CN116818643A - Method for measuring corrosion rate of aluminum foil for battery - Google Patents
Method for measuring corrosion rate of aluminum foil for battery Download PDFInfo
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- CN116818643A CN116818643A CN202310864455.7A CN202310864455A CN116818643A CN 116818643 A CN116818643 A CN 116818643A CN 202310864455 A CN202310864455 A CN 202310864455A CN 116818643 A CN116818643 A CN 116818643A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 107
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000011888 foil Substances 0.000 title claims abstract description 107
- 238000005260 corrosion Methods 0.000 title claims abstract description 44
- 230000007797 corrosion Effects 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000003792 electrolyte Substances 0.000 claims abstract description 41
- 238000007600 charging Methods 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 3
- 238000012360 testing method Methods 0.000 claims description 14
- 238000010280 constant potential charging Methods 0.000 claims description 12
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 10
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 9
- 229910052744 lithium Inorganic materials 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 7
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 229910013872 LiPF Inorganic materials 0.000 claims description 3
- 101150058243 Lipf gene Proteins 0.000 claims description 3
- 238000002848 electrochemical method Methods 0.000 claims description 3
- 230000002687 intercalation Effects 0.000 claims description 3
- 238000009830 intercalation Methods 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 229910010941 LiFSI Inorganic materials 0.000 claims 2
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical group [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 claims 2
- 239000008151 electrolyte solution Substances 0.000 claims 1
- 238000006864 oxidative decomposition reaction Methods 0.000 abstract description 6
- 238000012512 characterization method Methods 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 12
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 10
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 10
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 9
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 7
- 238000007599 discharging Methods 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 239000013543 active substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- -1 lithium bis-fluorosulfonyl imide Chemical class 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000003698 laser cutting Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000270722 Crocodylidae Species 0.000 description 1
- 238000006424 Flood reaction Methods 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CXULZQWIHKYPTP-UHFFFAOYSA-N cobalt(2+) manganese(2+) nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[O--].[Mn++].[Co++].[Ni++] CXULZQWIHKYPTP-UHFFFAOYSA-N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- LNNWVNGFPYWNQE-GMIGKAJZSA-N desomorphine Chemical compound C1C2=CC=C(O)C3=C2[C@]24CCN(C)[C@H]1[C@@H]2CCC[C@@H]4O3 LNNWVNGFPYWNQE-GMIGKAJZSA-N 0.000 description 1
- 238000009791 electrochemical migration reaction Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 239000011532 electronic conductor Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000003797 solvolysis reaction Methods 0.000 description 1
- VKJKOXNPYVUXNC-UHFFFAOYSA-K trilithium;trioxido(oxo)-$l^{5}-arsane Chemical compound [Li+].[Li+].[Li+].[O-][As]([O-])([O-])=O VKJKOXNPYVUXNC-UHFFFAOYSA-K 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Secondary Cells (AREA)
Abstract
The invention relates to the technical field of aluminum foil detection methods, and discloses a method for measuring the corrosion rate of an aluminum foil for a battery, which comprises the following steps: s1, assembling an aluminum foil to be tested, electrolyte and an auxiliary electrode into an electrolytic cell; s2, taking the aluminum foil to be detected as a battery anode and an auxiliary electrode as a battery cathode, and charging electrolysis Chi Hengya to enable the aluminum foil to undergo oxidation reaction; s3, representing the corrosion rate of the aluminum foil through a weightlessness method. According to the invention, the aluminum foil to be tested is subjected to oxidation reaction in the electrolyte in a constant-pressure mode, and the influence of solvent oxidative decomposition on corrosion rate measurement can be prevented in principle due to the fact that the potential of the auxiliary electrode is constant or the change is tiny, so that the precision and the stability are higher; the control of each condition parameter is matched with each other, so that the accuracy and stability of the aluminum foil corrosion rate characterization are higher, and the determination method is more convenient and rapid.
Description
Technical Field
The invention relates to the technical field of aluminum foil detection methods, in particular to a method for measuring the corrosion rate of an aluminum foil for a battery.
