneglycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:LiFSi is taken, and LiFSi is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixed
Close liquid;The molar concentration of the LiFSi is 0.8mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 1.5% in the semi-finished product electrolyte;
Step 4:Silicic acid tetrem fat is taken, and silicic acid tetrem fat is slowly added to the semi-finished product electrolyte described in step 3, is made
Reference electrolyte;The mass fraction of silicic acid tetrem fat is 5% in the reference electrolyte.Two kinds of solvents in the step 1
Mass ratio is 1:1.
Example IV
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,
4- dioxane, second of solvent are:Glycol dimethyl ether;Described lithium salts is LiBF4;The improvement cycle performance addition
Agent is APTES.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take Isosorbide-5-Nitrae-two
The ring of oxygen six and glycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:Take LiBF4, and by LiBF4It is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixed
Close liquid;The LiBF4Molar concentration be 0.8mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 1.5% in the semi-finished product electrolyte;
Step 4:APTES is taken, and APTES is slowly added to step 3
Described in semi-finished product electrolyte, reference electrolyte is made;APTES in the reference electrolyte
Mass fraction is 5%.The mass ratio of two kinds of solvents in the step 1 is 1:1.
Embodiment five
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1
, 4- dioxane, second of solvent be:Tetraethyleneglycol dimethyl ether;Described lithium salts is LiTFSi;The improvement cycle performance is used
Additive is hexamethyldisilane.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take Isosorbide-5-Nitrae-two
The ring of oxygen six and tetraethyleneglycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:LiTFSi is taken, and LiTFSi is slowly added in the ether solvent described in step 1, uniformly mixing, is made
Mixed liquor;The molar concentration of the LiTFSi is 1.5mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 0.1% in the semi-finished product electrolyte;
Step 4:Hexamethyldisilane is taken, and hexamethyldisilane is slowly added to the semi-finished product electrolyte described in step 3,
Reference electrolyte is made;The mass fraction of hexamethyldisilane is 10% in the reference electrolyte.Two kinds in the step 1
The mass ratio of solvent is 1:1.
Embodiment six
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,
3- dioxolanes, second of solvent are:Diethylene glycol dimethyl ether;Described lithium salts is LiBOB;The improvement cycle performance is with adding
It is silicic acid tetrem fat to add agent.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take 1,3- bis-
Oxygen five rings and diethylene glycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:LiBOB is taken, and LiBOB is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixed
Close liquid;The molar concentration of the LiBOB is 1.15mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 1.5% in the semi-finished product electrolyte;
Step 4:Silicic acid tetrem fat is taken, and silicic acid tetrem fat is slowly added to the semi-finished product electrolyte described in step 3, is made
Reference electrolyte;The mass fraction of silicic acid tetrem fat is 5% in the reference electrolyte.Two kinds of solvents in the step 1
Mass ratio is 1:1.
Embodiment seven
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,
3- dioxolanes, second of solvent are:Glycol dimethyl ether;Described lithium salts is LiTFSi;The improvement cycle performance is with adding
It is APTES to add agent.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take 1,3- bis-
Oxygen five rings and glycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:LiTFSi is taken, and LiTFSi is slowly added in the ether solvent described in step 1, uniformly mixing, is made
Mixed liquor;The molar concentration of the LiTFSi is 0.8mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 3% in the semi-finished product electrolyte;
Step 4:APTES is taken, and APTES is slowly added to step 3
Described in semi-finished product electrolyte, reference electrolyte is made;APTES in the reference electrolyte
Mass fraction is 5%.The mass ratio of two kinds of solvents in the step 1 is 1:1.
Embodiment eight
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,
3- dioxolanes, second of solvent are:Diethylene glycol dimethyl ether;Described lithium salts is LiPF6;The improvement cycle performance is with adding
It is hexamethyldisilane to add agent.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take 1,3- bis-
Oxygen five rings and diethylene glycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:Take LiPF6, and by LiPF6It is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixed
Close liquid;The LiPF6Molar concentration be 1.15mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 0.1% in the semi-finished product electrolyte;
Step 4:Hexamethyldisilane is taken, and hexamethyldisilane is slowly added to the semi-finished product electrolyte described in step 3,
Reference electrolyte is made;The mass fraction of hexamethyldisilane is 1% in the reference electrolyte.Two kinds in the step 1
The mass ratio of solvent is 1:1.
Embodiment nine
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1,
3- dioxolanes, second of solvent are:Tetraethyleneglycol dimethyl ether;Described lithium salts is LiBF4;The improvement cycle performance is with adding
It is silicic acid tetrem fat to add agent.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take 1,3- bis-
Oxygen five rings and tetraethyleneglycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:Take LiBF4, and by LiBF4It is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixed
Close liquid;The LiBF4Molar concentration be 1.15mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 0.1% in the semi-finished product electrolyte;
Step 4:Silicic acid tetrem fat is taken, and silicic acid tetrem fat is slowly added to the semi-finished product electrolyte described in step 3, is made
Reference electrolyte;The mass fraction of silicic acid tetrem fat is 1% in the reference electrolyte.Two kinds of solvents in the step 1
Mass ratio is 1:1.
Embodiment ten
A kind of reference electrolyte that can improve lithium-sulfur cell cycle performance, the reference electrolyte include ether solvent, lithium salts, nitre
Sour lithium and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, and the first solvent is:1
, 4- dioxane, second of solvent be:Glycol dimethyl ether;Described lithium salts is LiTFSi;The improvement cycle performance is with adding
It is APTES to add agent.
A kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance, comprises the following steps:
Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take Isosorbide-5-Nitrae-two
The ring of oxygen six and glycol dimethyl ether uniformly mix, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than
1ppm;
Step 2:LiTFSi is taken, and LiTFSi is slowly added in the ether solvent described in step 1, uniformly mixing, is made
Mixed liquor;The molar concentration of the LiTFSi is 1.15mol/L;
Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made
Liquid, the mass fraction of lithium nitrate is 0.1% in the semi-finished product electrolyte;
Step 4:APTES is taken, and APTES is slowly added to step 3
Described in semi-finished product electrolyte, reference electrolyte is made;APTES in the reference electrolyte
Mass fraction is 10%.The mass ratio of two kinds of solvents in the step 1 is 1:1.
Experimental example one
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment one, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 1, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 1 is identical with embodiment one, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 1, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 1, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example two
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment two, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 2, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 2 is identical with embodiment two, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 2, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 2, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example three
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment three, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 3, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 3 is identical with embodiment three, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 3, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 3, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example four
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in example IV, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 4, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 4 is identical with example IV, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 4, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 4, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example five
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment five, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 5, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 5 is identical with embodiment five, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 5, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 5, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example six
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment six, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 6, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 6 is identical with embodiment six, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 6, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 6, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example seven
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment seven, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 7, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 7 is identical with embodiment seven, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 7, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 7, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example eight
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment eight, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 8, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 8 is identical with embodiment eight, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 8, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 8, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example nine
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment nine, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 9, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge
Electric circulating current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 9 is identical with embodiment nine, but omits step 4, and not addition improves
Cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 9, adds and completes
Stirring at normal temperature 1 hour afterwards, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 9, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
Experimental example ten
The 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte prepared in embodiment ten, after the completion of addition often
Temperature stirring 1 hour, all configurations operate in the not exceeded argon gas atmosphere glove box of water oxygen content.By purity be 99.5% with
On sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses 1-METHYLPYRROLIDONE
(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.Lithium metal is used as negative pole, electricity
Solution liquid is above-mentioned electrolyte, is assembled into the battery of experimental example 10, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), fill
Discharge cycles electric current is that density is 0.5C.
The preparation method of the reference electrolyte of comparative example 10 is identical with embodiment ten, but omits step 4, and not addition changes
Kind cycle performance additive, the 3-APS that mass ratio is 5% is added on the basis of the reference electrolyte of comparative example 10, has been added
Into rear stirring at normal temperature 1 hour, all configurations operated in the not exceeded argon gas atmosphere glove box of water oxygen content.It is by purity
More than 99.5% sublimed sulfur, acetylene black, PVDF in mass ratio 70:20:10 is well mixed, and mixed solvent uses N- methylpyrroles
Alkanone(NMP), it is mixed into slurry and is coated on aluminium foil, 80 DEG C is dried in vacuo 12 hours, and positive plate is made.It is negative to use lithium metal
Pole, electrolyte are above-mentioned electrolyte, are assembled into the battery of comparative example 10, discharge and recharge blanking voltage be 1.5-3.0V (vs. Li/ Li+), charge and discharge cycles electric current is that density is 0.5C.
By above-mentioned experimental example one, experimental example two, experimental example three, experimental example four, experimental example five, experimental example six, experimental example seven,
Battery in experimental example eight, experimental example nine and experimental example ten is tested, in configuration condition and the situation of test price adjustment all same
Under, its test result such as following table:
As seen from the above table, it is electrolysed in the present invention by the battery overall performance of reference electrolyte in embodiment better than comparative example benchmark
Battery prepared by liquid, the battery capacity conservation rate prepared particularly by electrolyte of the present invention reach more than 39.8%.
Claims (3)
- A kind of 1. reference electrolyte that can improve lithium-sulfur cell cycle performance, it is characterised in that:The reference electrolyte includes ether Class solvent, lithium salts, lithium nitrate and improvement cycle performance additive;Described ether solvent is the mixture of two kinds of solvents, The first solvent is:Any one in 3- dioxolanes or 1,4- dioxane, second of solvent is:Glycol dimethyl ether, Any one in diethylene glycol dimethyl ether or tetraethyleneglycol dimethyl ether;Described lithium salts is LiPF6、LiBF4、LiTFSi、 Any one in LiFSi or LiBOB;The improvement cycle performance is APTES, six with additive Any one in methyl disilane or silicic acid tetrem fat.
- 2. a kind of preparation method for the reference electrolyte that can improve lithium-sulfur cell cycle performance as claimed in claim 1, its It is characterised by:The preparation method comprises the following steps:Step 1:Make to be in argon gas atmosphere inside glove box, and under the conditions of internal water oxygen content value is not exceeded, take two kinds it is molten Agent uniformly mixes, and ether solvent is made;The water content value is less than 1ppm, and oxygen content value is less than 1ppm;Step 2:Lithium salts is taken, and lithium salts is slowly added in the ether solvent described in step 1, uniformly mixing, is made mixing Liquid;The molar concentration of the lithium salts is 0.8~1.5mol/L;Step 3:Lithium nitrate is taken, and lithium nitrate is slowly added in the mixed liquor described in step 2, semi-finished product electrolysis is made Liquid, the mass fraction of lithium nitrate is 0.1%~3% in the semi-finished product electrolyte;Step 4:Taking improves cycle performance additive, and the improvement cycle performance is slowly added in step 3 with additive Described semi-finished product electrolyte, is made reference electrolyte;Improve the quality of cycle performance additive in the reference electrolyte Fraction is 1%~10%.
- A kind of 3. preparation method of the lithium sulphur electrolyte of negative pole lithium protection according to claim 2, it is characterised in that:It is described The mass ratio of two kinds of solvents in step 1 is 1:1.
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