CN113916965B - Method for detecting content of magnetic substance in lithium ion battery anode material - Google Patents
Method for detecting content of magnetic substance in lithium ion battery anode material Download PDFInfo
- Publication number
- CN113916965B CN113916965B CN202111188392.5A CN202111188392A CN113916965B CN 113916965 B CN113916965 B CN 113916965B CN 202111188392 A CN202111188392 A CN 202111188392A CN 113916965 B CN113916965 B CN 113916965B
- Authority
- CN
- China
- Prior art keywords
- electrode
- concentration
- solution
- lithium ion
- standard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 26
- 239000000126 substance Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000010405 anode material Substances 0.000 title claims abstract description 9
- 239000012086 standard solution Substances 0.000 claims abstract description 29
- 239000007774 positive electrode material Substances 0.000 claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 12
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 12
- 239000007853 buffer solution Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000003755 preservative agent Substances 0.000 claims description 8
- 230000002335 preservative effect Effects 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000000523 sample Substances 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000000872 buffer Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 239000012535 impurity Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
-
- 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 provides a method for detecting the content of magnetic substances in a lithium ion battery anode material, which comprises the steps of coating nano Fe with carbon 3 O 4 The suspension of the composite material is coated with a glassy carbon electrode to be used as a working electrode, and under a three-electrode system, fe under different concentration gradients is tested respectively 2+ Standard solution, co 2+ Standard solution, ni 2+ The voltage-current curve of the standard solution is then used to construct Fe respectively with the concentration as the abscissa and the current value of the peak as the ordinate 2+ Standard solution, co 2+ Standard solution, ni 2+ Testing the content of magnetic substances in the positive electrode material of the lithium ion battery based on the standard curve of the standard solution; compared with the prior art, the detection method provided by the invention has high sensitivity, can reach the level of trace detection, can eliminate the interference of other metal ions, and has low cost and simple operation.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a method for detecting the content of magnetic substances in a lithium ion battery anode material.
Background
In recent years, with the wide application of lithium ion batteries in the fields of power batteries and energy storage, high energy density, high potential and high safety performance have become the main development trend in the future, and the safety performance is a key performance index of lithium ion batteries.
The positive electrode material of the lithium ion battery is often mixed with magnetic substances in the manufacturing process, and is generally formed by singly or mixed metal elements such as Fe, co, ni and the like. The presence of such magnetic impurity particles can lead to reduced battery life, consistency and safety. The magnetic substance impurity in the positive electrode material of the lithium ion battery has direct influence on the self-discharge of the battery, and the content of the magnetic substance impurity is in direct proportion to the self-discharge rate of the battery, namely the higher the content of the magnetic substance is, the higher the self-discharge rate of the battery formed by the positive electrode material is.
If the content of the magnetic impurity particles in the positive electrode material of the lithium ion battery cannot be effectively detected, and then the magnetic substances are controlled in the production link of the positive electrode material, the performance of the battery can be seriously affected. In the prior art, a method for detecting magnetic substances in a positive electrode material of a lithium ion battery is not available.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for detecting the content of magnetic substances in the positive electrode material of the lithium ion battery, which can reach the level of trace detection, has low cost and is simple to operate.
