CN109946366A - The measuring method of metal impurities in lithium-ion battery electrolytes - Google Patents
The measuring method of metal impurities in lithium-ion battery electrolytes Download PDFInfo
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Abstract
The invention discloses a kind of measuring methods of metal impurities in lithium-ion battery electrolytes, metal impurities include K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn, include the following steps, one, configuration standard solution, standard solution include Li, K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn element;Two, testing sample solution is taken, diluent solution dilutes testing sample solution;Three, using inductive coupling plasma emission spectrograph, the diluted multiple of concentration value, testing sample solution of standard solution is inputted respectively, sequentially determining analysis margin, standard solution and testing sample solution, using diluent solution as analysis margin, using the curve of the standard solution of measurement as standard curve, the content (ppm) of K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn in testing sample solution are calculated using external standard method.The present invention has the advantages that accuracy is good, it is at low cost.
Description
Technical field
The present invention relates to the measuring methods of metal impurities in lithium-ion battery electrolytes.
Background technique
It include lithium salts and organic component etc. in lithium-ion battery electrolytes, wherein organic component is one or more carbonic esters
The novel organic matter of class, carboxylic acid esters and boracic, sulfur-bearing, phosphorous etc.;Lithium salts therein is the electrolysis of one or more elemental lithiums
Matter, including LiPF6(lithium hexafluoro phosphate), LiBF4(single oxalic acid is double by (LiBF4), LiBOB (dioxalic acid lithium borate), LiODFB
Lithium fluoroborate), LiFSI (double fluorine sulfimide lithiums) etc..
Lithium-ion battery electrolytes are the important components of lithium ion battery, carry between positive and negative anodes and pass in the battery
The performances such as the operating temperature, cycle efficieny, safety of battery are played great influence by the effect of transmission of electricity lotus.Lithium ion battery battery
The height of metals content impurity plays conclusive effect to the performance of lithium ion battery in solution liquid.Therefore lithium ion battery electrolysis
The measurement of metal impurities is of crucial importance in liquid.Metal impurities generally comprise in lithium-ion battery electrolytes: K, Na, Fe, Ca, Pb,
Cu, Cr, Ni, Al, Zn etc..
The measurement of metal impurities mainly uses inductive coupling plasma emission spectrograph in lithium-ion battery electrolytes
(ICP).It is measured and is had the following problems using inductive coupling plasma emission spectrograph at present: one, lithium-ion electric to be measured
Pond electrolyte needs to carry out pre-treatment using pure water acid adding system or a purely organic system or micro-wave digestion mode, using pure water acid adding
When system, the organic component dissolubility in lithium-ion battery electrolytes is poor, leads to Lower result;When using a purely organic system, this
Height is required to inductive coupling plasma emission spectrograph, needs to be equipped with specialized equipment accessory, this results in cost of determination high,
It is poor additionally, due to dissolubility of the beavy metal impurity in a purely organic system, this make a purely organic system to the lithiums of complicated components from
Sub- battery electrolyte does not have preferable applicability, to cause measurement result relatively low yet;Using micro-wave digestion, then require in addition to match
Microwave dissolver is set, it is at high cost.Two, when being measured using ICP, required standard solution usually only comprising K, Na, Fe, Ca, Pb,
The element to be measured such as Cu, Cr, Ni, Al, Zn, however a large amount of electricity that the lithium salts of lithium-ion battery electrolytes middle and high concentration to be measured ionizes out
Son, can inhibit the ionization of K, Na, thus inductive coupling plasma emission spectrograph with above-mentioned standard solution measurement lithium from
The result of K, Na for obtaining when sub- battery electrolyte then can be higher.
Summary of the invention
The object of the present invention is to provide the measurement sides of metal impurities in a kind of good lithium-ion battery electrolytes of accuracy
Method.
