CN113206299A - Electrolyte of lithium ion battery and preparation method thereof - Google Patents
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Abstract
The invention discloses an electrolyte of a lithium ion battery, which comprises an organic solvent and a solute, wherein the organic solvent is a mixed solution formed by mixing five components of ethylene carbonate, methyl ethyl carbonate, dimethyl carbonate, fluoroethylene carbonate and dimethyl sulfoxide; the solute comprises two components of lithium salt and ionic liquid, or three components of lithium salt, ionic liquid and lithium fluoride, wherein the ionic liquid is N-octyl pyridine tetrafluoroborate. The invention also discloses a preparation method of the electrolyte. According to the invention, the N-octyl pyridine tetrafluoroborate is used as the ionic liquid, an SEI film can be effectively formed, but the conductivity of the electrolyte is reduced, so that the conductivity of the electrolyte is improved by adding lithium fluoride, and the performance of the electrolyte is further improved.
Description
Technical Field
The invention relates to the field of lithium ion battery electrolyte, in particular to lithium ion battery electrolyte and a preparation method thereof.
Background
Lithium ion batteries in widespread use today are composed mainly of a combustible organic electrolyte, such as a mixture of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Ethyl Methyl Carbonate (EMC) and fluoroethylene carbonate (FEC), an active oxygen-containing positive electrode as oxidant, such as LiCoO2And graphite cathode capable of supporting combustionAnd (4) forming. When the battery encounters abnormal conditions such as overcharge, internal short circuit or mechanical damage, the battery temperature increases and the rate of exothermic chemical reactions within the battery also increases, forming a malignant positive feedback cycle; the electrolyte inside the lithium ion battery is inherently a flammable solvent, and when the temperature continues to rise to a certain level, it causes fire and combustion, which is a serious disaster for large-sized batteries. Therefore, it is a better strategy to reduce the flammability of the organic electrolyte to protect the battery.
Currently, the general strategies for reducing the flammability of lithium ion batteries are: 1) adding a flame retardant: starting from the electrolyte, the electrolyte is one of the methods for solving the safety problem of the lithium battery, and the electrolyte can have better flame resistance by adding a solvent which has high solubility and is not flammable, such as phosphate, fluorinated ester and the like, so that the safety of the battery is improved. 2) Adding an ionic liquid: the ionic liquid is a non-volatile solvent, has good thermal stability, chemical stability and electrochemical stability, and can be used as an independent electrolyte, an additive, a filler in a gel polymer electrolyte and the like.
The ionic liquid structurally consists of anions and cations, and the ions interact with each other through coulomb force. Due to the strong electrostatic interaction between ions, the ionic liquid has higher viscosity compared with the traditional organic solvent. Ionic liquids are generally relatively viscous, exhibiting low vapor pressure and strong supercooling tendencies. The ionic liquid is not flammable due to low vapor pressure, and the non-flammable property of the ionic liquid is one of the main reasons for using the ionic liquid as the flame retardant of the lithium ion battery electrolyte. Pure ionic liquid electrolyte generally cannot form an effective SEI film on a graphite negative electrode, so that reductive decomposition or cation intercalation in graphite occurs inevitably on the graphite negative electrode, and the battery cannot be charged and discharged normally. In order to enhance the compatibility of the ionic liquid with the graphite negative electrode, organic additives such as Ethylene Carbonate (EC), dimethyl carbonate (DMC), EMC (ethyl methyl carbonate), and the like are generally introduced into the ionic liquid electrolyte to optimize the interfacial properties between the graphite negative electrode and the ionic liquid. The properties of ionic liquids can be modified by various structural changes of cations and anions.
Low rate, low Li of battery due to high viscosity of ionic liquid+The disadvantages of high migration number and cost, such as the general problem of conductivity reduction, and the safety problem of the lithium ion battery still need to be solved. LiPF6Is a widely used lithium ion battery electrolyte material, has good conductivity and electrochemical stability, but has poor thermal stability, and is easy to decompose to generate PF when the storage temperature is too high5Gas, affecting the chemical and electrochemical properties of the electrolyte, and LiPF6Susceptible to hydrolysis, resulting in reaction with water to release HF gas, for LiCoO2Or LiMn2O4The cycling performance of (c) has an adverse effect. LiPF6The heat resistance stability under different conditions is still not solved, so that the problem of conductivity reduction of the lithium ion battery electrolyte after the ionic liquid is added is solved, and the LiPF is improved6The thermal stability, the inhibition of degradation and degeneration of the lithium ion battery are problems which are urgently needed to be solved in the field of lithium ion batteries.
