CN104934639A - Preparation method of lithium ion battery electrolyte solution - Google Patents
Preparation method of lithium ion battery electrolyte solution Download PDFInfo
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- CN104934639A CN104934639A CN201510209907.3A CN201510209907A CN104934639A CN 104934639 A CN104934639 A CN 104934639A CN 201510209907 A CN201510209907 A CN 201510209907A CN 104934639 A CN104934639 A CN 104934639A
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- lithium
- salt
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- sodium
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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
- H01M10/058—Construction or manufacture
-
- 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
- H01M2300/00—Electrolytes
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a lithium ion battery electrolyte solution and a preparation method thereof. The solvent of the lithium ion battery electrolyte can be water or an organic solvent, and contains lithium salt and an additive; the content of the additive accounts for 0.01% to 20% of the total weight of the electrolyte lithium salt; and the lithium ion battery electrolyte is particularly suitable for a water system or organic system lithium ion battery using a lithium manganese oxide or lithium-rich manganese based material as a cathode. The special electrolyte salt additive is introduced, so that comprehensive performance of the electrolyte is improved, the specific discharge capacity of the lithium ion battery using the lithium manganese oxide or lithium-rich manganese based material as the cathode is obviously increased, high coulombic efficiency and long cycle stability are maintained, and the internal resistance of the battery is reduced to a certain extent. Moreover, the lithium ion battery electrolyte can enable the lithium ion battery using the lithium manganese oxide or lithium-rich manganese based material as the cathode to be of good overcharging performance.
Description
Technical field
The invention belongs to Electrochemical Engineering and commercial plant field, belong to lithium ion battery electrolyte aspect, relate to a kind of preparation method of lithium ion battery electrolyte solution more specifically, for the lithium ion battery being positive pole with manganese oxide lithium, lithium-rich manganese base material etc.
Background technology
Be developed so far, low capacity organolithium ion battery has possessed good conditions for sports industry.In recent years, safety, inexpensive aquo-lithium ion battery are also subject to extensive concern.Aquo-lithium ion battery electrode material is mostly based on the research of organic lithium ion battery material, and the feature in conjunction with aqueous electrolyte is introduced and improved.In numerous anode material for lithium-ion batteries, spinel-type LiMn
2o
4there is the desirable main body of Lithium-ion embeding/deviate from, promoter manganese enriches, environmental friendliness, low price, overcharging resisting, security performance are good, and the advantage such as structure remained stable, is able to commercialization extensive use, and becomes the positive electrode of aquo-lithium ion battery most application prospect in charge and discharge cycles process.
But, spinelle LiMn
2o
4for lower (the theoretical capacity 148mAh g of energy density during stoichiometric proportion
-1, actual discharge capacity 100 ~ 120mAh g
-1), due to Jahn-Teller distortion can be there is in charge and discharge process, cause structure progressively to be caved in circulation; And disproportionated reaction can occur material in the electrolytic solution and Mn dissolves, cause capacitance loss serious, cycle performance is poor, and especially under high temperature, capacity attenuation is very fast.For aquo-lithium ion battery, spinelle LiMn
2o
4capacity fade problem exists and more outstanding equally, is that in the aqueous solution, the solvation degree of lithium is high because metal ion is soluble by the effect of polar water molecules on the one hand; On the other hand owing to analysing the impact of oxygen side reaction.
In recent years, with Li
2mnO
3based on composite positive pole Li
2mnO
3-LiMO
2(M=Co, Ni, Fe, Ni
0.5mn
0.5) receive the concern of researcher.Relative to spinel-type LiMn
2o
4or pure layered lithium manganese oxide LiMnO
2, the Li/Mn mol ratio of this type of material is all more than 2, and magnesium-yttrium-transition metal is based on Mn, is therefore called stratiform lithium-rich manganese base material.Due to many LiMO
2with Li
2mnO
3mostly be isomorphism thing, generally use LiMO
2(M=Co, Ni, Fe, Ni
0.5mn
0.5deng) material and Li
2mnO
3compound, makes it to form solid solution, obtains Li
2mnO
3with other nonwoven fabric from filaments LiMO
2composite material.These composite positive poles have the good characteristic of high potential, height ratio capacity and high-energy-density, but the relative spinelle LiMn of this type of stratiform lithium-rich manganese base material
2o
4, capacity attenuation is even more serious.Along with people are to the understanding of positive electrode and electrolyte interface importance, LiMn2O4 and stratiform lithium-rich manganese base material surface modified be the focus paid close attention to of people and study hotspot always, but the problem of capacity attenuation is not able to basic solution.