To achieve the above object, the technical solution adopted by the present invention is that: the survey of metal impurities in lithium-ion battery electrolytes
Determine method, metal impurities include K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn, it is characterised in that: include the following steps, one, match
Standard solution is set, standard solution includes Li, K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn element;Two, take sample to be tested molten
Liquid dilutes testing sample solution with diluent solution, and diluent solution is the mixed solution of nitric acid, ethyl alcohol and deionized water;Three,
Using inductive coupling plasma emission spectrograph, diluted times of concentration value, testing sample solution of standard solution is inputted respectively
Number, sequentially determining analysis margin, standard solution and testing sample solution, using diluent solution as analysis margin, with measurement
Standard solution curve as standard curve, using external standard method calculate K, Na in testing sample solution, Fe, Ca, Pb, Cu,
The content (ppm) of Cr, Ni, Al, Zn.
Further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein in diluent solution
The volume ratio of nitric acid, ethyl alcohol and deionized water is 5:25:70.
Further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein sample to be tested is molten
The diluted multiple of liquid is 25.
Still further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein diluent solution
Middle nitric acid grade is excellent pure grade (GR) or more, and ethyl alcohol is dehydrated alcohol.
Further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein standard solution includes
First standard solution, the second standard solution, third standard solution, Li/ in the first, second, third standard solution (K, Na, Fe,
Ca, Pb, Cu, Cr, Ni, Al, Zn) concentration be respectively as follows: 5.0000ppm/0.1000ppm, 10.0000ppm/0.2000ppm,
15.0000ppm/0.3000ppm。
Further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein standard solution
Configuration step is as follows: successively accurately weighed in the Polypropylene bottle of three 250mL on electronic balance 0.1000g,
0.2000g, 0.3000g concentration are that the complex element standard comprising K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn of 100ppm is molten
Liquid, it is 1000ppm's that 0.5000g, 1.0000g, 1.5000g concentration are then successively added in above-mentioned three Polypropylene bottles
Solution in three Polypropylene bottles is then diluted to 100g to get arriving with diluent solution by elemental lithium standard solution
The concentration of Li/ (K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn) is respectively 5.0000ppm/0.1000ppm, 10.0000ppm/
The first standard solution, the second standard solution, the third standard solution of 0.2000ppm, 15.0000ppm/0.3000ppm.
Still further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein complex element mark
The error range of quasi- solution concentration is 100 ± 0.3ppm, and the error range of elemental lithium concentration of standard solution is 1000 ± 3ppm.
Still further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein electronic balance
Precision is 0.0001g.
Still further, in lithium-ion battery electrolytes above-mentioned metal impurities measuring method, wherein the lithium from
Sub- battery electrolyte includes lithium salts and organic component, and wherein lithium salts is LiPF6(lithium hexafluoro phosphate), LiBF4(LiBF4),
One of LiBOB (dioxalic acid lithium borate), LiODFB (single oxalic acid double lithium fluoroborates), LiFSI (double fluorine sulfimide lithiums) or
A variety of, organic component is one or more carbonates, carboxylic acid esters and boracic, sulfur-bearing, phosphorous ester-based organic compound.
The invention has the advantages that using the measuring method of metal impurities in lithium-ion battery electrolytes of the present invention,
The dissolubility of lithium-ion battery electrolytes to be measured is good, while eliminating lithium-ion battery electrolytes middle and high concentration lithium salts pair to be measured
The accuracy of the interference of measurement, the metals content impurity determined is good.In addition, this method emits light to inductively coupled plasma body
The requirement of spectrometer (ICP) is relatively low, and without in addition configuring special accessory, analysis cost is low.
Specific embodiment
It elaborates below to the measuring method of metal impurities in lithium-ion battery electrolytes.
Lithium-ion battery electrolytes include lithium salts and organic component.Wherein lithium salts is LiPF6(lithium hexafluoro phosphate), LiBF4
(LiBF4), LiBOB (dioxalic acid lithium borate), LiODFB (the double lithium fluoroborates of single oxalic acid), LiFSI (double fluorine sulfimides
Lithium) one of or it is a variety of.Wherein organic component is one or more carbonates, carboxylic acid esters and boracic, sulfur-containing, phosphorus-containing
Ester-based organic compound, specifically include that DMC (dimethyl carbonate), DEC (diethyl carbonate), EMC (methyl ethyl carbonate), EC (carbonic acid
Vinyl acetate), PC (propene carbonate), EA (ethyl acetate), PP (propyl propionate), FEC (fluorinated ethylene carbonate), BP (connection
Benzene), VC (vinylene carbonate), PS (1,3- propane sultone), SN (succinonitrile), ESI (ethylene sulfite), BXZ (1,3-
Propene sultone), ESA (sulfuric acid vinyl ester), MMDS (methane-disulfonic acid methylene ester), TMSB (three (trimethyl silane) boric acid
Ester), TMSP (three (trimethyl silane) phosphates), the organic component in lithium-ion battery electrolytes is one such or more
Kind.