The technical scheme adopted by the invention is as follows:
a method for detecting the content of a magnetic substance in a positive electrode material of a lithium ion battery, the method comprising the steps of:
(1) Placing the lithium ion battery anode material and the magnet wrapped by the preservative film into the dispersion liquid, and stirring by ultrasonic;
(2) Placing the magnet wrapped by the preservative film in a container, adding dilute sulfuric acid and dilute nitric acid into the container once, and heating and ultrasonically stirring the mixture;
(3) Centrifuging the solution obtained in the step (2), diluting the solution with dilute hydrochloric acid until the solution is weak acid, and then fixing the volume to obtain a sample solution;
(4) Coating carbon with nano Fe 3 O 4 Ultrasonically dissolving the composite material in deionized water to obtain a suspension;
(5) Uniformly coating the suspension on the polished glassy carbon electrode, and drying to obtain working electrodes A, B, C, D respectively;
(6) Placing working electrode A into NH 3 -NH 4 In Cl buffer solution, a three-electrode system is formed by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, and Fe is added dropwise into the three-electrode system 2+ Standard solution, test to obtain different Fe 2+ Voltage-current curve at concentration and with Fe 2+ Concentration is on the abscissa, fe 2+ Constructing a standard curve by taking the current value of the peak as the ordinate to obtain a linear equation A;
(7) Placing working electrode B into NH 3 -NH 4 In a Cl buffer solution, a three-electrode system is formed by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, and Co is added dropwise into the three-electrode system 2+ Standard solution, test to obtain different Co 2+ Voltage-current curve at concentration and with Co 2+ The concentration is on the abscissa, co 2+ Constructing a standard curve by taking the current value of the peak as the ordinate to obtain a linear equation B;
(8) Placing working electrode C into NH 3 -NH 4 Cl buffer compositionIn the mixed solution of (2), a three-electrode system is formed by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, and Ni is added dropwise into the three-electrode system 2+ Standard solution, test to obtain different Ni 2+ Voltage-current curve at concentration and with Ni 2+ Concentration is on the abscissa, ni 2+ Constructing a standard curve by taking the current value of the peak as the ordinate to obtain a linear equation C;
(9) Placing working electrode E in NH 3 -NH 4 In a Cl buffer solution, a three-electrode system is formed by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, the sample liquid in the step (3) is added into the three-electrode system, a voltage-current curve of a sample is obtained by testing, and Fe on the voltage-current curve is obtained 2+ Peak current value, co 2+ Peak current value, ni 2+ The peak current values are respectively substituted into a linear equation A, B, C to obtain Fe in the sample liquid 2+ 、Co 2+ 、Ni 2+ Is a concentration of (2); and further, the contents of Fe, co and Ni in the positive electrode material of the lithium ion battery can be calculated.
In the step (1), the dispersion liquid is deionized water.
In the step (2), the volume fractions of the dilute nitric acid and the dilute sulfuric acid are 30-38%; the volume ratio of the dilute nitric acid to the dilute sulfuric acid is 1:2-5.
In the step (3), dilute hydrochloric acid is used for diluting to the pH value of the solution to 6-7.
In steps (6) - (9), the NH 3 -NH 4 The Cl buffer was used in an amount of 20mL at a concentration of 0.1M and at a pH of 5.0.
In the steps (6) to (9), the concentration gradient of each standard solution added is 30, 60, 90, 120, 150, 180, 210, 240, 270, 300ppb.
In the steps (6) - (9), a desorption voltage of 0.6V is required to be applied under stirring after the test is completed, and the desorption is carried out for 60 seconds.
In the test method provided by the invention, carbon is used for coating nano Fe 3 O 4 The suspension of the composite material is coated with a glassy carbon electrode to be used as a working electrode, and under a three-electrode system, fe under different concentration gradients is tested respectively 2+ Standard solution, co 2+ Standard solution, ni 2+ The voltage-current curve of the standard solution is then used to construct Fe respectively with the concentration as the abscissa and the current value of the peak as the ordinate 2+ Standard solution, co 2+ Standard solution, ni 2+ And (3) testing the content of the magnetic substance in the positive electrode material of the lithium ion battery based on the standard curve of the standard solution.
When the preparation of the sample solution is carried out, firstly, the anode material of the lithium ion battery and the magnet wrapped by the preservative film are placed in dispersion liquid, and ultrasonic stirring is carried out to screen out magnetic substances in the anode material of the lithium ion battery; then the magnetic substance is dissolved by dilute nitric acid and dilute sulfuric acid, and the obtained solution is diluted to pH 6-7 by dilute hydrochloric acid after centrifugation, and then the volume is fixed.
Compared with the prior art, the detection method provided by the invention has high sensitivity, can reach the level of trace detection, can eliminate the interference of other metal ions, and has low cost and simple operation.
