CN109148895A - A kind of method of the electrochemistry roughening treatment of anode current collector of lithium ion battery - Google Patents
A kind of method of the electrochemistry roughening treatment of anode current collector of lithium ion battery Download PDFInfo
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- CN109148895A CN109148895A CN201811015634.9A CN201811015634A CN109148895A CN 109148895 A CN109148895 A CN 109148895A CN 201811015634 A CN201811015634 A CN 201811015634A CN 109148895 A CN109148895 A CN 109148895A
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- roughening
- aluminium
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- lithium ion
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/72—Grids
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
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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
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- ing And Chemical Polishing (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The present invention relates to etching technique fields, the method of the electrochemistry roughening treatment of specifically a kind of anode current collector of lithium ion battery, the following steps are included: firstly, aluminum foil of anode current collector of lithium ion battery asperities is carried out electrochemical polishing treatment in bipolar chamber cationic membrane electrolytic cell；Then, in bipolar chamber cationic membrane electrolytic cell, using the cheap sodium silicate solution of abundance as coarsening solution, aluminium foil surface is roughened using constant-potential electrolysis mode；Finally, the roughening aluminium collector for containing dense oxide aluminium film in surface can be obtained in the aluminium foil cleaning, drying after roughening；The present invention is compared with the existing technology, only need one-step electrolysis that can prepare the good aluminium foil of roughening effect, this method is efficient, easy, pollution-free, it may be directly applied to industrialized production, be able to solve dry etching to the high request of equipment and wet etching carve serious, Graph Control and fidelity is poor, selectivity is high.
Description
[technical field]
The present invention relates to etching technique field, the electrochemistry of specifically a kind of anode current collector of lithium ion battery is roughened
The method of processing.
[background technique]
In current field of semiconductor manufacture, the material that aluminum metal is commonly electrically interconnected as one kind is used to form gold
Belong to interconnection line or contact pad designed etc., is widely used in integrated circuit.And with the development of technology and people require mention
Height, in semiconductor chip manufacturing industry, chip line width is smaller and smaller, and integrated level is higher and higher, and the requirement to board is also higher and higher.
Aluminium etching is one of main etching technics of field of semiconductor manufacture, and metal layer uses fine aluminium, aluminum bronze, aluminium silicon, aluminium silicon mostly
The alloys such as copper, and the main function of aluminium etching is exactly by designed metal connecting line pattern transfer to product, thus the company of realization
The effect of line or grid.
Conventional method etching is mainly dry etching and wet etching, but its disadvantage is obvious, and dry etching equipment is wanted
Ask high therefore at high cost, such as patent 201610718552.5；And wet etching carve it is serious, poor to the controlling of figure,
It cannot be used for small characteristic size, a large amount of chemical waste fluid, such as patent 201310263046.8 can be generated.And chemical etching
Side etching phenomenon can be overcome when normal etching scheme etching speed is slow, etching is deep serious etc. to determine, such as patent
200610172613.9。
Lithium ion battery plays the role of conductive and bonding with cathode metal collector, but due to will receive strong oxidizing property
The corrosion of organic electrolyte, causes electrical property to decline；Adhesion property between smooth aluminium foil and active material layer is poor, therefore both
Oxidation resistance may be implemented again to increase the adhesive force of collector to be the selection to accompany each other.And patent
201611117185.X carries out method of roughening using jet-propelled chemistry, and coarsening rate is slow, and coarsening solution contains heavy metal ion, specially
Benefit 201310627045.7 is roughened in the form of the conversion fluid of acid & alkali liquid cleaning, the ion containing high oxidation impregnates, not only dirty
Dye is serious, and technique is cumbersome.
Therefore, in order to pursue high-environmental, efficient method of roughening, if can by means of the principle of aluminium foil chemical etching,
It is roughened using bipolar chamber cationic membrane electrolytic cell one-step method, and it is cheap that raw material sources are enriched, and heavy metal free ion
Pollution, will have very important significance.
[summary of the invention]
A kind of electrification of anode current collector of lithium ion battery is provided present invention aim to solve above-mentioned deficiency
The method for learning roughening treatment is able to solve dry etching and carves serious, Graph Control to the high request of equipment and wet etching
Property and fidelity it is poor, selectivity is high, and heavy metal free ionic soil, and raw material sources are abundant, cheap.
The method for designing a kind of electrochemistry roughening treatment of anode current collector of lithium ion battery to achieve the above object, including
Following steps: 1) firstly, by aluminum foil of anode current collector of lithium ion battery asperities in bipolar chamber cationic membrane electrolytic cell, electricity is carried out
Chemical polishing processing；2) then, in bipolar chamber cation-exchange membrane electrolytic cell, using sodium silicate solution as coarsening solution, using perseverance
Pressure electrolysis mode is roughened aluminium foil surface；3) finally, the aluminium foil cleaning, drying after roughening is contained densification to get to surface
The roughening aluminium collector of aluminum oxide film.