Metal impurities in lithium-ion battery electrolytes specifically include that K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn etc..
The measuring method of metal impurities, includes the following steps in lithium-ion battery electrolytes.
One, configuration standard solution, standard solution include Li, K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn element.Mark
The purpose that elemental lithium is added in quasi- solution is: overcoming lithium-ion battery electrolytes middle and high concentration lithium salts dry to the measurement of K, Na
It disturbs.The present embodiment Plays solution include the first standard solution, the second standard solution, third standard solution, the first standard solution,
Second standard solution, third standard solution constitute three gradients of standard solution.Li/ in first, second, third standard solution
The concentration of (K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn) is respectively 5.0000ppm/0.1000ppm, 10.0000ppm/
0.2000ppm、15.0000ppm/0.3000ppm。
The configuration step of standard solution is as follows: successively accurate in the Polypropylene bottle of three 250mL on electronic balance
Weighing 0.1000g, 0.2000g, 0.3000g concentration is the mixed comprising K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn of 100ppm
Elemental standard solution is closed, it is dense that 0.5000g, 1.0000g, 1.5000g are then successively added in above-mentioned three Polypropylene bottles
Degree is the elemental lithium standard solution of 1000ppm, is then diluted the solution in three Polypropylene bottles with diluent solution
To 100g to get being respectively 5.0000ppm/ to the concentration of Li/ (K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn)
The first standard solution of 0.1000ppm, 10.0000ppm/0.2000ppm, 15.0000ppm/0.3000ppm, the second standard are molten
Liquid, third standard solution.The error range of complex element concentration of standard solution is 100 ± 0.3ppm, and elemental lithium standard solution is dense
The error range of degree is 1000 ± 3ppm.The precision of electronic balance is 0.0001g.Complex element standard solution and elemental lithium mark
Quasi- solution is commercially available.
Two, testing sample solution is taken, testing sample solution is diluted with diluent solution, testing sample solution dilution
Multiple be preferably 25 times.It is good that the accuracy measured under the conditions of testing sample solution dilutes 25 times is obtained through long term test.
Diluent solution used in first, second step is the mixed solution of nitric acid, ethyl alcohol and deionized water, nitre
The volume ratio of acid, ethyl alcohol and deionized water is 5:25:70.Wherein nitric acid grade is excellent pure grade (GR) or more, and ethyl alcohol is anhydrous
Ethyl alcohol.
Three, using inductive coupling plasma emission spectrograph, the dense of the first, second, third standard solution is inputted respectively
The diluted multiple of angle value, testing sample solution, sequentially determining analysis margin, the first, second, third standard solution and to test sample
Product solution, using diluent solution as analysis margin, using the curve of the first, second, third standard solution of measurement as standard
Curve calculates the content (ppm) of K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn in testing sample solution using external standard method.
Different experiments are given below, the present invention is done and is further described in detail.
Experiment one
Observe the influence that high concentration lithium salts measures K, Na in lithium-ion battery electrolytes.
Configure K, Na complex element solution of various concentration.Due to metal impurities technical indicator in lithium-ion battery electrolytes
It is general to require are as follows:≤2ppm, in industry in lithium-ion battery electrolytes formula metals content impurity mostly in 1ppm or less.Therefore
Configure K, Na complex element solution of three gradients, the concentration of three gradients be respectively as follows: 0.5000ppm, 1.0000ppm,
2.0000ppm。
Configure Li, K, Na complex element solution.In view of lithium salt in lithium ion battery electrolyte mass percent in industry
Be 12.5% or so, dilution 25 times after lithium salt not more than 500ppm, therefore K, Na concentration be 0.5000ppm,
In each gradient solution of 1.0000ppm, 2.0000ppm, then it is separately added into the Li element of seven gradient concentrations, seven gradients are dense
Degree be respectively 5ppm, 10ppm, 20ppm, 50ppm, 100ppm, 200ppm, 500ppm to get to Li, K of 21 groups of various concentrations,
Na complex element solution.