Drawings
FIG. 1 shows the different Fe values in example 1 2+ Voltage-current curve at concentration and Fe 2+ Concentration is on the abscissa, fe 2+ Constructing a standard curve A by taking the current value of the peak as the ordinate;
FIG. 2 is a graph of different Co in example 1 2+ Voltage-current curve at concentration and Co 2+ The concentration is on the abscissa, co 2+ Constructing a standard curve B by taking the current value of the peak as the ordinate;
FIG. 3 shows the Ni values of example 1 2+ Voltage-current curve at concentration and Ni 2+ Concentration is on the abscissa, ni 2+ Constructing a standard curve C by taking the current value of the peak as the ordinate;
FIG. 4 is a plot of voltage versus current for the sample solution of example 2 without addition.
Detailed Description
The following is a detailed description of embodiments with reference to the accompanying drawings.
Carbon-coated nano Fe used in the present invention 3 O 4 The preparation method of the composite material is described in the example of Chinese patent CN101728526A1, and a method disclosed in 1.
Fe 2+ Standard solution, co 2+ Standard solution, ni 2+ The preparation method of the standard solution comprises the following steps: and respectively dissolving the ferrous chloride standard substance, the cobalt chloride standard substance and the nickel chloride standard substance in deionized water, and gradually diluting the solution with deionized water until the concentration is 10ppb.
The conditions of the electrochemical workstation are: the frequency was 25Hz, the amplitude was 25mV, and the incremental potential was 4mV.
After the test of each test system is completed, a desorption voltage of 0.6V is required to be applied under the condition of stirring, and the desorption is carried out for 60 seconds, so that the residual metal on the electrode is eliminated.
Example 1
The construction method of each standard curve is as follows:
s1, coating 0.25mg of carbon on nano Fe 3 O 4 Ultrasonic dissolving the composite material in 20mL of deionized water to obtain a suspension;
s2, polishing the glassy carbon electrode by using 0.3 mu m alumina, uniformly coating 5 mu L of suspension on the polished glassy carbon electrode, and naturally air-drying to obtain working electrodes A, B, C, D respectively;
s3, placing a three-electrode system consisting of a working electrode A, a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode into 20mL of 0.1M NH with pH of 5.0 3 -NH 4 In the Cl buffer solution, an electrochemical workstation is connected, and Fe is added into the mixed solution A dropwise 2+ Standard solution, added Fe 2+ The concentration gradients of the standard solutions are 30, 60, 90, 120, 150, 180, 210, 240ppb; testing to obtain different Fe 2+ Voltage-current curve at concentration and with Fe 2+ Concentration is on the abscissa, fe 2+ The peak current value is taken as an ordinate to construct a standard curve A, and as shown in FIG. 1, a linear equation A is obtained: y= -0.7839+41.93x, linear correlation coefficient R 2 =0.993 wherein Y is a current value in μa; x is Fe 2+ Is the concentration in ppb;
s4, placing a three-electrode system consisting of a working electrode B, a platinum wire electrode serving as a counter electrode and a saturated Ag/AgCl electrode serving as a reference electrode into 20mL of 0.1M pH 5.NH of 0 3 -NH 4 In the Cl buffer solution, an electrochemical workstation is connected, co is added into the mixed solution B dropwise 2+ Standard solution, co added 2+ The concentration gradients of the standard solutions are 30, 60, 90, 120, 150, 180, 210, 240ppb; testing to obtain different Co 2+ Voltage-current curve at concentration and with Co 2+ The concentration is on the abscissa, co 2+ The peak current value is taken as an ordinate to construct a standard curve B, and as shown in FIG. 2, a linear equation B is obtained: y= -7.6088+30.27x, linear correlation coefficient R 2 =0.999 wherein Y is a current value in μa; x is Co 2+ Is the concentration in ppb;
s5, placing a three-electrode system consisting of a working electrode C, a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode into 20mL of 0.1M NH with pH of 5.0 3 -NH 4 In the Cl buffer solution, an electrochemical workstation is connected, ni is added into the mixed solution C dropwise 2+ Standard solution, ni added 2+ The concentration gradients of the standard solutions are 30, 60, 90, 120, 150, 180, 210, 240ppb; testing to obtain different Ni 2+ Voltage-current curve at concentration and with Ni 2+ Concentration is on the abscissa, ni 2+ The peak current value is taken as an ordinate to construct a standard curve C, and as shown in FIG. 3, a linear equation C is obtained: y= -7.21+29.47x, linear correlation coefficient R 2 =0.998 wherein Y is a current value in μa; x is Ni 2+ Is in ppb.