Further, in step 1), in the processing step of electrochemical polishing treatment, the preparation method of polishing fluid is to incite somebody to action
120ml phosphoric acid, 32ml sulfuric acid, 8ml ethylene glycol, add water to 400ml.
Further, in step 1), in the processing step of electrochemical polishing treatment, polishing process is current density 100-
300mA/cm2, 90 DEG C are heated to, is polished under magnetic stirring.
Further, in step 2), constant-potential electrolysis roughening treatment processing step are as follows: be electrolysed in bipolar chamber cation-exchange membrane
In slot, using sodium silicate solution as anolyte, using sodium hydroxide solution as catholyte, it is with aluminum foil of anode current collector of lithium ion battery
Anode is electrolysed 10-30min at 20-60 DEG C by the way of constant-potential electrolysis using inert electrode as cathode.
Further, in step 2), the cationic membrane that the bipolar chamber cation-exchange membrane uses is perfluorosulfonic acid ion
Exchange membrane, the concentration of the sodium silicate solution are 0.0001-0.1mol/L, and the concentration of the sodium hydroxide solution is 0.0001-
0.1mol/L, the inert electrode are stainless steel electrode or Ti electrode, and the voltage of the constant-potential electrolysis is 10-400V.
Further, the cleaning, drying processing step in step 3), after roughening are as follows: wash the aluminium foil of roughening with dehydrated alcohol
It washs, until pH close to neutrality, then puts it into 60-100 DEG C of drying in air dry oven.
The present invention compared with the existing technology, has the advantages that
(1) present invention is since the cationic membrane used in preparation process is with certain selective penetrated property, especially
Nafion series perfluorinated sulfonic acid cation-exchange membrane can allow the Na+ ion in anode chamber to enter cathode chamber through ionic membrane, from
And influence of the Na+ ionic impurity to roughening effect is eliminated；
(2) reaction time of the invention is short, as can be seen that its electrolytic preparation time is less than 0.5h from specific embodiment,
The good aluminium foil plus plate current-collecting body of roughening effect can be obtained, roughening treatment is simple, so that preparation cost reduces；
(3) present invention is due to only needing one-step electrolysis that can prepare the good aluminium foil of roughening effect, this method efficiently, it is easy,
It is pollution-free, it may be directly applied to industrialized production；
(4) plus plate current-collecting body obtained by this method greatly improves the corrosion resistance of electrolyte, and this collector
Irregular pit is included, the adhesive property of collector and active material layer is increased.
[Detailed description of the invention]
Fig. 1 is the SEM figure of untreated aluminium foil in the embodiment of the present invention 1；
Fig. 2 is the SEM figure of aluminium foil after electrochemical polish in the embodiment of the present invention 1；
Fig. 3 is the SEM figure of the aluminium of the roughening of 50V obtained in the embodiment of the present invention 1；
Fig. 4 is the SEM figure of the aluminium of the roughening of 100V obtained in the embodiment of the present invention 1；
Fig. 5 is the SEM figure of the aluminium of the roughening of 150V obtained in the embodiment of the present invention 1；
Fig. 6 is the SEM figure of the aluminium of the roughening of 200V obtained in the embodiment of the present invention 1；
Fig. 7 is the SEM figure of the aluminium of the roughening of 250V obtained in the embodiment of the present invention 1；
Fig. 8 is the SEM figure of the roughening of 300V obtained in the embodiment of the present invention 1；
Fig. 9 is the SEM figure of the aluminium of the roughening of room temperature obtained in the embodiment of the present invention 2；
Figure 10 is the SEM figure of the aluminium of 35 DEG C of roughening obtained in the embodiment of the present invention 2；
Figure 11 is the SEM figure of the aluminium of 55 DEG C of roughening obtained in the embodiment of the present invention 2.
[specific embodiment]
The present invention provides a kind of method of the electrochemistry roughening treatment of anode current collector of lithium ion battery, specifically include as
Lower step: aluminum foil of anode current collector of lithium ion battery asperities is subjected to electrochemical polish in bipolar chamber cationic membrane electrolytic cell first
Processing, using the cheap sodium silicate solution of abundance as coarsening solution, uses then in bipolar chamber cationic membrane electrolytic cell
Constant-potential electrolysis mode is roughened aluminium foil surface, finally by the aluminium foil cleaning, drying after roughening, surface can be obtained and contain cause
The roughening aluminium collector of close aluminum oxide film.