Above-mentioned K, Na complex element solution and 21 groups of Li, K, Na complex element solution, with inductance coupled plasma
Emission spectrometer (ICP) is measured respectively, and concentration is used to mix for K, Na of 0.1000ppm, 0.2000ppm, 0.3000ppm
Element Solution is as standard solution, and the curve which measures is as standard curve.
It is as shown in table 1 to analyze comparing result.
Table 1:
Found by 1 data analysis of table: the measurement result that high concentration elemental lithium will lead to K, Na is higher, and this higher
Phenomenon K, Na concentration be 0.5000ppm, be added Li concentration of element 20ppm, 50ppm, 100ppm, 200ppm, 500ppm, or
K, Na concentration is 1.0000ppm, Li concentration of element 50ppm, 100ppm, 200ppm, 500ppm is added, or is in K, Na concentration
It is as a result higher to substantially remain in same level when 2.0000ppm, addition Li concentration of element 100ppm, 200ppm, 500ppm.?
K, Na concentration is 0.5000ppm, 1.0000ppm, 2.0000ppm, and when Li concentration of element is identical, the result error measured is not
Greatly.Comprehensively consider economic rationality, therefore obtain: when inductive coupling plasma emission spectrograph (ICP) measures, using Li element
Concentration is 50 times of complex element solution of K, Na concentration as standard solution, high concentration lithium salts can be overcome substantially to do K, Na measurement
It disturbs.
Experiment two
The complex element solution without Li for configuring K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn, the mixing member without Li
There are three gradients, respectively 0.1000ppm, 0.2000ppm, 0.3000ppm for plain solution concentration tool.
The complex element solution containing Li for configuring Li, K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn, the mixing member containing Li
There are three gradient, the concentration of Li/ (K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn) is respectively as follows: plain solution concentration tool
5.0000ppm/0.1000ppm、10.0000ppm/0.2000ppm、15.0000ppm/0.3000ppm。
Six groups of testing sample solutions are taken respectively, and every kind of testing sample solution is all made of diluent solution and is diluted, dilution
Multiple is 25 times.The diluent solution is that the mixing of nitric acid, ethyl alcohol and deionized water that volume ratio is 5:25:70 is molten
Liquid.
Respectively using above-mentioned the complex element solution without Li and the complex element solution containing Li as standard solution, use
Inductive coupling plasma emission spectrograph (ICP) is respectively to six groups of testing sample solution measurement analyses, and the results are shown in Table 2.
Table 2:
It is found by 2 data analysis of table: in measurement lithium-ion battery electrolytes when metal impurities, using the mark that elemental lithium is added
Directrix curve, substantially without influence, and can eliminate high concentration lithium salts pair to the measurement of the elements such as Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn
K, the influence of Na measurement.
Experiment three.
With experiment two identical six groups of testing sample solutions in be separately added into known concentration comprising K, Na, Fe, Ca,
The complex element solution of Pb, Cu, Cr, Ni, Al, Zn element, addition concentration gradient be 0.2000ppm, 0.5000ppm,
1.0000ppm.Using the complex element solution containing Li in experiment two as standard solution, inductively coupled plasma body emits light
Spectrometer (ICP) measures six groups of testing sample solutions and calculates the rate of recovery.Measurement result and the rate of recovery are as shown in table 3.
Table 3:
It is can be found that by 3 result of table: using the measurement side of metal impurities in lithium-ion battery electrolytes of the present invention
For the standard recovery rate of method 95%~105%, precision of analysis is good.
Experiment four.