Example 2
The method for detecting the content of the magnetic substance in the positive electrode material of the lithium ion battery comprises the following steps:
(1) Placing 10mg of a cherry-like magnet wrapped by the lithium ion battery anode material and the preservative film in deionized water, and stirring for 30min by ultrasonic waves; thus, magnetic substances in the positive electrode material of the lithium ion battery can be adsorbed on the surface of the magnet wrapped by the preservative film;
(2) Placing the magnet wrapped by the preservative film taken out from the step (1) into a beaker, sequentially adding 20mL of 38% dilute sulfuric acid and 30mL of 38% dilute nitric acid into the magnet, and heating, stirring and ultrasonically stirring for 2h;
(3) Centrifuging the solution obtained in the step (2), concentrating and drying under reduced pressure, and then adding deionized water to fix the volume to 5mL to obtain a sample solution;
(4) A three-electrode system consisting of a working electrode E, a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode is put into 20mL of NH with the pH of 0.1M being 5 3 -NH 4 To the Cl buffer solution, 5mL of the sample solution in step (3) was added, and the voltage-current curve was tested, as shown in FIG. 4;
(5) Fe on the voltage-current curve in step (4) 2+ The peak current value is substituted into the linear equation A, co 2+ The peak current value is substituted into the linear equation B, ni 2+ Substituting the peak current value into a linear equation C to calculate Fe in the sample liquid 2 + 、Co 2+ 、Ni 2+ Is a concentration of (2); and further, the contents of Fe, co and Ni in the positive electrode material of the lithium ion battery can be calculated.
The above detailed description of a method for detecting the content of magnetic substances in a positive electrode material of a lithium ion battery with reference to the embodiments is illustrative and not restrictive, and several embodiments can be listed according to the defined scope, so that variations and modifications without departing from the general inventive concept shall fall within the scope of protection of the present invention.
Claims (6)
1. A method for detecting the content of a magnetic substance in a positive electrode material of a lithium ion battery, the method comprising the steps of:
(1) Placing the lithium ion battery anode material and the magnet wrapped by the preservative film into the dispersion liquid, and stirring by ultrasonic;
(2) Placing the magnet wrapped by the preservative film in a container, sequentially adding dilute sulfuric acid and dilute nitric acid into the container, and stirring by ultrasonic waves;
(3) Centrifuging the solution obtained in the step (2), concentrating and drying under reduced pressure, and then adding deionized water to fix the volume to obtain a sample solution;
(4) Coating carbon with nano Fe 3 O 4 Ultrasonically dissolving the composite material in deionized water to obtain a suspension;
(5) Uniformly coating the suspension on the polished glassy carbon electrode, and drying to obtain working electrodes A, B, C, D respectively;
(6) Placing working electrode A into NH 3 -NH 4 In Cl buffer solution, a three-electrode system is formed by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, and Fe is added dropwise into the three-electrode system 2+ Standard solution, test to obtain different Fe 2+ Voltage-current curve at concentration and with Fe 2+ Concentration is on the abscissa, fe 2+ Constructing a standard curve by taking the current value of the peak as the ordinate to obtain a linear equation A;
(7) Placing working electrode B into NH 3 -NH 4 In a Cl buffer solution, a three-electrode system is formed by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, and Co is added dropwise into the three-electrode system 2+ Standard solution, test to obtain different Co 2+ Voltage-current curve at concentration and with Co 2+ The concentration is on the abscissa, co 2+ Constructing a standard curve by taking the current value of the peak as the ordinate to obtain a linear equation B;
