CN114552133B - Preparation method of negative electrode lug with surface inert metal coating and lithium battery - Google Patents
Preparation method of negative electrode lug with surface inert metal coating and lithium battery Download PDFInfo
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- CN114552133B CN114552133B CN202111080670.5A CN202111080670A CN114552133B CN 114552133 B CN114552133 B CN 114552133B CN 202111080670 A CN202111080670 A CN 202111080670A CN 114552133 B CN114552133 B CN 114552133B
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- inert metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/50—Current conducting connections for cells or batteries
- H01M50/531—Electrode connections inside a battery casing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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 relates to the technical field of lithium batteries, and discloses a preparation method of a negative electrode lug with an inert metal coating on the surface and a lithium battery, which are characterized in that the thickness of the inert metal coating is 1-2 mu m, and the preparation method comprises the following steps: (1) substrate pretreatment: cleaning the substrate with alkali liquor, then pickling the substrate, and refining the crystal grains on the surface of the substrate after cleaning and drying; (2) Nickel plating: plating nickel on the surface of the substrate obtained in the step (1), cleaning and drying, and then removing the surface tensile stress to obtain a nickel-plated substrate; (3) inert metal plating: plating an inert metal layer on the surface of the nickel-plated substrate obtained in the step (2), cleaning and drying, and then removing the surface tensile stress to obtain a substrate with a surface inert metal coating; and (4) manufacturing a tab: and heating and pressing the base material with the surface plated with the inert metal and the tab adhesive to obtain the negative electrode tab. According to the invention, the inert metal layer is plated on the surface of the tab, so that the erosion of the electrolyte to the tab can be avoided, and the durability and reliability of the battery are improved.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a negative electrode lug with an inert metal coating on the surface and a lithium battery.
Background
In order to avoid the corrosion of electrolyte to the tab, prevent the separation of tab glue and tab conductor and avoid the leakage of soft-package lithium battery, the current conductor of the negative tab for the lithium ion battery is usually formed by compounding a copper sheet with nickel plated surface and tab glue. The nickel plating layer is favorable for welding the tab and preventing the oxidation of the copper tab. During preparation, a layer of nickel is plated on the copper conductor uniformly, and then the middle part of the conductor is compounded with upper tab glue. The nickel layer on the copper surface is easily corroded by the electrolyte, and particularly under the conditions of high temperature and high humidity, the corrosion is accelerated. After the nickel layer is corroded and removed, the tab adhesive and the copper conductor are peeled off, so that leakage of the soft-package battery is caused, and great potential safety hazards are brought. In the long-term use of the lithium ion battery, the leakage caused by the separation of the negative electrode lug structure occupies a large proportion, and brings great risk to the application of the soft package battery. Particularly in special fields such as military, aviation, aerospace and the like, the working environment is bad, the requirements on the service life and reliability of the lithium battery are very high, the risk of leakage of the soft package battery in long-term use is higher, and the problem of leakage needs to be further solved.
Publication number CN109285987A discloses a flexible package lithium ion battery tab and a manufacturing method thereof, wherein the flexible package lithium ion battery tab comprises a conductor and an insulating layer, and the conductor is arranged between the two insulating layers; the conductor is one of an aluminum strip, a copper strip or a nickel-plated copper strip, the conductor is in a cuboid shape, the width of the conductor is D, D is more than or equal to 100mm, and the edges of the conductor in the width direction are provided with chamfers; the purpose of chamfering the two ends of the conductor is to reduce the step drop of the section, so that the fusion of PP and the end face is better when the two ends of the conductor with the width of 280 mm are thermally compounded with PP glue, and the sealing performance of the battery is ensured. But the problem of liquid leakage caused by corrosion of the nickel plating layer cannot be solved.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a negative electrode lug with an inert metal coating on the surface and a lithium battery. An inert metal layer is plated on the surface of the electrode lug, so that the electrode lug can be prevented from being corroded by electrolyte; the preparation method is simple, and the surface coating has strong binding force.