Background
The aluminum foil is used as an important auxiliary material of the lithium ion battery and is used as an electronic conductor of the battery, when the battery discharges, the aluminum foil plays a role in collecting electrons generated by active substances and gathers the electrons to the tabs, so that high power output energy of the battery is ensured, and when the battery charges, the aluminum foil equally distributes current to the active substances, so that the active substances can be oxidized due to positive charges. During the service life of the battery, on one hand, the contact between the active substance and the aluminum foil is not firm or tight due to the problems of binder consumption, floating and the like. On the other hand, components in the electrolyte, such as LiFSI (lithium bis-fluorosulfonyl imide) and LiTFSI (lithium bis-trifluoromethanesulfonyl imide), corrode the aluminum foil, and trace amounts of hydrofluoric acid in the electrolyte also corrode the aluminum foil, which can cause the contact resistance between the active material and the aluminum foil to become large. In 1991Journal of Power SourcesPublished in the sectionElectrolytes of advanced batteriesThe literature reports the application of the electrolyte in lithium ion batteries for the first time, and also reports the characteristics of the electrolyte for corroding aluminum current collectors. The adhesion force between the aluminum foil and the active material and the corrosion resistance thereof are related to the cycle life, charge and discharge capacity, rate discharge and other performances of the battery.
Lithium hexafluorophosphate is used as an electrolyte with the most widely used, and has better film forming property compared with lithium tetrafluoroborate, higher stability compared with lithium perchlorate and environmental friendliness compared with lithium arsenate. In recent years, with the increase of the demand of energy storage and passenger car markets for lithium ion batteries, the markets have put higher demands on the performances of battery cycle life, charge-discharge multiplying power and the like, which forces battery manufacturing enterprises to start to adopt electrolyte containing LiFSI or LiTFSI. The lithium ion battery adopting the electrolyte has more excellent cycle life and charge-discharge rate performance, but also faces new risks, namely aluminum foil corrosion.
The metal aluminum is a material for sub passivation, the aluminum foil for the battery is generally a micron-sized foil obtained by multi-pass rolling of a 1-series aluminum alloy, and the 1-series aluminum alloy is similar to pure aluminum in composition and only a very small amount of alloying elements such as Si, fe, cu and the like are added. In general, corrosion of aluminum foil generates Al 3+ Belongs to oxidation reaction. At present, the lithium ion battery using nickel cobalt manganese oxide as the positive electrode material has the highest energy density, and when the battery is fully charged, the potential of the positive electrode is higher, and the battery has stronger oxidizing capability, so that the corrosion resistance of the aluminum foil is weakest, and the highest balance electrode potential of the positive electrode is 4.30-4.40V (vs. Li/Li) + )。
Disclosure of Invention
In order to solve the technical problems, the invention provides the method for measuring the corrosion rate of the aluminum foil for the battery, and the aluminum foil to be measured is subjected to oxidation reaction in a constant voltage charging mode in the electrolyte, so that the accuracy and stability of the corrosion rate characterization of the aluminum foil are higher, and the measuring method is more convenient and faster.
The aim of the invention is realized by the following technical scheme: a method for measuring the corrosion rate of an aluminum foil for a battery, comprising the steps of:
s1, assembling an aluminum foil to be tested, electrolyte and an auxiliary electrode into an electrolytic cell;
s2, taking the aluminum foil to be detected as a battery anode and an auxiliary electrode as a battery cathode, and charging electrolysis Chi Hengya to enable the aluminum foil to undergo oxidation reaction;
s3, representing the corrosion rate of the aluminum foil through a weightlessness method.