Wherein, in the processing step of electrochemical polishing treatment, the preparation of polishing fluid: 120ml phosphoric acid+32ml sulfuric acid+8ml second
Glycol adds water to 400ml；Polishing process: 100~300mA/cm of current density2, 90 DEG C are heated to, is polished under magnetic stirring.
Constant-potential electrolysis roughening treatment processing step is as follows, in dual chamber cationic membrane electrolytic cell, using sodium silicate solution as anolyte, with hydrogen
Sodium hydroxide solution is catholyte, using aluminum foil of anode current collector of lithium ion battery as anode, using inert electrode as cathode, using constant pressure
The mode of electrolysis is electrolysed 10-30min at 20-60 DEG C；Wherein, the cationic membrane that dual chamber cation-exchange membrane uses is perfluor sulphur
Acid ion exchange membrane；The concentration of sodium silicate solution is 0.0001-0.1mol/L；Sodium hydroxide solution is that concentration is 0.0001-
0.1mol/L；Inert electrode is stainless steel electrode, Ti electrode；The voltage of constant-potential electrolysis is 10-400V.Cleaning after roughening is dried
Dry processing step is as follows: the aluminium foil of roughening being washed with dehydrated alcohol, until then pH puts it into forced air drying close to neutrality
60-100 DEG C of drying in case.
The present invention is made combined with specific embodiments below further explained below:
Perfluorinated sulfonic acid cation-exchange membrane used in various embodiments of the present invention is the Nafion of DuPont Corporation's production
212 type cation-exchange membrane of perfluorinated sulfonic acid.
Embodiment 1
A kind of method of the electrochemistry roughening treatment of anode current collector of lithium ion battery, specifically comprises the following steps:
(1) processing step of electrochemical polishing treatment is as follows.The preparation of polishing fluid: 120ml phosphoric acid+32ml sulfuric acid+8ml second
Glycol adds water to 400ml；Polishing process: current density 100-300mA/cm2, 90 DEG C are heated to, is polished under magnetic stirring
15min。
(2) using sodium silicate solution as anolyte, using sodium hydroxide solution as catholyte, using aluminium flake as anode, with inertia electricity
Extremely cathode is electrolysed 10-30min at normal temperature by the way of constant-potential electrolysis；Wherein, inert electrode is DSA titanium net；Sodium metasilicate
Solution concentration is 0.00075mol/L；Sodium hydroxide solution is that concentration is 0.001mol/L；Cationic membrane be perfluorinated sulfonic acid sun from
Proton exchange；Electrolysis temperature is 25 DEG C of room temperature；Electrolysis time is 15min；The voltage of the constant-potential electrolysis is respectively 50,100,
150,200,250,300V；
(3) after being electrolysed, with washes of absolute alcohol aluminium flake, until pH is close to neutrality；Then air dry oven is put it into
In 70 DEG C of dry 1h.
As shown in Figure 1, 2, more preferably to show its experiment effect, the aluminium foil after original aluminium foil and electrochemical polish is also tested
SEM。
As shown in figure 3, the SEM figure after the aluminium roughening of 15min is electrolysed at 25 DEG C for 50V constant-potential electrolysis.
As shown in figure 4, the SEM figure after the aluminium roughening of 15min is electrolysed at 25 DEG C for 100V constant-potential electrolysis.
As shown in figure 5, the SEM figure after the aluminium roughening of 15min is electrolysed at 25 DEG C for 150V constant-potential electrolysis.
As shown in fig. 6, the SEM figure after the aluminium roughening of 15min is electrolysed at 25 DEG C for 200V constant-potential electrolysis.
As shown in fig. 7, the SEM figure after the aluminium roughening of 15min is electrolysed at 25 DEG C for 250V constant-potential electrolysis.
As shown in figure 8, the SEM figure after the aluminium roughening of 15min is electrolysed at 25 DEG C for 300V constant-potential electrolysis.
Embodiment 2
Electrochemical polish and post-processing step are same as Example 1.
Steps are as follows for electrochemistry roughening process: using phosphoric acid solution as anolyte, using sodium hydroxide solution as catholyte, with aluminium
Piece is anode, using inert electrode as cathode, is electrolysed 10-30min at room temperature by the way of constant-potential electrolysis；Wherein, inertia electricity
Extremely DSA titanium net；Phosphoric acid solution pH ≈ 6；Sodium hydroxide solution is that concentration is 0.001mol/L；Cationic membrane is perfluorinated sulfonic acid sun
Amberplex；Electrolysis temperature is 25 DEG C, 35 DEG C, 55 DEG C of room temperature；Electrolysis time is 15min；The voltage of constant-potential electrolysis is 300V.