Disclosure of Invention
The invention aims to provide an electrolyte of a lithium ion battery and a preparation method thereof, and aims to solve the problem that an effective SEI film cannot be formed when an ionic liquid is added into the lithium ion battery in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the electrolyte of the lithium ion battery comprises an organic solvent and a solute, wherein the solute is dissolved in the organic solvent to form a solution with the molar concentration of 3.7-5.1mo1/L, and the optimal value is 4.0 mol/L.
The organic solvent is composed of five components of ethylene carbonate, methyl ethyl carbonate, dimethyl carbonate, fluoroethylene carbonate and dimethyl sulfoxide which are subjected to drying dehydration treatment by a molecular sieve or calcium hydride, wherein the fluoroethylene carbonate is dissolved in the other four components to obtain a mixed solution, the volume ratio of the ethylene carbonate, the methyl ethyl carbonate, the dimethyl carbonate and the dimethyl sulfoxide in the organic solvent is 1.0:1.0:1.0 (0.1-0.5), and the weight percentage of the fluoroethylene carbonate in the organic solvent is 3 wt%.
The solute comprises two components of lithium salt and ionic liquid, or three components of lithium salt, ionic liquid and lithium fluoride. Wherein:
the ionic liquid is N-octyl pyridine tetrafluoroborate, and the cationic structural formula in the N-octyl pyridine tetrafluoroborate is as follows:
the anion structural formula in the N-octyl pyridine tetrafluoroborate is as follows:
the lithium salt is lithium hexafluorophosphate (LiPF)6)。
When only two components of the lithium salt and the ionic liquid are contained in the solute, the molar ratio of the lithium salt to the ionic liquid is 1.0: 1.4.
When the solute comprises three components of lithium salt, ionic liquid and lithium fluoride, the molar ratio of the lithium salt to the ionic liquid to the lithium fluoride is 1.0:1.4 (1.3-5.1), and the optimal value is 1.0:1.4: 4.0.
The preparation method of the lithium ion battery electrolyte comprises the following steps:
(1) respectively weighing ethylene carbonate, methyl ethyl carbonate, dimethyl carbonate, fluoroethylene carbonate and dimethyl sulfoxide according to the using amount of each component in the organic solvent, and then mixing to obtain the organic solvent;
(2) weighing the components according to the using amount of the components in the solute;
(3) and putting each component in the solute into an organic solvent, wherein:
in the step (3), if the solute is formed by mixing lithium salt and ionic liquid, firstly adding lithium salt into the organic solvent, stirring for 30min at a stirring speed of 60r/min, standing for 24h, and then adding the ionic liquid into the organic solvent.
In the step (3), if the solute is formed by mixing lithium salt, ionic liquid and lithium fluoride, firstly adding the lithium salt into the solvent, stirring for 30min at a stirring speed of 60r/min, and then standing for 24 h; then adding ionic liquid into the organic solvent, stirring for 30min at a stirring speed of 60r/min, and standing for 24 h; finally, lithium fluoride is added to the solvent.
Compared with the prior art, the invention has the advantages that:
1. the invention utilizes LiPF6And N-octyl pyridine tetrafluoroborate ionic liquid as solute salt and lithium fluoride are co-dissolved in the composite solvent, due to competition between cations of the ionic liquid and lithium ion cations and electron-withdrawing effect of pyridine amino in the cations of the ionic liquid, the solvation number of solvent molecules coordinated to the lithium ions in the electrolyte is changed, and further the film forming mechanism of the surface of the graphite electrode is changed, and due to LiCoO2And the ionic liquid and graphite have better adsorbability, and the ionic liquid participates in the coaction to form a thin and compact SEI film on the surface of the graphite electrode, so that the internal resistance of the battery is reduced, the capacity retention rate of the battery is improved, and the cycle performance of the battery is improved.