The invention adopts a constant voltage mode, and the auxiliary electrode has constant potential or tiny change, so that the influence of solvent oxidative decomposition on corrosion rate measurement can be prevented in principle, and the precision and the stability are higher. A large number of experiments show that if the metal is corroded by adopting a constant current and dynamic voltage mode, the corrosion is realized in practiceIn the actual operation process, polarization difference is caused due to the corrosion resistance difference of the foil, so that electrode potential difference is caused, uncontrollable experimental factors are more, and larger experimental errors are caused. At high current densities, the oxidative decomposition voltage of the solvent is very accessible, so that the solvent is oxidatively decomposed, and therefore the applied anodic current is not entirely from M to M n+ +e - The electrode reactions of (a) result, i.e. the influence of solvolysis on the corrosion rate measurement cannot be completely excluded. And the gas production is large, the electrolyte consumption is fast, the accuracy cannot be evaluated due to the side reaction to a large extent, and certain potential safety hazards exist.
Therefore, the aluminum foil to be tested is subjected to oxidation reaction in the electrolyte, and the accuracy and stability of the aluminum foil corrosion rate characterization are higher, and the determination method is more convenient and rapid by adopting a constant voltage charging mode and controlling various condition parameters.
Preferably, the corrosion rate v is calculated as follows: v= (m 1 -m 2 )/(2.7*2*l*d*t)*1000，µm/d；
Wherein m is 1 The initial weight of the aluminum foil is in mg; m is m 2 Taking out the aluminum foil to be tested after the constant voltage charging process is finished, and weighing the aluminum foil to be tested after cleaning, baking and cooling in turn, wherein the unit is mg; l is the length of the aluminum foil in mm; d is the width of the aluminum foil, and the unit is mm; t is the constant voltage charging time of the electrolytic cell in d days.
Preferably, the test aluminum foil is cut into a regular shape, such as a rectangle, and the tab is reserved, and the weight of the cut aluminum foil to be tested is weighed by using an electronic balance with the precision of 0.1 mg and recorded as m 1 The length and width of the cut aluminum foil to be measured are respectively marked as l and d by using a length measuring tool with the precision of 0.5 mm. The tab is connected with the positive electrode lead of the battery charging and discharging cabinet.
Preferably, after the constant voltage charging process is completed, taking out the aluminum foil to be tested, cleaning the aluminum foil to be tested by using EMC or DEC, baking the aluminum foil to be tested by using a vacuum oven to remove cleaning solvent in order to prevent the aluminum foil from being oxidized, wherein the baking temperature is less than or equal to 60 ℃, weighing the aluminum foil to be tested again by using an electronic balance after cooling, and recording that the weight is m at the moment 2 。
Preferably, the electrolyte includes a solvent and an electrolyte; the concentration of electrolyte in the electrolyte is 0.8-1.2 mol/L.
The electrolyte composition can prevent the electrolyte from oxidative decomposition, and avoid inaccurate test results. The electrolyte is used in an amount to ensure that the liquid level just floods the length direction of the aluminum foil to be measured.
Preferably, the solvent is one of EC (ethylene carbonate) and DEC (diethyl carbonate), EC (ethylene carbonate) and EMC (methyl ethyl carbonate), EC (ethylene carbonate) and DMC (dimethyl carbonate), PC (propylene carbonate) and DEC (diethyl carbonate), PC (propylene carbonate) and EMC (methyl ethyl carbonate), PC and DMC (dimethyl carbonate) binary mixed solvents.
EC and PC are cyclic solvents, belong to high dielectric constant solvents, and can dissociate more lithium salts, so that more lithium/sodium ions exist in the solution, but the viscosity is higher, and the ionic migration is not facilitated. EMC/DEC/DMC is a linear organic solvent, has very low dielectric constant and very low viscosity, and is beneficial to improving lithium/sodium ion migration. The binary mixing can balance ion conductivity and ion migration resistance, so that the accuracy and stability of the aluminum foil corrosion rate characterization are higher.
Preferably, the electrolyte is LiFSI and LiPF 6 Or LiTFSI with LiPF 6 Is a mixture of (a) and (b).
Preferably, the LiFSI and LiPF 6 Or LiTFSI and LiPF 6 The mass ratio of (2) is 0.2-5.
Preferably, the expansion area of the auxiliary electrode is not smaller than the expansion area of the aluminum foil to be tested.
The expanding area of the auxiliary electrode which is more than or equal to the test aluminum foil is used for controlling the current density of the auxiliary electrode which is less than or equal to the current density of the test electrode, so that the electrode potential of the test electrode is conveniently controlled, and the corrosion rate is measured more accurately.
Preferably, the auxiliary electrode is a metal lithium belt or an artificial graphite negative plate; the artificial graphite negative electrode sheet is required to be subjected to lithium intercalation by an electrochemical method before the test is started, so that the electrode is balancedThe potential is 80-100 mV (vs. Li/Li) + )。
The potential of the graphite electrode only changes within the range of 80-100 mV, which is beneficial to accurately controlling the electrode potential of the test electrode.
Preferably, the voltage control range of charging is 0-5V, and the charging time is 24-72 h. The ohmic resistance of the positive and negative leads is less than or equal to 1 m omega.
The voltage is controlled within the range of 0-5V, so that the test electrode can be controlled to generate good oxidation reaction.
Preferably, in the corrosion rate measurement process of the aluminum foil to be measured, the environmental moisture content is less than or equal to 1000 ppm, the oxygen content is less than or equal to 1000 ppm, and the environmental temperature is 20-30 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) The constant voltage mode is adopted, and the influence of the oxidative decomposition of the solvent on the corrosion rate measurement can be prevented in principle because the potential of the auxiliary electrode is constant or the change is tiny, so that the accuracy and the stability are higher;
(2) The electrolyte composition can not only corrode the aluminum foil to be tested, but also prevent the electrolyte from oxidative decomposition, so that inaccurate test results are avoided;
(3) The control of each condition parameter is matched with each other, so that the accuracy and stability of the aluminum foil corrosion rate characterization are higher, and the determination method is more convenient and rapid.
Drawings
FIG. 1 is a schematic diagram showing structural connection of a corrosion rate measuring method of an aluminum foil for a battery according to the present invention;
fig. 2 is a schematic diagram of an aluminum foil to be tested in the present invention.
The reference numerals are: the battery charging and discharging cabinet 1, the electrolytic cell 2, the electrolyte 3, the aluminum foil 4 to be tested, the auxiliary electrode 5, the sealing cover 6, the positive electrode lead 7 and the negative electrode lead 8.
Detailed Description
The technical scheme of the present invention is described below by using specific examples, but the scope of the present invention is not limited thereto:
a corrosion rate measuring method of aluminum foil for a battery ensures that the ambient moisture is less than or equal to 1000 ppm, the oxygen content is less than or equal to 1000 ppm and the ambient temperature is 20-30 ℃; the method specifically comprises the following steps:
s1, as shown in FIG. 1, assembling an aluminum foil 4 to be tested, an electrolyte 3 and an auxiliary electrode 5 into an electrolytic cell 2;
the electrolyte comprises a solvent and an electrolyte; the solvent is one of EC and DEC, EC and EMC, EC and DMC, PC and DEC, PC and EMC, PC and DMC binary mixed solvent; the electrolyte is LiFSI and LiPF with the mass ratio of 0.2-5 6 Or LiTFSI and LiPF with a mass ratio of 0.2-5 6 The concentration of the electrolyte is 0.8-1.2 mol/L;
the auxiliary electrode is a metal lithium belt or an artificial graphite negative plate; the artificial graphite negative electrode sheet is subjected to lithium intercalation by an electrochemical method before the test starts, so that the potential of a balance electrode is 80-100 mV (vs. Li/Li) + )。
S2, connecting an aluminum foil 4 to be tested with a positive electrode lead 7 to serve as a battery positive electrode, connecting an auxiliary electrode 5 with a negative electrode lead 8 to serve as a battery negative electrode, wherein the expansion area of the auxiliary electrode is not smaller than that of the aluminum foil to be tested, the positive electrode lead 7 and the negative electrode lead 8 are respectively connected with a battery charging and discharging cabinet 1, after a sealing cover 6 of an electrolytic cell 2 is covered, the aluminum foil is subjected to oxidation reaction through constant-voltage charging of the electrolytic cell 2, the charging voltage control range is 0-5V, and the charging time is 24-72 h.