Researcher, for the research of organic lithium-ion battery electrolytes, mainly concentrates on organic solvent, additive and lithium salts electrolyte, to improve ionic conductivity, the stability of electrolyte and to widen stable electrochemical window.And for the research of aquo-lithium ion battery electrolyte, also only pay close attention to the comparison of different inorganic lithium salt character.So far there are no from the angle changing liquid electrolytic fluid component, to significantly improve the report of electrode material capacity and long circulating stability.
The invention provides a kind of preparation method of lithium ion battery electrolyte solution, by adding cationic additive in the electrolytic solution, the specific capacity of manganese cathode material and cyclical stability are significantly improved, contribute to the specific energy and the cycle life that improve water system and organic system lithium ion battery, have the advantages that cost is low, effectiveness is high, have broad application prospects in the energy storage such as electric tool, electric motor car, electrical network.
Summary of the invention
The object of the present invention is to provide a kind of lithium ion battery electrolyte solution and preparation method, to solve the problem of LiMn2O4 and low, the long-term cycle performance difference of manganese cathode material specific capacity such as lithium-rich manganese-based.Technical problem solved by the invention realizes by the following technical solutions:
The preparation method of lithium ion battery electrolyte solution of the present invention is as follows: 1, a kind of preparation method of lithium ion battery electrolyte solution, it is characterized in that this preparation method's step is as follows:
Electrolyte solution is by lithium salts, cation salt form additive and solvent composition, lithium salts and cation salt form additive dissolve in a solvent, wherein cation salt form additive is more than one in zinc salt, magnesium salts, calcium salt, strontium salt, sodium salt, sylvite, rubidium salt, cesium salt, manganese salt, cobalt salt, nickel salt, mantoquita, aluminium salt, gallium salt and indium salt, cation salt form additive level accounts for 0.01 ~ 20% of electrolyte lithium salt, and the total concentration of lithium salts is in 0.2 ~ 3 mol/L;
Described solvent is more than one in water, N-METHYLFORMAMIDE, DMF and acetonitrile, linear carbonate, cyclic carbonate, carboxylate, chain ether, cyclic ether, ethylene carbonate, propene carbonate, gamma-butyrolacton, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dimethoxymethane, dimethoxy-ethane, diethoxyethane, oxolane, 2-methyltetrahydrofuran, ethyl acetate, methyl butyrate;
Lithium salts is lithium sulfate, lithium chloride, lithium nitrate, lithium acetate, lithium hexafluoro phosphate, hexafluoroarsenate lithium, lithium perchlorate, LiBF4, LiCF
3sO
3, LiN (CF
3sO
2)
2, LiN (R
foSO
2)
2, LiC (SO
2cF
3)
3in more than one;
The anion that cation salt form additive is corresponding is sulfate radical, chlorine root, fluorine root, nitrate anion, acetate, hexafluoro-phosphate radical, hexafluoroarsenate root, perchlorate, tetrafluoroborate, CF
3sO
3root, N (CF
3sO
2)
2root, N (R
foSO
2)
2root, C (SO
2cF
3)
3more than one in root.
When this electrolyte solution is used for sodium metal or sodium ion to embed/deviate from material is the battery of negative pole, add sodium salt 0.2 ~ 3 mol/L in this electrolyte solution, sodium salt is sodium sulphate, sodium chloride, sodium fluoride, sodium nitrate, sodium acetate, sodium hexafluoro phosphate, hexafluoroarsenate sodium, sodium perchlorate, sodium tetrafluoroborate, NaCF
3sO
3, NaN (CF
3sO
2)
2, NaN (R
foSO
2)
2, NaC (SO
2cF
3)
3in more than one.
When this electrolyte solution is used for metallic zinc or zinc ion to embed/deviate from material is the battery of negative pole, add zinc salt 0.2 ~ 3 mol/L in this electrolyte solution, zinc salt is zinc sulfate, zinc chloride, zinc fluoride, zinc nitrate, zinc acetate, hexafluorophosphoric acid zinc, hexafluoroarsenate zinc, zinc perchlorate, tetrafluoro boric acid zinc, Zn (CF
3sO
3)
2, ZnN [(CF
3sO
2)
2]
2, Zn [N (R
foSO
2)
2]
2, Zn [C (SO
2cF
3)
3]
2in more than one.