The specific technical scheme of the invention is as follows: the preparation method of the negative electrode lug with the surface inert metal coating, wherein the thickness of the inert metal coating is 1-2 mu m, comprises the following steps:
(1) Pretreatment of a matrix: cleaning the substrate with alkali liquor, then pickling the substrate, and refining the crystal grains on the surface of the substrate after cleaning and drying;
(2) Nickel plating: plating nickel on the surface of the substrate obtained in the step (1), cleaning and drying, and then removing the surface tensile stress to obtain a nickel-plated substrate;
(3) Inert metal plating: plating an inert metal layer on the surface of the nickel-plated substrate obtained in the step (2), cleaning and drying, and then removing the surface tensile stress to obtain a substrate with a surface inert metal coating;
(4) Manufacturing a tab: and heating and pressing the base material with the surface plated with the inert metal and the tab adhesive to obtain the negative electrode tab.
In the step (1), alkali liquor is treated to remove organic matters and the like on the surface, acid washing is performed to take out a surface oxide layer, and a substrate surface manager is thinned to enhance the binding force between the substrate and the coating and reduce the grain size of the coating. In the step (2), due to poor binding force of the plating layer between the base material and the inert metal, the nickel plating layer is transited in the scheme, the nickel plating layer is deposited on the surface of the base material to have certain surface tensile stress, the surface tensile stress is removed, the surface performance of the nickel plating layer is improved, and in addition, the nickel plating layer also has the effect of being used as a second protective layer. In the step (3), the inert metal plating layer is deposited on the surface of the nickel layer and has a certain surface tensile stress, and the removal of the surface tensile stress is beneficial to improving the surface performance of the inert metal plating layer, enhancing the surface compactness and improving the corrosion resistance of the inert metal plating layer, and the common material of the matrix is copper.
Preferably, in the step (1), the refinement treatment method of the crystal grains on the surface of the substrate is that haok energy is refined, the surface roughness of the refined substrate is Ra0.1-0.5, and the grain size grade is 10-12 grade.
The surface roughness of the base material can be controlled through haok energy treatment, so that the binding force of the coating is ensured; the grains of the surface layer of the substrate which can be treated by haok are thinned, so that the binding force between the substrate and the plating layer can be enhanced; changing the surface stress distribution, removing the influence of surface tensile stress, and preventing the plating layer from falling off.
Preferably, in the step (1), the pH of the alkali liquor is 9-12, and the pH of the acid liquor is 2-4.
Preferably, in the step (2), the surface tensile stress removing mode is haok energy treatment, and the surface roughness of the nickel-plated substrate after the tensile stress is removed is Ra0.1-0.5.
The nickel plating layer can control the surface roughness of the nickel plating layer through haok energy treatment, improve the density, strengthen the binding force with the base material, prevent the nickel plating layer from falling off; changing the surface stress distribution, and guaranteeing the binding force with the next inert metal coating; the grains of the surface layer of the nickel plating layer which can be processed by haok are thinned, and the binding force between the nickel plating layer and the inert metal plating layer can be enhanced.
Preferably, in the step (2), the nickel plating mode on the surface of the substrate is electrochemical plating or chemical plating; the thickness of the nickel layer is 1-10 mu m.
Preferably, in the step (3), the inert metal of the inert metal plating layer is one of Au, pt or Pd.
Preferably, the plating method of the inert metal is chemical plating, specifically, the nickel plating base material obtained in the step (2) is immersed in an inert metal salt solution added with a reducing agent and a dispersing agent, and the reaction is carried out for 60-180min at the temperature of 25-100 ℃; the molar concentration ratio of the inert metal salt solution, the reducing agent and the dispersing agent is 0.1-1:0.1-0.2:0.01-0.05.
Preferably, the inert metal salt solution is one of chloroauric acid, chloroplatinic acid and chloropalladac acid, the reducing agent is citric acid or vitamin C, and the dispersing agent is polyvinylpyrrolidone.
Preferably, in the step (3), the surface tensile stress removing mode is haok energy treatment.
The haok energy treatment of the inert metal coating can strengthen the binding force with the nickel layer, improve the surface density and prevent the inert metal coating from falling.