Pure water acid system solution and volume ratio is respectively adopted as the mixed of the nitric acid of 5:25:70, ethyl alcohol and deionized water
Solution is closed as diluent solution pair to be diluted with experiment two, three identical six groups of testing sample solutions of experiment, diluted times
Number is 25 times.It is 5% nitric acid solution that pure water acid system solution, which is specially mass concentration, in this experiment.In experiment two
Complex element solution containing Li is as standard solution, and inductive coupling plasma emission spectrograph (ICP) is to six groups of samples to be tested
Solution is measured, and measurement result is as shown in table 4.
Table 4:
It analyzes to obtain by 4 data result of table: using pure water acid solution as diluent solution and analysis margin, measurement
As a result relatively low, especially heavy metal, such as Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn, this is because being made using pure water acid solution
When for diluent, the organic component in testing sample solution will appear the phenomenon that being layered with water phase, i.e., in testing sample solution
Organic component cannot sufficiently be dissolved, relatively low so as to cause measurement result.And use volume ratio for 5:25:70 nitric acid, ethyl alcohol
And the mixed solution of deionized water, as diluent solution, ethyl alcohol just overcomes drawbacks described above, it is molten so as to effectively avoid
It solves incomplete phenomenon to occur, this can greatly improve the accuracy of measurement result.
The component of the six groups of testing sample solutions used in above-mentioned experiment is as follows:
Sample 1#:DMC+EC+EMC+EA+LiPF6+ FEC (mass ratio 1: 0.9: 0.9: 1 of DMC, EC, EMC, EA, LiPF6
Molar concentration be 1mol/L, the mass concentration of FEC is 1%~10%).
Sample 2#:DMC+EC+EMC+EA+LiPF6+ LiODFB+FEC (mass ratio 1: 0.9: 0.9 of DMC, EC, EMC, EA:
1, LiPF6Concentration be 1mol/L, the mass concentration of LiODFB is that 0.1%~0.5%, FEC mass concentration is 1%~10%).
Sample 3#:DMC+EC+PP+LiPF6+ESA+LiBF4(mass ratio 0.9: 1: 1.1 of DMC, EC, PP, LiPF6It is dense
Degree is 1mol/L, LiBF4Mass concentration be 0.1%~0.5%, ESA mass concentration be 1%~2%).
Sample 4#:DMC+EC+EMC+LiPF6(mass ratio of DMC, EC, EMC are 1: 1: 1, LiPF to+MMDS6For 1mol/L,
The mass concentration of MMDS is 1%~2%).
Sample 5#:EC+EMC+PP+LiPF6(mass ratio of EC, EMC, PP are 1: 1: 1, LiPF to+LiFSI+TMSB+VC6's
Molar concentration is 1.1mol/L, and the mass concentration that the mass concentration of LiFSI is 0.5%~1%, TMSB is 0.5%~1%, VC
Mass concentration be 0.5%~5%).
Sample 6#:DMC+EC+PC+EMC+PP+LiPF6+ TMSP (mass ratio of DMC, EC, PC, EMC, PP are 1: 1: 0.1:
1: 0.8, LiPF6Concentration be 1mol/L, the mass concentration of TMSP is 0.5%~1%).
Above-mentioned experiment material code, is shown in material code table.
Material code table
In summary each analysis of experimental data the result shows that: using metal in lithium-ion battery electrolytes of the present invention
The dissolubility of the measuring method of impurity, lithium-ion battery electrolytes to be measured is good, while eliminating lithium ion battery electrolysis to be measured
The accuracy of interference of the liquid middle and high concentration lithium salts to measurement, the metals content impurity determined is good.In addition, this method is to inductance coupling
The requirement for closing plasma emission spectrometer (ICP) is relatively low, and without in addition configuring special accessory, analysis cost is low.
Claims (9)
1. the measuring method of metal impurities in lithium-ion battery electrolytes, metal impurities include K, Na, Fe, Ca, Pb, Cu, Cr,
Ni, Al, Zn, it is characterised in that: include the following steps, one, configuration standard solution, standard solution include Li, K, Na, Fe, Ca,
Pb, Cu, Cr, Ni, Al, Zn element;Two, testing sample solution is taken, dilutes testing sample solution with diluent solution, diluent is molten
Liquid is the mixed solution of nitric acid, ethyl alcohol and deionized water;Three, it using inductive coupling plasma emission spectrograph, inputs respectively
The diluted multiple of concentration value, testing sample solution of standard solution, sequentially determining analysis margin, standard solution and sample to be tested
Solution, using diluent solution as analysis margin, using the curve of the standard solution of measurement as standard curve, using external standard method meter
Calculate the content (ppm) of K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn in testing sample solution.
2. the measuring method of metal impurities in lithium-ion battery electrolytes according to claim 1, it is characterised in that: dilution
The volume ratio of nitric acid, ethyl alcohol and deionized water is 5:25:70 in agent solution.
3. the measuring method of metal impurities in lithium-ion battery electrolytes according to claim 2, it is characterised in that: to be measured
The diluted multiple of sample solution is 25.
4. the measuring method of metal impurities, feature exist in lithium-ion battery electrolytes according to claim 1 or 2 or 3
In: nitric acid grade is excellent pure grade (GR) or more in diluent solution, and ethyl alcohol is dehydrated alcohol.
5. the measuring method of metal impurities, feature exist in lithium-ion battery electrolytes according to claim 1 or 2 or 3
In: standard solution includes the first standard solution, the second standard solution, third standard solution, the first, second, third standard solution
The concentration of middle Li/ (K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn) be respectively as follows: 5.0000ppm/0.1000ppm,
10.0000ppm/0.2000ppm、15.0000ppm/0.3000ppm。
6. the measuring method of metal impurities in lithium-ion battery electrolytes according to claim 5, it is characterised in that: standard
The configuration step of solution is as follows: successively accurately weighed in the Polypropylene bottle of three 250mL on electronic balance 0.1000g,
0.2000g, 0.3000g concentration are that the complex element standard comprising K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn of 100ppm is molten
Liquid, it is 1000ppm's that 0.5000g, 1.0000g, 1.5000g concentration are then successively added in above-mentioned three Polypropylene bottles
Solution in three Polypropylene bottles is then diluted to 100g to get arriving with diluent solution by elemental lithium standard solution
The concentration of Li/ (K, Na, Fe, Ca, Pb, Cu, Cr, Ni, Al, Zn) is respectively 5.0000ppm/0.1000ppm, 10.0000ppm/
The first standard solution, the second standard solution, the third standard solution of 0.2000ppm, 15.0000ppm/0.3000ppm.
7. the measuring method of metal impurities in lithium-ion battery electrolytes according to claim 6, it is characterised in that: mixing
The error range of elemental standard solution concentration is 100 ± 0.3ppm, the error range of elemental lithium concentration of standard solution is 1000 ±
3ppm。
8. the measuring method of metal impurities in lithium-ion battery electrolytes according to claim 6, it is characterised in that: electronics
The precision of balance is 0.0001g.
9. the measuring method of metal impurities in lithium-ion battery electrolytes according to claim 6, it is characterised in that: described
Lithium-ion battery electrolytes include lithium salts and organic component, wherein lithium salts is LiPF6(lithium hexafluoro phosphate), LiBF4(tetrafluoro boron
Sour lithium), LiBOB (dioxalic acid lithium borate), LiODFB (single oxalic acid double lithium fluoroborates), in LiFSI (double fluorine sulfimide lithiums)
One or more, organic component is that one or more carbonates, carboxylic acid esters and boracic, sulfur-bearing, phosphorous esters are organic
Object.
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Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08152427A (en) * | 1994-11-29 | 1996-06-11 | Horiba Ltd | Icp emission spectroanalysis method |
CN1621808A (en) * | 2004-12-10 | 2005-06-01 | 张家港市国泰华荣化工新材料有限公司 | Method for measuring lithium salt in lithium ion battery electrolyte |
CN1888889A (en) * | 2006-07-21 | 2007-01-03 | 天津力神电池股份有限公司 | Method for measuring organic component in lithium ion cell electrolyte |
CN101551357A (en) * | 2009-02-26 | 2009-10-07 | 中国兵器工业集团第五三研究所 | ICP-MS measuring method of trace metal impurities in high purity lead |
CN102023155A (en) * | 2010-12-13 | 2011-04-20 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method for simultaneously measuring migrated masses of lead, cadmium, chromium, arsenic, antimony and germanium in plastic packaging container for foods by ICP-AES (inductively coupled plasma emission spectrometry) method |
CN102192886A (en) * | 2010-03-17 | 2011-09-21 | 深圳市比克电池有限公司 | Method for measuring lithium salt in electrolyte of lithium ion battery |
CN103091277A (en) * | 2012-08-28 | 2013-05-08 | 河北工业大学 | Method for detecting organic contamination on surface of large-sized monocrystalline silicon wafer by infrared transmission |
CN104792901A (en) * | 2015-05-06 | 2015-07-22 | 哈尔滨工业大学 | Quantitative measuring method of lithium ion battery electrolyte solvent |
CN106018382A (en) * | 2016-05-17 | 2016-10-12 | 深圳市宁深检验检测技术有限公司 | Method for rapidly testing impurity elements in high-purity gold |
-
2017
- 2017-12-20 CN CN201711381112.6A patent/CN109946366B/en active Active
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08152427A (en) * | 1994-11-29 | 1996-06-11 | Horiba Ltd | Icp emission spectroanalysis method |
CN1621808A (en) * | 2004-12-10 | 2005-06-01 | 张家港市国泰华荣化工新材料有限公司 | Method for measuring lithium salt in lithium ion battery electrolyte |
CN1888889A (en) * | 2006-07-21 | 2007-01-03 | 天津力神电池股份有限公司 | Method for measuring organic component in lithium ion cell electrolyte |
CN101551357A (en) * | 2009-02-26 | 2009-10-07 | 中国兵器工业集团第五三研究所 | ICP-MS measuring method of trace metal impurities in high purity lead |
CN102192886A (en) * | 2010-03-17 | 2011-09-21 | 深圳市比克电池有限公司 | Method for measuring lithium salt in electrolyte of lithium ion battery |
CN102023155A (en) * | 2010-12-13 | 2011-04-20 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method for simultaneously measuring migrated masses of lead, cadmium, chromium, arsenic, antimony and germanium in plastic packaging container for foods by ICP-AES (inductively coupled plasma emission spectrometry) method |
CN103091277A (en) * | 2012-08-28 | 2013-05-08 | 河北工业大学 | Method for detecting organic contamination on surface of large-sized monocrystalline silicon wafer by infrared transmission |
CN104792901A (en) * | 2015-05-06 | 2015-07-22 | 哈尔滨工业大学 | Quantitative measuring method of lithium ion battery electrolyte solvent |
CN106018382A (en) * | 2016-05-17 | 2016-10-12 | 深圳市宁深检验检测技术有限公司 | Method for rapidly testing impurity elements in high-purity gold |
Non-Patent Citations (4)
Title |
---|
庄全超 等: "锂离子电池电解液杂质的影响及去除技术", 《电池工业》 * |
辛仁轩 等: "镍电解液中主要成分和微量成分的ICP-AES测定", 《光谱实验室》 * |
陈希 等: "电感耦合等离子体原子发射光谱法同时测定锌电解液中铜镉钴", 《冶金分析》 * |
陈黎明: "ICP-AES法测定锂离子电池电解液中金属杂质元素", 《福建分析测试》 * |
Cited By (5)
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CN112213299A (en) * | 2019-07-12 | 2021-01-12 | 张家港市国泰华荣化工新材料有限公司 | Method for measuring TMSB in lithium battery electrolyte |
CN110412116A (en) * | 2019-08-27 | 2019-11-05 | 东莞东阳光科研发有限公司 | The test method and its application of sulfur content |
CN113030286A (en) * | 2019-12-25 | 2021-06-25 | 张家港市国泰华荣化工新材料有限公司 | Determination of hexamethyldisilazane content in tris (trimethylsilyl) phosphate |
CN114965444A (en) * | 2022-06-07 | 2022-08-30 | 沈阳有色金属研究院有限公司 | Method for rapidly determining 12 impurity elements in battery-grade cobalt sulfate |
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