When this electrolyte solution is used for metallic potassium or potassium ion to embed/deviate from material is the battery of negative pole, add sylvite 0.2 ~ 3 mol/L in this electrolyte solution, sylvite is potassium sulfate, potassium chloride, potassium fluoride, potassium nitrate, potassium acetate, Potassium Hexafluorophosphate, potassium hexafluoroarsenate, potassium hyperchlorate, potassium tetrafluoroborate, KCF
3sO
3, KN (CF
3sO
2)
2, KN (R
foSO
2)
2, KC (SO
2cF
3)
3in more than one.
When this electrolyte solution is used for magnesium metal or magnesium ion to embed/deviate from material is the battery of negative pole, add sodium salt 0.2 ~ 3 mol/L in this electrolyte solution, magnesium salts is magnesium sulfate, magnesium chloride, magnesium fluoride, magnesium nitrate, magnesium acetate, hexafluorophosphoric acid magnesium, hexafluoroarsenate magnesium, magnesium perchlorate, tetrafluoro boric acid magnesium, Mg (CF
3sO
3)
2, Mg [N (CF
3sO
2)
2]
2, Mg [N (R
foSO
2)
2]
2, Mg [C (SO
2cF
3)
3]
2in more than one.
In the present invention, the action principle introducing cation salt form additive is that the cation introduced can embed in manganese base battery material lattice by trace, thus contribute to significantly reducing the embedding of lithium ion in lattice/deviate from potential barrier, improve Lithium-ion embeding/deviate from speed and quantity, thus specific capacity is constantly increased.Our research finds, multiple cation can be worked in coordination with trace and be embedded in manganese base battery material lattice, makes the effect of improvement stability and raising specific capacity better.
Beneficial effect of the present invention: by introducing cation salt form additive, improve the combination property of manganese cathode material, the lithium ion battery specific discharge capacity that to make with LiMn2O4 or the material such as lithium-rich manganese-based be positive pole increases 2 ~ 4 times than existing positive electrode, reach the specific capacity of 300 ~ 700mAh/g, and keep the long-term cyclical stability of more than 95% high coulombic efficiency and more than 1000 times, internal resistance of cell decrease to some degree simultaneously.In addition, the lithium ion battery that to use the lithium ion battery electrolyte solution prepared of the present invention can make with LiMn2O4 or the material such as lithium-rich manganese-based be positive pole has good overcharging resisting performance.
Accompanying drawing explanation
Fig. 1 is containing ZnSO to the lithium-rich manganese base material of electrode with zinc
4li
2sO
4typical charging and discharging curve in the aqueous solution
Fig. 2 is containing ZnSO to the lithium-rich manganese base material of electrode with zinc
4li
2sO
4cycle performance in the aqueous solution
Embodiment
Embodiment 1
(H in the glove box of high-purity argon gas is full of in drying
2o < 5ppm; O
2< 2ppm), by each organic solvent (neat solvent after dewatering) according to EC: DMC: EA=1: 1: 1 (wt.%) weighing, mixing in proportion.Lithium hexafluoro phosphate (LiPF
6, after dewatering), take 1.0 moles; Zinc salt Zn (BF
4)
2(after dewatering), takes 1.0 moles; Cation salt form additive Mg (BF
4)
2(after dewatering), takes 0.01 mole; Cation salt form additive NaClO
4(after dewatering), takes 0.01 mole; Cation salt form additive KClO
4(after dewatering), takes 0.01 mole.Get the above-mentioned mixed solvent 800ml mixed, add this 800ml mixed solvent successively, full and uniform stirring, dissolving by the various salt amounts of above-mentioned weighing, then add the above-mentioned mixed solvent mixed with constant volume to 1000ml.Namely lithium ion battery electrolyte solution of the present invention is obtained, the organic system lithium ion battery (negative pole is that metallic zinc or zinc embed/deviate from class material) that to can be used for LiMn2O4 or the material such as lithium-rich manganese-based be positive pole.