S3, representing corrosion rate v= (m) of aluminum foil through weightlessness method 1 -m 2 )/(2.7*2*l*d*t)*1000，µm/d；
Wherein m is 1 The initial weight of the aluminum foil is in mg; m is m 2 Taking out the aluminum foil to be tested after the constant voltage charging process is finished, and weighing the aluminum foil to be tested after cleaning, baking and cooling in turn, wherein the unit is mg; l is the length of the aluminum foil in mm; d is the width of the aluminum foil, and the unit is mm; t is the constant voltage charging time of the electrolytic cell in d days.
Example 1
S1, as shown in FIG. 2, the test aluminum foil is cut into a rectangle, and the tab is reserved, and the aluminum foil 114 x 113mm (l x d) to be tested and the artificial graphite auxiliary electrode 114 x 113mm are cut by using a laser cutting die. And the weight of the aluminum foil to be measured is weighed by using an electronic balance with the precision of 0.1 mg to be measuredThe weight of the aluminum foil is 521.9 mg (m) 1 ）。
S2, forming a battery by the artificial graphite auxiliary electrode and the lithium iron phosphate positive plate, charging the battery, and charging the battery to 3.60V by using a current with the rate of 0.5C after the formation is finished. When the water oxygen content in the glove box is less than or equal to 500 ppm, the battery is disassembled in the glove box, the artificial graphite auxiliary electrode is taken out, and the potential of the balance electrode is approximately equal to 80 and mV (vs. Li/Li) + )。
S3, 30% EC+58% DEC+9% LiPF 6 The mass fraction of +3% LiFSI is used for preparing electrolyte.
S4, assembling the cut aluminum foil, electrolyte and artificial graphite auxiliary electrode into an electrolytic cell according to the diagram shown in the figure 1, wherein the electrolyte is used in an amount to ensure that the liquid level just submerges the length direction of the aluminum foil to be detected, the electrode lugs are connected with the positive and negative electrode leads of the charging and discharging cabinet, and the cover of the electrolytic cell is covered. The constant voltage charging is carried out on the electrolytic cell through the computer-controlled battery charging and discharging test cabinet, the charging voltage is 4.40V, and the charging time is 2d (t).
S5, cleaning the aluminum foil to be tested by EMC after charging, and weighing again after vacuum drying, wherein the weight is 515.7 mg (m 2 ）。
Corrosion rate v= (m) of aluminum foil 1 -m 2 ) V is 0.00891 μm/d,/(2.7 x 2 x l x d x t) 1000.
Example 2
S1, cutting an aluminum foil 114 x 113mm (l x d) to be tested and an artificial graphite auxiliary electrode by using a laser cutting die. And the weight of the aluminum foil to be measured was weighed using an electronic balance with an accuracy of 0.1 mg, and the weight of the aluminum foil to be measured was 521.9 mg (m 1 ）。
S2, cutting out rectangular lithium foil by using scissors to serve as an auxiliary electrode, wherein the length of the auxiliary electrode is 120 mm, the width of the auxiliary electrode is 115mm, and one end of the auxiliary electrode is clamped by using crocodile clips.
S3, 30% EC+58% DEC+6% LiPF 6 The mass fraction of +6% LiFSI is used for preparing electrolyte.
S4, assembling the cut aluminum foil, electrolyte and auxiliary electrodes into an electrolytic cell according to the diagram shown in the FIG 1, wherein the electrolyte is used in an amount to ensure that the liquid level just submerges the length direction of the aluminum foil to be detected, the electrode lugs are connected with the positive and negative electrode leads of the charging and discharging cabinet, and the cover of the electrolytic cell is covered. The constant voltage charging is carried out on the electrolytic cell through the computer-controlled battery charging and discharging test cabinet, the charging voltage is 4.30V, and the charging time is 2d (t).
S5, cleaning the aluminum foil to be tested by EMC after charging, and weighing again after vacuum drying, wherein the weight is 517.4 mg (m 2 ）。
Corrosion rate v= (m) of aluminum foil 1 -m 2 ) V is 0.00646 μm/d,/(2.7 x 2 x l x d x t) 1000.
The foregoing description is only of the preferred embodiments of the present invention, and is not intended to limit the scope of the invention, but rather is intended to cover any equivalents of the structures disclosed herein or modifications in the equivalent processes, or any application of the structures disclosed herein, directly or indirectly, in other related arts.
Claims (10)
1. A method for measuring the corrosion rate of an aluminum foil for a battery, comprising the steps of:
s1, assembling an aluminum foil to be tested, electrolyte and an auxiliary electrode into an electrolytic cell;
s2, taking the aluminum foil to be detected as a battery anode and an auxiliary electrode as a battery cathode, and charging electrolysis Chi Hengya to enable the aluminum foil to undergo oxidation reaction;
s3, representing the corrosion rate of the aluminum foil through a weightlessness method.
2. The method for measuring the corrosion rate of an aluminum foil for a battery according to claim 1, wherein the corrosion rate v is calculated as follows: v= (m 1 -m 2 )/(2.7*2*l*d*t)*1000，µm/d；
Wherein m is 1 The initial weight of the aluminum foil is in mg; m is m 2 Taking out the aluminum foil to be tested after the constant voltage charging process is finished, and weighing the aluminum foil to be tested after cleaning, baking and cooling in turn, wherein the unit is mg; l is the length of the aluminum foil in mm; d is the width of the aluminum foil, and the unit is mm; t is the constant voltage charging time of the electrolytic cell in d days.
3. The method for measuring the corrosion rate of an aluminum foil for a battery according to claim 1 or 2, wherein the electrolytic solution comprises a solvent and an electrolyte; the concentration of electrolyte in the electrolyte is 0.8-1.2 mol/L.
4. The method for measuring the corrosion rate of the aluminum foil for a battery according to claim 3, wherein the solvent is one of EC and DEC, EC and EMC, EC and DMC, PC and DEC, PC and EMC, PC and DMC binary mixed solvent.
5. The method for measuring the corrosion rate of an aluminum foil for a battery according to claim 3, wherein the electrolyte is LiFSI or LiPF 6 Or LiTFSI with LiPF 6 Is a mixture of (a) and (b).
6. The method for measuring the corrosion rate of an aluminum foil for a battery according to claim 5, wherein the LiFSI and LiPF are 6 Or LiTFSI and LiPF 6 The mass ratio of (2) is 0.2-5.
7. The method for measuring the corrosion rate of an aluminum foil for a battery according to claim 1, wherein the development area of the auxiliary electrode is not smaller than the development area of the aluminum foil to be measured.
8. The method for measuring the corrosion rate of an aluminum foil for a battery according to claim 1 or 7, wherein the auxiliary electrode is a metallic lithium strip or an artificial graphite negative electrode sheet; the artificial graphite negative electrode sheet is subjected to lithium intercalation by an electrochemical method before the test is started, so that the potential of a balance electrode is 80-100 mV (vs. Li/Li) + )。
9. The method for measuring the corrosion rate of the aluminum foil for a battery according to claim 1 or 2, wherein the voltage control range for charging is 0 to 5V and the charging time is 24 to 72 hours.
10. The method for measuring the corrosion rate of the aluminum foil for the battery according to claim 1 or 2, wherein the aluminum foil to be measured is required to ensure that the ambient moisture is less than or equal to 1000 ppm, the oxygen content is less than or equal to 1000 ppm and the ambient temperature is 20-30 ℃ in the corrosion rate measuring process.
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| CN (1) | CN116818643A (en) |
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2023
- 2023-07-14 CN CN202310864455.7A patent/CN116818643A/en active Pending
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