As shown in figure 9, the aluminium directional etching SEM figure of 15min is electrolysed at 25 DEG C for 300V constant-potential electrolysis.
As shown in Figure 10, the aluminium directional etching SEM figure of 15min is electrolysed at 35 DEG C for 300V constant-potential electrolysis.
As shown in figure 11, the aluminium directional etching SEM figure of 15min is electrolysed at 55 DEG C for 300V constant-potential electrolysis.
In conclusion the present invention is due to using cation-exchange membrane electrolysis method, constant pressure 10-300V electrolysis, electrolysis temperature
Degree is 20-60 DEG C, electrolysis time 10-30min, the available roughening aluminium foil to work well, and the electrolytic preparation time
No more than 0.5h, final resulting aluminium foil roughening effect is good.Meanwhile with the increase of voltage, erosional surface is wider, and roughening effect is got over
It is good；Cooling, it is advantageous to experiment effect.
The present invention is simultaneously not limited to the embodiments described above, other any without departing from spiritual essence and principle of the invention
Changes, modifications, substitutions, combinations, simplifications made by lower, should be equivalent substitute mode, are included in protection model of the invention
Within enclosing.
Claims (6)
1. a kind of method of the electrochemistry roughening treatment of anode current collector of lithium ion battery, which comprises the following steps:
1) firstly, by aluminum foil of anode current collector of lithium ion battery asperities in bipolar chamber cationic membrane electrolytic cell, electrochemistry is carried out
Polishing treatment；
2) then, in bipolar chamber cation-exchange membrane electrolytic cell, using sodium silicate solution as coarsening solution, using constant-potential electrolysis mode
Aluminium foil surface is roughened；
3) finally, the aluminium foil cleaning, drying after roughening to be contained to the roughening aluminium collector of dense oxide aluminium film to surface.
2. the method as described in claim 1, it is characterised in that: in step 1), in the processing step of electrochemical polishing treatment, throw
The preparation method of light liquid is, by 120ml phosphoric acid, 32ml sulfuric acid, 8ml ethylene glycol, to add water to 400ml.
3. method according to claim 2, it is characterised in that: in step 1), in the processing step of electrochemical polishing treatment, throw
Light technology is current density 100-300mA/cm2, 90 DEG C are heated to, is polished under magnetic stirring.
4. the method as described in claim 1, it is characterised in that: in step 2), constant-potential electrolysis roughening treatment processing step are as follows:
In bipolar chamber cation-exchange membrane electrolytic cell, using sodium silicate solution as anolyte, using sodium hydroxide solution as catholyte, with lithium from
Sub- battery plus plate current-collecting body aluminium foil is that anode is electrolysed at 20-60 DEG C by the way of constant-potential electrolysis using inert electrode as cathode
10-30min。
5. method as claimed in claim 4, it is characterised in that: in step 2), what the bipolar chamber cation-exchange membrane used
Cationic membrane is perfluorinated sulfonic acid ion exchange membrane, and the concentration of the sodium silicate solution is 0.0001-0.1mol/L, the hydroxide
The concentration of sodium solution is 0.0001-0.1mol/L, and the inert electrode is stainless steel electrode or Ti electrode, the constant-potential electrolysis
Voltage be 10-400V.
6. the method as described in claim 1, it is characterised in that: the cleaning, drying processing step in step 3), after roughening are as follows: will
The aluminium foil of roughening is washed with dehydrated alcohol, until pH close to neutrality, then puts it into 60-100 DEG C of drying in air dry oven.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114094053A (en) * | 2021-11-05 | 2022-02-25 | 惠州锂威新能源科技有限公司 | Tail aluminum foil processing method for improving safety test of lithium ion battery |
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| JP2017066513A (en) * | 2015-09-29 | 2017-04-06 | 日立金属株式会社 | Manufacturing method of aluminum foil and aluminum foil |
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| CN101285208A (en) * | 2007-04-12 | 2008-10-15 | 深圳市比克电池有限公司 | Coursing and hole-distributing method at aluminum foil surface for lithium ion secondary battery |
| CN102534577A (en) * | 2010-12-10 | 2012-07-04 | 比亚迪股份有限公司 | Roughening liquid and preparation method thereof, and acrylonitrile-butadiene-styrene terpolymer surface electroplating method |
| JP2017066513A (en) * | 2015-09-29 | 2017-04-06 | 日立金属株式会社 | Manufacturing method of aluminum foil and aluminum foil |
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| CN114094053A (en) * | 2021-11-05 | 2022-02-25 | 惠州锂威新能源科技有限公司 | Tail aluminum foil processing method for improving safety test of lithium ion battery |
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