The invention also provides a lithium battery manufactured by the negative electrode lug with the surface inert metal coating prepared by any method.
Compared with the prior art, the invention has the beneficial effects that:
1. an inert metal layer is plated on the surface of the electrode lug, so that the electrode lug can be prevented from being corroded by electrolyte;
2. the preparation method is simple, and the surface coating has strong binding force;
3. the surface properties of the matrix and the plating layer are easy to regulate and control, and the transition of the nickel layer plays a role in double-layer protection, so that the durability and the reliability of the battery are improved.
Detailed Description
The invention is further described below with reference to examples. The devices, reagents and methods referred to in this invention, unless otherwise specified, are those well known in the art.
Example 1
(1) Pretreatment of a matrix: cleaning the surface of a matrix by using NaOH solution with pH of 10, then pickling the matrix by using HCl solution with pH of 3, carrying out possible treatment on the substrate after cleaning and drying, and refining surface grains, wherein the surface roughness of the obtained substrate is Ra0.3, and the grain size grade is 10;
(2) Nickel plating: plating nickel on the surface of the base material obtained in the step (1) by an electrochemical method, cleaning and drying, and then removing the surface tensile stress by using haok to obtain a nickel-plated base material with the surface roughness of Ra0.3 and the thickness of 5 mu m;
(3) Inert metal plating: immersing the nickel-plated substrate obtained in the step (2) into a mixed solution of vitamin C, polyvinylpyrrolidone and chloroauric acid in a molar concentration ratio of 0.1:0.02:0.5, reacting for 100min at 50 ℃, cleaning and drying, and removing surface tensile stress by using hawk to obtain a substrate with a surface inert metal coating; the thickness of the inert metal coating is 1.5 mu m;
(4) Manufacturing a tab: and heating and pressing the base material with the surface plated with the inert metal and the tab adhesive to obtain the negative electrode tab.
Example 2
(1) Pretreatment of a matrix: cleaning the surface of a matrix by using NaOH solution with pH of 10, then pickling the matrix by using HCl solution with pH of 3, carrying out possible treatment on the substrate after cleaning and drying, and refining surface grains to obtain the substrate with surface roughness of Ra0.1 and grain size grade of 12;
(2) Nickel plating: plating nickel on the surface of the base material obtained in the step (1) by an electrochemical method, cleaning and drying, and then removing the surface tensile stress by using haok to obtain a nickel-plated base material with the surface roughness of Ra0.1 and the thickness of 5 mu m;
(3) Inert metal plating: immersing the nickel-plated substrate obtained in the step (2) into a mixed solution of vitamin C, polyvinylpyrrolidone and chloroauric acid in a molar concentration ratio of 0.1:0.02:0.5, reacting for 100min at 50 ℃, cleaning and drying, and removing surface tensile stress by using hawk to obtain a substrate with a surface inert metal coating; the thickness of the inert metal coating is 1.5 mu m;
(4) Manufacturing a tab: and heating and pressing the base material with the surface plated with the inert metal and the tab adhesive to obtain the negative electrode tab.
Example 3
(1) Pretreatment of a matrix: cleaning the surface of a matrix by using NaOH solution with pH of 10, then pickling the matrix by using HCl solution with pH of 3, carrying out possible treatment on the substrate after cleaning and drying, and refining surface grains, wherein the surface roughness of the obtained substrate is Ra0.5, and the grain size grade is 10;
(2) Nickel plating: plating nickel on the surface of the base material obtained in the step (1) by an electrochemical method, cleaning and drying, and then removing the surface tensile stress by using haok to obtain a nickel-plated base material with the surface roughness of Ra0.5 and the thickness of 5 mu m;
(3) Inert metal plating: immersing the nickel-plated substrate obtained in the step (2) into a mixed solution of vitamin C, polyvinylpyrrolidone and chloroauric acid in a molar concentration ratio of 0.1:0.02:0.5, reacting for 100min at 50 ℃, cleaning and drying, and removing surface tensile stress by using hawk to obtain a substrate with a surface inert metal coating; the thickness of the inert metal coating is 1.5 mu m;
(4) Manufacturing a tab: and heating and pressing the base material with the surface plated with the inert metal and the tab adhesive to obtain the negative electrode tab.
Comparative example 1
Comparative example 1 is a common nickel plated tab.
Performance test: packaging an aluminum plastic film, making into a bag, injecting 100mL of lithium hexafluorophosphate electrolyte and 1000ppm of water, soaking the negative electrode lug obtained in comparative example 1 and the electrode lugs obtained in examples 1-3 in 85' C for 30, 60 and 90 days, and testing the stripping force of the electrode lug adhesive, wherein if the stripping force is less than 1N/mm, the use requirement cannot be met, and the battery is easy to leak, and compared with the following:
the negative electrode tab obtained in comparative example 1 and the tabs obtained in examples 1 to 3 were respectively prepared into 50AH ternary soft package lithium ion batteries, and the 50AH ternary soft package lithium ion batteries were placed in a 70 ℃ high temperature cabinet, stored for 60 days and 120 days, and observed for leakage, and compared as follows.
Tab | Tunneling ratio 1 | Example 1 | Example 2 | Example 3 |
For 60 days | Leakage at negative electrode lug | No leakage and good package | No leakage and good package | No leakage and good package |
120 days | No leakage and good package | No leakage and good package | No leakage and good package |
Therefore, compared with the common lug, the acid resistance of the lug is greatly improved, and the reliability of the soft-package battery using the lug is greatly improved.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent structural transformation made according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (8)
1. The preparation method of the negative electrode lug with the surface inert metal coating is characterized in that the thickness of the inert metal coating is 1-2 mu m, and the preparation method comprises the following steps:
(1) Pretreatment of a matrix: cleaning the substrate with alkali liquor, then pickling the substrate, and refining the crystal grains on the surface of the substrate after cleaning and drying; the refining treatment method of the crystal grains on the surface of the base material is that haok can be refined, the roughness of the surface of the refined base material is Ra0.1-0.5, and the grain size grade is 10-12 grade;
(2) Nickel plating: plating nickel on the surface of the substrate obtained in the step (1), cleaning and drying, and then removing the surface tensile stress to obtain a nickel-plated substrate; the surface tensile stress is removed by haok energy treatment, and the surface roughness of the nickel plating base material is Ra0.1-0.5 after the tensile stress is removed;
(3) Inert metal plating: plating an inert metal layer on the surface of the nickel-plated substrate obtained in the step (2), cleaning and drying, and then removing the surface tensile stress to obtain a substrate with a surface inert metal coating;
(4) Manufacturing a tab: and heating and pressing the base material with the surface plated with the inert metal and the tab adhesive to obtain the negative electrode tab.
2. The process according to claim 1, wherein in step (1), the pH of the alkaline solution is 9 to 12 and the pH of the acid solution used in the acid washing is 2 to 4.
3. The method of claim 1, wherein in step (2), the substrate surface is plated with nickel by electrochemical plating or electroless plating; the thickness of the nickel layer is 1-10 mu m.
4. The method of claim 1, wherein in step (3), the inert metal of the inert metal plating layer is one of Au, pt or Pd.
5. The method according to claim 4, wherein the plating method of the inert metal is electroless plating, specifically, the nickel-plated substrate obtained in the step (2) is immersed in an inert metal salt solution added with a reducing agent and a dispersing agent, and reacted for 60-180min at 25-100 ℃; the molar concentration ratio of the inert metal salt solution, the reducing agent and the dispersing agent is 0.1-1:0.1-0.2:0.01-0.05.
6. The method of claim 5, wherein the inert metal salt solution is one of chloroauric acid, chloroplatinic acid, and chloropalladate, the reducing agent is citric acid or vitamin C, and the dispersing agent is polyvinylpyrrolidone.
7. The method of claim 1, wherein in step (2), the surface tensile stress is removed by haok energy treatment.
8. A lithium battery fabricated from the negative electrode tab with a surface inert metal coating prepared by the method of any one of claims 1-7.
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