Embodiment 2
(H in the glove box of high-purity argon gas is full of in drying
2o < 5ppm; O
2< 2ppm), by each organic solvent (neat solvent after dewatering) according to EC: DME=1: 1 (wt.%) weighing, mixing in proportion.Lithium hexafluoro phosphate (LiPF
6, after dewatering), take 1.0 moles; Sodium hexafluoro phosphate (NaPF
6, after dewatering), take 1.0 moles; Cation salt form additive Mg (BF
4)
2(after dewatering), takes 0.01 mole; Cation salt form additive Mn (ClO
4)
2(after dewatering), takes 0.01 mole; Cation salt form additive KClO
4(after dewatering), takes 0.01 mole.Get the above-mentioned mixed solvent 800ml mixed, add this 800ml mixed solvent successively, full and uniform stirring, dissolving by the various salt amounts of above-mentioned weighing, then add the above-mentioned mixed solvent mixed with constant volume to 1000ml.Namely lithium ion battery electrolyte solution of the present invention is obtained, the organic system lithium ion battery (negative pole is that sodium metal or sodium embed/deviate from class material) that to can be used for LiMn2O4 or the material such as lithium-rich manganese-based be positive pole.
Embodiment 3
(H in the glove box of high-purity argon gas is full of in drying
2o < 5ppm; O
2< 2ppm), by each organic solvent (neat solvent after dewatering) according to EC: DMC=1: 1 (wt.%) weighing, mixing in proportion.Lithium hexafluoro phosphate (LiPF
6, after dewatering), take 1.0 moles; Cation salt form additive sodium hexafluoro phosphate (NaPF
6, after dewatering), take 0.01 mole; Cation salt form additive Mg (BF
4)
2(after dewatering), takes 0.01 mole; Cation salt form additive Mn (ClO
4)
2(after dewatering), takes 0.01 mole; Cation salt form additive KClO
4(after dewatering), takes 0.01 mole.Get the above-mentioned mixed solvent 800ml mixed, add this 800ml mixed solvent successively, full and uniform stirring, dissolving by the various salt amounts of above-mentioned weighing, then add the above-mentioned mixed solvent mixed with constant volume to 1000ml.Namely lithium ion battery electrolyte solution of the present invention is obtained, the organic system lithium ion battery (negative pole is that lithium metal or lithium embed/deviate from class material) that to can be used for LiMn2O4 or the material such as lithium-rich manganese-based be positive pole.
Embodiment 4
In air, solvent is deionized water; Lithium sulfate, takes 1.0 moles; Zinc sulfate, takes 0.5 mole; Cation salt form additive MgSO
4, take 0.01 mole; Cation salt form additive MnSO
4, take 0.01 mole; Cation salt form additive Na
2sO
4, take 0.01 mole; Cation salt form additive K
2sO
4, take 0.01 mole.Get above-mentioned deionized water 800ml, add in this 800ml deionized water successively by the various salt amounts of above-mentioned weighing, full and uniform stirring, dissolving, then add the above-mentioned mixed solvent mixed with constant volume to 1000ml.Namely lithium ion battery electrolyte solution of the present invention is obtained, the aquo-lithium ion battery (negative pole is that metallic zinc or zinc embed/deviate from class material) that to can be used for LiMn2O4 or the material such as lithium-rich manganese-based be positive pole.
Embodiment 5
In air, solvent is deionized water; Lithium sulfate, takes 1.5 moles; Cation salt form additive MgSO
4, take 0.01 mole; Cation salt form additive NiSO
4, take 0.01 mole; Cation salt form additive Ga
2(SO
4)
3, take 0.01 mole; Cation salt form additive A l
2(SO
4)
3, take 0.01 mole; Cation salt form additive MnSO
4, take 0.01 mole; Cation salt form additive Na
2sO
4, take 0.01 mole; Cation salt form additive K
2sO
4, take 0.01 mole.Get above-mentioned deionized water 800ml, add in this 800ml deionized water successively by the various salt amounts of above-mentioned weighing, full and uniform stirring, dissolving, then add the above-mentioned mixed solvent mixed with constant volume to 1000ml.Namely lithium ion battery electrolyte solution of the present invention is obtained, the aquo-lithium ion battery (negative pole is that lithium embeds/deviate from class material) that to can be used for LiMn2O4 or the material such as lithium-rich manganese-based be positive pole.
The effect of above embodiment: above-mentioned technical process prepares lithium-ion battery electrolytes, the combination property of lithium-ion battery electrolytes is improve by introducing additive, make to be that the water system of positive pole and organolithium ion battery specific discharge capacity significantly improve with lithium-rich manganese base material, reach 300 ~ 700mAh g
-1, and keep the long-term cyclical stability of more than 95% high coulombic efficiency and more than 1000 times.
Claims (5)
1. a preparation method for lithium ion battery electrolyte solution, is characterized in that this preparation method's step is as follows:
Electrolyte solution is by lithium salts, cation salt form additive and solvent composition, lithium salts and cation salt form additive dissolve in a solvent, wherein cation salt form additive is more than one in zinc salt, magnesium salts, calcium salt, strontium salt, sodium salt, sylvite, rubidium salt, cesium salt, manganese salt, cobalt salt, nickel salt, mantoquita, aluminium salt, gallium salt and indium salt, cation salt form additive level accounts for 0.01 ~ 20% of electrolyte lithium salt, and the total concentration of lithium salts is in 0.2 ~ 3 mol/L;
Described solvent is more than one in water, N-METHYLFORMAMIDE, DMF and acetonitrile, linear carbonate, cyclic carbonate, carboxylate, chain ether, cyclic ether, ethylene carbonate, propene carbonate, gamma-butyrolacton, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dimethoxymethane, dimethoxy-ethane, diethoxyethane, oxolane, 2-methyltetrahydrofuran, ethyl acetate, methyl butyrate;
Lithium salts is lithium sulfate, lithium chloride, lithium nitrate, lithium acetate, lithium hexafluoro phosphate, hexafluoroarsenate lithium, lithium perchlorate, LiBF4, LiCF
3sO
3, LiN (CF
3sO
2)
2, LiN (R
foSO
2)
2, LiC (SO
2cF
3)
3in more than one;
The anion that cation salt form additive is corresponding is sulfate radical, chlorine root, fluorine root, nitrate anion, acetate, hexafluoro-phosphate radical, hexafluoroarsenate root, perchlorate, tetrafluoroborate, CF
3sO
3root, N (CF
3sO
2)
2root, N (R
foSO
2)
2root, C (SO
2cF
3)
3more than one in root.
2. the preparation method of a kind of lithium ion battery electrolyte solution according to claim 1, it is characterized in that: when this electrolyte solution is used for sodium metal or sodium ion to embed/deviate from material be the battery of negative pole, add sodium salt 0.2 ~ 3 mol/L in this electrolyte solution, sodium salt is sodium sulphate, sodium chloride, sodium fluoride, sodium nitrate, sodium acetate, sodium hexafluoro phosphate, hexafluoroarsenate sodium, sodium perchlorate, sodium tetrafluoroborate, NaCF
3sO
3, NaN (CF
3sO
2)
2, NaN (R
foSO
2)
2, NaC (SO
2cF
3)
3in more than one.
3. the preparation method of a kind of lithium ion battery electrolyte solution according to claim 1, it is characterized in that: when this electrolyte solution is used for metallic zinc or zinc ion to embed/deviate from material be the battery of negative pole, add zinc salt 0.2 ~ 3 mol/L in this electrolyte solution, zinc salt is zinc sulfate, zinc chloride, zinc fluoride, zinc nitrate, zinc acetate, hexafluorophosphoric acid zinc, hexafluoroarsenate zinc, zinc perchlorate, tetrafluoro boric acid zinc, Zn (CF
3sO
3)
2, ZnN [(CF
3sO
2)
2]
2, Zn [N (R
foSO
2)
2]
2, Zn [C (SO
2cF
3)
3]
2in more than one.
4. the preparation method of a kind of lithium ion battery electrolyte solution according to claim 1, it is characterized in that: when this electrolyte solution is used for metallic potassium or potassium ion to embed/deviate from material be the battery of negative pole, add sylvite 0.2 ~ 3 mol/L in this electrolyte solution, sylvite is potassium sulfate, potassium chloride, potassium fluoride, potassium nitrate, potassium acetate, Potassium Hexafluorophosphate, potassium hexafluoroarsenate, potassium hyperchlorate, potassium tetrafluoroborate, KCF
3sO
3, KN (CF
3sO
2)
2, KN (R
foSO
2)
2, KC (SO
2cF
3)
3in more than one.
5. the preparation method of a kind of lithium ion battery electrolyte solution according to claim 1, it is characterized in that: when this electrolyte solution is used for magnesium metal or magnesium ion to embed/deviate from material be the battery of negative pole, add sodium salt 0.2 ~ 3 mol/L in this electrolyte solution, magnesium salts is magnesium sulfate, magnesium chloride, magnesium fluoride, magnesium nitrate, magnesium acetate, hexafluorophosphoric acid magnesium, hexafluoroarsenate magnesium, magnesium perchlorate, tetrafluoro boric acid magnesium, Mg (CF
3sO
3)
2, Mg [N (CF
3sO
2)
2]
2, Mg [N (R
foSO
2)
2]
2, Mg [C (SO
2cF
3)
3]
2in more than one.
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