2. Lithium fluoride can inhibit LiPF6On the other hand, the conductivity of the electrolyte can be increased, so that the following reactions proceed to the left: LiPF6(s)+H2O(g)→LiF(s)+OPF3(g) +2hf (g), whereby the conductivity properties of the electrolyte can be improved.
3. The ionic liquid and the lithium fluoride have convenient sources, the electrolyte has stable property, the preparation is simple, the conductivity is obviously improved, and the heat-resistant stability of the lithium ion battery electrolyte is enhanced, so the electrolyte has potential application prospect.
Drawings
FIG. 1 is a graph of conductivity versus time at different times when the solute of the present invention is composed of lithium salt, ionic liquid, and lithium fluoride, wherein the molar ratio of lithium salt, ionic liquid, and lithium fluoride in (a) is 1.0:1.4:5.1, and the molar ratio of lithium salt, ionic liquid, and lithium fluoride in (b) is 1.0:1.4: 1.3.
Detailed Description
Comparative example
Ethylene carbonate, methyl ethyl carbonate, dimethyl carbonate, fluoroethylene carbonate, dimethyl sulfoxide
Firstly, ethylene carbonate (hereinafter abbreviated as EC), ethyl methyl carbonate (hereinafter abbreviated as EMC), dimethyl carbonate (hereinafter abbreviated as DMC), fluoroethylene carbonate (hereinafter abbreviated as FEC) and dimethyl sulfoxide (hereinafter abbreviated as DMSO) are respectively subjected to molecular sieve drying or calcium hydride drying to remove trace moisture.
The electrolyte of the invention is prepared in a glove box, and the main components of the electrolyte comprise an organic solvent and a solute. The organic solvent is EC, EMC, DMC, FEC and DMSO mixed solution. The lithium salt being LiPF6The molar concentration of the lithium salt in the organic solvent is 1.0mo1/L, and the preparation method of the lithium ion battery electrolyte comprises the following steps:
weighing stoichiometric lithium salt LiPF according to the molar concentration of the electrolyte6Dissolving in a certain volume of EC/EMC/DMC/DMSO (volume ratio of 1.0:1.0:1.0 (0.1-0.5)) and FEC (3% wt) mixed solvent, stirring and mixing uniformly at 25 deg.C, standing to dissolve solute in organic solvent. The electrolyte of this comparative example was measured to have a conductivity of 6.45mScm-1。
In the above comparative example, the solute consists of lithium salt LiPF only6The conductivity of the electrolyte thus obtained was 6.45mScm-1As controls with several subsequent examples.
Example 1
Firstly, EC, EMC, DMC, FEC and DMSO are respectively dried by molecular sieve or calcium hydride to remove trace moisture.
The electrolyte of the invention is prepared in a glove box, and the main components of the electrolyte comprise an organic solvent and a solute. The organic solvent is EC, EMC, DMC, FEC and DMSO mixed solution. The solute is lithium salt and ionic liquid, wherein the lithium salt is LiPF6The ionic liquid is N-octyl pyridine tetrafluoroborate with the molar concentration of 1.4mol
In the solute, the molar concentration of the lithium salt in the organic solvent is 1.0mo1/L, the molar concentration of the N-octylpyridinium tetrafluoroborate (solute molar concentration) is 1.4mo1/L, and the total molar number of the solute is 2.4mo 1/L.
The preparation method of the lithium ion battery electrolyte comprises the following steps:
weighing stoichiometric LiPF according to the molar concentration of the electrolyte6And NThe-octyl pyridine tetrafluoroborate is dissolved in a certain volume of EC/EMC/DMC/DMSO (volume ratio is 1.0:1.0:1.0 (0.1-0.5)) and FEC (3% wt) mixed solvent in sequence at different time, fully stirred and uniformly mixed at 25 ℃, and kept stand to dissolve solute in the organic solvent.
The conductivity (mScm) of the electrolyte at different times in this example was measured in sequence-1) A, b, c and d have values of 6.45, 5.61, 5.31 and 4.92, respectively; wherein a is obtained according to the comparative example and has an initial conductivity of 6.45mScm for lithium salt only-1(ii) a b. c and d are the decrease after addition of the ionic liquid (N-octylpyridinium tetrafluoroborate). Conductivity of 6.45mScm obtained by the present example and comparative example-1In contrast, this example shows that the addition of the ionic liquid inhibits the conductivity of the electrolyte, resulting in a drop to 4.92mScm-1。
Example 2
Firstly, EC, EMC, DMC, FEC and DMSO are respectively dried by molecular sieve or calcium hydride to remove trace moisture.
The electrolyte of the invention is prepared in a glove box, and the main components of the electrolyte comprise an organic solvent and a solute. Wherein the organic solvent is a mixed solution of EC/EMC/DMC/DMSO (volume ratio of 1.0:1.0:1.0 (0.1-0.5)) and FEC (3% wt). The solute comprises lithium salt, ionic liquid and lithium fluoride, and the lithium salt is LiPF6The ionic liquid is N-octyl pyridine tetrafluoroborate, the molar ratio of the lithium salt to the ionic liquid to the lithium fluoride is 1.0:1.4:5.1, and the total molar concentration of the lithium salt to the ionic liquid to the lithium fluoride in the solute is 7.5mo 1/L.
The preparation method of the lithium ion battery electrolyte comprises the following steps:
And 2, weighing stoichiometric lithium fluoride according to the molar concentration of the electrolyte and the molar ratio of the lithium salt, the ionic liquid and the lithium fluoride, and dissolving the stoichiometric lithium fluoride in the mixed solution. In the process of putting lithium fluoride, stirring is carried out for 30min and standing is carried out for 24 h.
And 3, fully stirring and uniformly mixing the solution, and standing.
As shown in FIG. 1 (a), the conductivity (mScm) of the electrolyte was measured for different periods of time in this example-1) A, b, c, d, e, f and g have values of 6.45, 5.61, 5.31, 4.93, 5.06, 5.10 and 5.82, respectively; wherein a is the initial conductivity when only lithium salt is contained, and b, c and d are the drop values after the ionic liquid is added; e. f and g are the conductivity of the electrolyte after lithium fluoride is added; in LiPF6In solution, conductivity was from 6.45mScm when N-octyl pyridine tetrafluoroborate was added-1Down to 4.93mScm-1After the LiF is continuously added, the conductivity of the electrolyte rises to 5.82mScm-1。
Example 3
Firstly, respectively drying EC, EMC, DMC, FEC and DMSO by molecular sieves or calcium hydride to remove trace moisture;
the electrolyte of the invention is prepared in a glove box, and the main components of the electrolyte comprise an organic solvent and a solute. The organic solvents were EC/EMC/DMC/DMSO (volume ratio 1.0:1.0:1.0 (0.1-0.5)) and FEC (3% wt). The solute comprises lithium salt, ionic liquid and lithium fluoride, and the lithium salt is LiPF6The ionic liquid is N-octyl pyridine tetrafluoroborate; the molar ratio of the lithium salt, the ionic liquid and the lithium fluoride is 1.0:1.4:1.3, and the total molar concentration of the lithium salt, the ionic liquid and the lithium fluoride in the solute is 3.7mo 1/L.
The preparation method of the lithium ion battery electrolyte comprises the following steps:
step 1: drying and dehydrating EC, EMC, DMC, FEC and DMSO solvents by molecular sieve or calcium hydride respectively;
step 2: weighing stoichiometric LiPF according to the molar concentration of the electrolyte and the molar ratio of the lithium salt to the ionic liquid6Sequentially dissolving N-octyl pyridine tetrafluoroborate in a certain volume of EC/EMC/DMC/DMSO (volume ratio is 1.0:1.0:1.0 (0.1-0.5)) and FEC (3% wt)) solvent according to different time, stirring and mixing uniformly, and standing;
and step 3: according to the molar concentration of the electrolyte and the molar ratio of the lithium salt, the ionic liquid and the lithium fluoride; weighing stoichiometric lithium fluoride at different time, dissolving the stoichiometric lithium fluoride in the mixed solution, stirring and mixing uniformly, and standing;
and 4, step 4: the solution is stirred and left for a period of time.
As shown in FIG. 1 (b), the conductivity (mScm) of the electrolyte was measured for different periods of time in this example-1) A, b, c, d, e, f, g and h have values of 6.45, 5.62, 5.32, 4.92, 5.07, 5.31, 5.75 and 5.95mScm-1(ii) a Wherein a is the conductivity of the electrolyte after lithium salt is added; b. c, d and e are the conductivity of the electrolyte after the ionic liquid is added, and f, g and h are the conductivity of the electrolyte after the lithium fluoride is added; in LiPF6In solution, conductivity was from 6.45mScm when N-octyl pyridine tetrafluoroborate was added-1Down to 4.92mScm-1After the LiF is continuously added, the conductivity of the electrolyte rises to 5.95mScm-1. Therefore, the conductivity of the lithium ion battery electrolyte can be obviously improved by the lithium fluoride.
The embodiments of the present invention are described only for the preferred embodiments of the present invention, and not for the limitation of the concept and scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the design concept of the present invention shall fall into the protection scope of the present invention, and the technical content of the present invention which is claimed is fully set forth in the claims.
Claims (8)
1. An electrolyte of a lithium ion battery, which is characterized by comprising an organic solvent and a solute, wherein the solute is dissolved in the organic solvent to form a solution with the molar concentration of 3.7-5.1mo1/L, and the electrolyte comprises:
the organic solvent is composed of five components of ethylene carbonate, methyl ethyl carbonate, dimethyl carbonate, fluoroethylene carbonate and dimethyl sulfoxide, wherein the fluoroethylene carbonate is dissolved in the other four components to obtain a mixed solution, the volume ratio of the ethylene carbonate, the methyl ethyl carbonate, the dimethyl carbonate and the dimethyl sulfoxide in the organic solvent is 1.0:1.0:1.0 (0.1-0.5), and the weight percentage of the fluoroethylene carbonate in the organic solvent is 3 wt%;
the solute comprises two components of lithium salt and ionic liquid, wherein the ionic liquid is N-octyl pyridine tetrafluoroborate, and the cationic structural formula of the N-octyl pyridine tetrafluoroborate is as follows:
the anion structural formula in the N-octyl pyridine tetrafluoroborate is as follows:
the molar ratio of lithium salt to ionic liquid in the solute is 1.0: 1.4.
2. The electrolyte of a lithium ion battery according to claim 1, wherein the organic solvent is a mixed solution obtained by mixing ethylene carbonate, ethyl methyl carbonate, dimethyl carbonate, fluoroethylene carbonate, and dimethyl sulfoxide, which are respectively dehydrated, and then dissolving fluoroethylene carbonate in the remaining four components.
3. The electrolyte for a lithium ion battery according to claim 1, wherein the lithium salt is lithium hexafluorophosphate.
4. The electrolyte of the lithium ion battery according to claim 1, wherein the solute further comprises lithium fluoride, and the molar ratio of the lithium salt to the ionic liquid to the lithium fluoride is 1.0:1.4 (1.3-5.1).
5. A method for preparing the electrolyte of the lithium ion battery of any one of claims 1 to 4, which is characterized in that: the method comprises the following steps:
(1) respectively weighing ethylene carbonate, methyl ethyl carbonate, dimethyl carbonate, fluoroethylene carbonate and dimethyl sulfoxide according to the using amount of each component in the organic solvent, and then mixing to obtain the organic solvent;
(2) weighing the components according to the using amount of the components in the solute;
(3) and putting the components in the solute into an organic solvent, stirring at 23-27 ℃, and standing to completely dissolve the solute in the organic solvent to obtain the electrolyte.
6. The method for preparing the lithium ion battery electrolyte according to claim 5, wherein: in the step (3), if the solute is formed by mixing lithium salt and ionic liquid, firstly adding lithium salt into the organic solvent, then stirring for 30min, standing for 24h, and then adding ionic liquid into the organic solvent to form the solute.
7. The method for preparing the lithium ion battery electrolyte according to claim 5, wherein: in the step (3), if the solute is formed by mixing lithium salt, ionic liquid and lithium fluoride, firstly, adding the lithium salt into the solvent, stirring for 30min, and then standing for 24 h; then adding ionic liquid into the organic solvent, stirring for 30min, and standing for 24 h; finally, lithium fluoride is added to the solvent.
8. The method for preparing the lithium ion battery electrolyte according to claim 5, wherein: the stirring speed in the step (3) is 60 r/min.
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