(8) Placing working electrode C into NH 3 -NH 4 In the mixed solution composed of Cl buffer solution, a three-electrode system is composed of a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, ni is added dropwise 2+ Standard solution, test to obtain different Ni 2+ Voltage-current curve at concentration and with Ni 2+ Concentration is on the abscissa, ni 2+ Constructing a standard curve by taking the current value of the peak as the ordinate to obtain a linear equation C;
(9) Placing working electrode E in NH 3 -NH 4 In a Cl buffer solution, a three-electrode system is formed by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode, the sample liquid in the step (3) is added into the three-electrode system, a voltage-current curve of a sample is obtained by testing, and Fe on the voltage-current curve is obtained 2+ Peak current value, co 2+ Peak current value, ni 2+ The peak current values are respectively substituted into a linear equation A, B, C to obtain Fe in the sample liquid 2+ 、Co 2+ 、Ni 2+ Is a concentration of (2); and further, the contents of Fe, co and Ni in the positive electrode material of the lithium ion battery can be calculated.
2. The method of claim 1, wherein in step (1), the dispersion is deionized water.
3. The method according to claim 1, wherein in the step (2), the volume fractions of the dilute sulfuric acid and the dilute nitric acid are 30-38%; the volume ratio of the dilute sulfuric acid to the dilute nitric acid is 1.5-5:1.
4. The method according to claim 1, wherein in steps (6) - (9), the NH is 3 -NH 4 The Cl buffer was used in an amount of 20mL at a concentration of 0.1M and at a pH of 5.0.
5. The method according to claim 1, wherein in the steps (6) to (9), the concentration gradient of each of the standard solutions to be added is 30, 60, 90, 120, 150, 180, 210, 240, 270, 300ppb.
6. The method according to claim 1, wherein in the steps (6) to (9), a desorption voltage of 0.6V is applied under stirring for 60 seconds after the completion of the test.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111188392.5A CN113916965B (en) | 2021-10-12 | 2021-10-12 | Method for detecting content of magnetic substance in lithium ion battery anode material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111188392.5A CN113916965B (en) | 2021-10-12 | 2021-10-12 | Method for detecting content of magnetic substance in lithium ion battery anode material |
Publications (2)
Publication Number | Publication Date |
---|---|
CN113916965A CN113916965A (en) | 2022-01-11 |
CN113916965B true CN113916965B (en) | 2023-12-15 |
Family
ID=79239523
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111188392.5A Active CN113916965B (en) | 2021-10-12 | 2021-10-12 | Method for detecting content of magnetic substance in lithium ion battery anode material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113916965B (en) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103884571A (en) * | 2014-04-11 | 2014-06-25 | 深圳市德方纳米科技有限公司 | Method for testing content of magnetic substances in lithium ion battery anode material |
CN106610352A (en) * | 2015-10-22 | 2017-05-03 | 深圳市比克动力电池有限公司 | Method for detecting magnetic substance content of lithium ion battery positive electrode material |
JP2018169399A (en) * | 2018-04-26 | 2018-11-01 | 御国色素株式会社 | Method for detecting iron, method for producing slurry containing carbon material, and method for producing lithium ion battery controlled by method of detecting same |
CN110411914A (en) * | 2019-07-30 | 2019-11-05 | 厦门凯纳石墨烯技术股份有限公司 | Lithium ion battery magnetism of material substance detecting method |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9511670B2 (en) * | 2011-12-07 | 2016-12-06 | GM Global Technology Operations LLC | Magnetic sensor transformer for determining state of charge for iron phosphate lithium ion batteries |
-
2021
- 2021-10-12 CN CN202111188392.5A patent/CN113916965B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103884571A (en) * | 2014-04-11 | 2014-06-25 | 深圳市德方纳米科技有限公司 | Method for testing content of magnetic substances in lithium ion battery anode material |
CN106610352A (en) * | 2015-10-22 | 2017-05-03 | 深圳市比克动力电池有限公司 | Method for detecting magnetic substance content of lithium ion battery positive electrode material |
JP2018169399A (en) * | 2018-04-26 | 2018-11-01 | 御国色素株式会社 | Method for detecting iron, method for producing slurry containing carbon material, and method for producing lithium ion battery controlled by method of detecting same |
CN110411914A (en) * | 2019-07-30 | 2019-11-05 | 厦门凯纳石墨烯技术股份有限公司 | Lithium ion battery magnetism of material substance detecting method |
Non-Patent Citations (1)
Title |
---|
锂离子电池原料中磁性杂质检测;崔雪红;王淑霞;张明春;;天津化工(03);全文 * |
Also Published As
Publication number | Publication date |
---|---|
CN113916965A (en) | 2022-01-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US10386326B2 (en) | Flexible electrical devices and methods | |
Dollé et al. | Development of reliable three-electrode impedance measurements in plastic Li-ion batteries | |
Zen et al. | Square-wave voltammetric determination of uric acid by catalytic oxidation at a perfluorosulfonated ionomer/ruthenium oxide pyrochlore chemically modified electrode | |
CN109613090B (en) | Sea urchin type Prussian blue-palladium core-shell structure loaded nitrogen-doped graphene nanocomposite material, electrode prepared from composite material and application of composite material | |
CN103884571A (en) | Method for testing content of magnetic substances in lithium ion battery anode material | |
Itagaki et al. | Deviations of capacitive and inductive loops in the electrochemical impedance of a dissolving iron electrode | |
Alvarez et al. | Cathodic stripping voltammetry of paraquat on a carbon paste electrode modified with amberlite XAD-2 resin | |
Duay et al. | Stripping voltammetry for the real time determination of zinc membrane diffusion coefficients in high pH: towards rapid screening of alkaline battery separators | |
CN113138345A (en) | Method for evaluating performance of lithium ion battery by using symmetric battery | |
CN113916965B (en) | Method for detecting content of magnetic substance in lithium ion battery anode material | |
CN109655098A (en) | The failure analysis method of secondary cell battery core | |
CN112179894A (en) | Method for detecting free iron in lithium iron phosphate anode slurry of lithium ion battery | |
CN111366631B (en) | Determining adsorption performance of material by electrochemical polarization curve and/or electrochemical impedance spectrum | |
Qin et al. | Electrochemical sensor based on Nafion/gold nanoparticle/electrochemically reduced graphene oxide composite-modified glassy carbon electrode for the detection of diuron | |
Tanaka et al. | In vivo voltammetry with an ultramicroelectrode | |
CN110412098B (en) | Flower-ball-shaped Mn-Fe Prussian blue analogue material and preparation method and application thereof | |
CN111999358A (en) | Application of graphite-like phase carbon nitride nano material as electrochemical modified electrode material in methyl mercury detection | |
JP2001110458A (en) | Method for inspecting short circuit of battery abd apparatus for inspecting short circuit of battery | |
Zhang et al. | Detection of chromium (VI) in water using an electrochemical sensor based on Ketjen black-modified carbon cloth | |
CN114563537B (en) | Method for rapidly judging cycle life of lithium iron phosphate battery | |
CN214957012U (en) | Miniature device for testing electrochemical performance of lithium ion battery | |
CN107121465A (en) | A kind of working electrode of complex carbon material modification detects the electrochemical method of heavy metal | |
JP4236746B2 (en) | Method for inspecting oxidation degree of negative electrode material for battery | |
CN114923967B (en) | Laminated electrochemical sensing device based on carbon paper electrode and application of laminated electrochemical sensing device in heavy metal detection | |
US7988844B2 (en) | Method for measuring an iodine adsorption number of carbon black, electrolytic cell, and kit for measuring an iodine adsorption number of carbon black |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |