CN105734598B - The environment protection chemical surface treatment method of aluminium foil in lithium battery flexible packaging aluminum plastic film - Google Patents
The environment protection chemical surface treatment method of aluminium foil in lithium battery flexible packaging aluminum plastic film Download PDFInfo
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- CN105734598B CN105734598B CN201610185706.9A CN201610185706A CN105734598B CN 105734598 B CN105734598 B CN 105734598B CN 201610185706 A CN201610185706 A CN 201610185706A CN 105734598 B CN105734598 B CN 105734598B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
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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
- H01M50/10—Primary casings, jackets or wrappings of a single cell or a single battery
-
- 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 discloses the environment protection chemical surface treatment methods of aluminium foil in lithium battery flexible packaging aluminum plastic film, include the following steps：（1）Make aluminium foil surface degreasing with lye and remove the oxidation film of aluminium foil surface, lye solute is KOH, K2CO3、K3PO4Any one of or the mixture more than any two, concentration be 0.025 ~ 0.1mol/L；（2）Clear water washes down；（3）Aluminium foil surface roughness is improved with acid solution and forms the stabilization passivating film of hydrofluoric acid corrosion resistance, and acid solution solute is HNO3、HCI、H2SO4, any one of HF or the mixture more than any two, concentration be 0.5 ~ 3mol/L；（4）Clear water washes down.Ingredient used in this method is environment-friendly materials, is free of chromium, safer, and can be continuously recycled, and cost is lower, and obtained aluminium foil has more excellent resistant to hydrogen fluoric acid corrosive nature, and corresponding aluminum plastic film obtained has higher peeling force.
Description
Technical field
The present invention relates to the environmental protection of aluminium foil in the surface treatment method of aluminium foil more particularly to lithium battery flexible packaging aluminum plastic film
Chemical method for treating surface.
Background technique
The nineties in last century, Sony have invented commercial lithium ion battery.In more than the 20 years later times, lithium from
Sub- battery achieves rapid development, application throughout mobile communication, laptop, video camera, electric car, people according to satellite,
The numerous areas closely related to human life such as energy storage.
Aluminum plastic film is current lithium ion battery flexible packing material widely applied on the market, because it has every wet, oxygen barrier, easy
The advantages that machine-shaping, good encapsulation adhesion.The structure of aluminum plastic film is multilayer film, including intermediate aluminium foil layer, aluminium foil smooth surface side
Glue-line and polypropylene layer, the glue-line of aluminium foil dull surface side and the composite materials such as nylon layer or PET.Lithium ion battery Organic Electricity
Salt (LiPF6) in solution liquid, which easily reacts with steam, generates the hydrofluoric acid with strong corrosive.Flexible package as battery
Material, aluminum plastic film inside（Aluminium foil smooth surface side）It is directly to be contacted with electrolyte.When the hydrofluoric acid in electrolyte penetrates poly- third
It can be acted on aluminium foil smooth surface after alkene layer and glue-line and aluminium foil is caused to be perforated, therefore aluminium foil must have higher hydrofluoric acid corrosion resistance
Performance.Meanwhile the safety in order to guarantee soft-package battery, glue-line wants sufficiently large with the intensity that is bonded of aluminium foil smooth surface, therefore aluminium
It foil surface should roughness with higher.In order to reach two above requirement, the aluminium foil in aluminum plastic film must before applying bond paper facing
Certain surface treatment must be passed through.Widespread practice is to do surface passivating treatment to aluminium foil with the acid solution containing chromium, and pass through at present
The aluminium foil surface for crossing the processing of liquid containing chromium passivating will be with the presence of sexavalence chromium compounds.It is well known that Cr VI has severe toxicity, chromate
Using also strictly being limited by countries in the world.If passivating solution or aluminum plastic film containing chromium, which are dealt with improperly, to cause pole to natural environment
Big pollution, and then seriously endanger the health of people.
Therefore, exist in face of people to the increasingly soaring of lithium ion battery demand and at this stage in aluminum plastic film manufacturing process
Huge latency environment threaten, there is an urgent need to develop a kind of more environmentally friendly and efficient aluminium foil surface processing methods.
Summary of the invention
The present invention for it is existing in the prior art aluminium foil surface is handled when very big dirt can be caused to natural environment
The defects of contaminating, and then seriously endangering people's health provides aluminium foil in the new lithium battery flexible packaging aluminum plastic film of one kind
Environment protection chemical surface treatment method.
In order to solve the above-mentioned technical problem, the invention is realized by the following technical scheme：
The environment protection chemical surface treatment method of aluminium foil, includes the following steps in lithium battery flexible packaging aluminum plastic film：
（1）Base extraction：Aluminium foil is handled with lye, make aluminium foil surface degreasing and removes the oxide of aluminium foil surface
Film, the solute of the lye are KOH, K2CO3、K3PO4Any one of or the mixture more than any two, the lye
Concentration be 0.025 ~ 0.1mol/L；
（2）Aluminium foil after base extraction is washed down with clear water；
（3）Acid solution processing：Aluminium foil is handled with acid solution, improve the roughness of aluminium foil surface and is formed in aluminium foil surface
The stabilization passivating film of hydrofluoric acid corrosion resistance, the solute of the acid solution are HNO3、HCl、H2SO4, any one of HF or any two
Above mixture, the concentration of the acid solution are 0.5 ~ 3mol/L；
（4）It will treated that aluminium foil is washed down with clear water by acid solution.
Wherein base extraction can make aluminium foil surface degreasing and remove the oxidation film of aluminium foil surface, prevent aluminium foil surface
Grease, oxidation film etc. influence the passivation effect when processing of aluminium foil acid solution, are washed down to aluminium foil with clear water after base extraction is complete, can
The remaining lye of aluminium foil surface is removed, so that the acid solution in lye and subsequent step be avoided to neutralize and influence aluminium foil surface processing
Effect, acid solution processing can be improved the roughness of aluminium foil surface and form stablizing for hydrofluoric acid corrosion resistance in aluminium foil surface and be passivated
Film, the intensity that is bonded on the one hand being able to ascend between glue-line and aluminium foil, on the other hand can make aluminium foil have hydrofluoric acid corrosion resistance
Performance, acid solution again washes down aluminium foil with clear water after having handled, and the remaining acid solution of aluminium foil surface can be removed, to avoid residual
The acid solution stayed influences the bonding effect between subsequent aluminium foil and glue-line.
This method is environment-friendly materials in acid solution used, lye formula when handling aluminium foil surface, is free of chromium
Element during processing will not pollute natural environment, thus human health will not be damaged, it is safer,
And treated lye and acid solution can continuously be recycled, cost is lower.By this method treated aluminium foil, compared to by existing
The aluminium foil for having technical treatment to obtain has more excellent resistant to hydrogen fluoric acid corrosive nature, and made of the aluminium foil obtained with this method
Aluminum plastic film made of the aluminium foil that aluminum plastic film obtains compared with prior art has higher peeling force.
Preferably, in lithium battery flexible packaging aluminum plastic film described above aluminium foil environment protection chemical surface treatment method,
The step（1）In, the mode of the base extraction is immersion treatment, and the alkali liquid temperature is 10 ~ 40 DEG C, when immersion
Between be 10 ~ 60s.By this immersion treatment mode, enable to aluminium foil surface degreasing and oxidation film removably more thorough
Bottom, to promote aluminium foil surface treated performance.
Preferably, in lithium battery flexible packaging aluminum plastic film described above aluminium foil environment protection chemical surface treatment method,
The step（1）In, the mode of the base extraction is spray process, and the alkali liquid temperature is 30 ~ 60 DEG C, when spray
Between be 20 ~ 90s.Spray process mode can reach while saving lye and make aluminium foil surface degreasing and remove aluminium foil surface
The purpose of oxidation film, more saving cost.
Preferably, in lithium battery flexible packaging aluminum plastic film described above aluminium foil environment protection chemical surface treatment method,
The step（3）In, it also include additive in the acid solution, the concentration of the additive is 0.005 ~ 0.03mol/
L, the additive are KMnO4、KClO4、K2S2O8、TiCl4、FeCl3、ZnCl2、ZnSO4、ZnF2Any one of or wantonly two
Kind or more mixture.The above additive can be improved effect when acid solution processing, so that aluminium foil surface is with higher coarse
Degree, and the passivating film for forming hydrofluoric acid corrosion resistance is more stable.
Preferably, in lithium battery flexible packaging aluminum plastic film described above aluminium foil environment protection chemical surface treatment method,
The step（3）In, the mode of the described acid solution processing is immersion treatment, and the acid liquor temperature is 10 ~ 40 DEG C, when immersion
Between be 10 ~ 60s.By this immersion treatment mode, enable to acid solution more uniform when handling aluminium foil surface.
Preferably, in lithium battery flexible packaging aluminum plastic film described above aluminium foil environment protection chemical surface treatment method,
The step（3）In, the mode of the described acid solution processing is spray process, and the acid liquor temperature is 30 ~ 60 DEG C, when spray
Between be 20 ~ 90s.Spray process mode can achieve the purpose that surface treatment, more saving cost while saving acid solution.
Preferably, in lithium battery flexible packaging aluminum plastic film described above aluminium foil environment protection chemical surface treatment method,
The step（2）And step（4）In, the mode that the clear water washes down is spray or impregnates, and the water temperature is room temperature ~ 60
℃.Spray or immersion way can relatively rapid remove the lye or acid solution of aluminium foil surface, and more save cost.
The present invention has the advantages that：
（1）It is environment-friendly materials in acid solution used, lye formula, low in cost, the environmental pollution for avoiding chromium is asked
Topic, will not damage the health of people, safer；
（2）There is excellent resistant to hydrogen fluoric acid corrosive nature by this method treated aluminium foil, have after aluminum plastic film is made
Very high peeling force；
（3）Treatment process is simple, easily operated, low energy consumption, and acid solution and lye can be recycled continuously, and cost is more
It is low；
（4）Treatment process controllability is strong, can be integrated with subsequent handling, carries out the large-scale production of aluminum plastic film.
Detailed description of the invention
Fig. 1 is the optical microphotograph amplification of " O " state aluminium foil in the embodiment of the present invention 1 Jing Guo chemically treated model 8021
Picture；
Fig. 2 is the optical microphotograph amplification of " O " state aluminium foil of the model 8021 without any processing in the embodiment of the present invention 1
Picture；
Fig. 3 is the optical microphotograph amplification of " O " state aluminium foil in the embodiment of the present invention 2 Jing Guo chemically treated model 8079
Picture；
Fig. 4 is the optical microphotograph amplification of " O " state aluminium foil of the model 8079 without any processing in the embodiment of the present invention 2
Picture.
Specific embodiment
Present invention is further described in detail for 1-4 and specific embodiment with reference to the accompanying drawing, but they are not to this
The limitation of invention：
Embodiment 1
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH and 0.03mol/L containing 0.025mol/L
K2CO3Aqueous solution, acid solution be specially the HNO containing 0.5mol/L3With the aqueous solution of the HF of 0.5mol/L, also it is added in acid solution
The additive of 0.01mol/L, the additive are KMnO4Aqueous solution.
Adjustment alkali liquid temperature first is to 25 DEG C, by aluminium foil to be processed（" O " state aluminium foil of model 8021）It is dipped to lye
In and keep 30s, then take out and aluminium foil and rinsed well with 50 DEG C of deionized water from lye, then the aluminium foil is dipped to temperature
In the acid solution that degree is 30 DEG C and 30s is kept, aluminium foil is finally taken out from acid solution and is rinsed well with 50 DEG C of deionized water.Wherein
It can be spray or immersion with the mode that deionized water is rinsed well.
It will dry by above-mentioned chemically treated aluminium foil and do morphology analysis.Fig. 1 is to pass through above-mentioned chemically treated aluminium foil
Optical microphotograph amplification picture, as a comparison, Fig. 2 be the original aluminium foil without any processing（" O " state aluminium of model 8021
Foil）Optical microphotograph amplification picture.Obviously, after above-mentioned chemical treatment, there is the pitting largely corroded in aluminium foil surface, thick
Rough degree significantly becomes larger, this is beneficial to the adhesion strength for promoting it with glue-line.
In order to evaluate the adhesion strength by above-mentioned chemically treated aluminium foil and glue-line, and gluing and patch are carried out to the aluminium foil
PP layers of processing are closed so that aluminum plastic film is made.Gained aluminum plastic film is cut into width to be the band-like of 15mm and do tensile test, in 50mm/
Under the peeling rate of min, the peeling force of the aluminum plastic film is 11.9N.Again by the aluminum plastic film through lithium-ion battery electrolytes at 80 DEG C
Under the conditions of impregnate 4h after, peeling force is still 5.2N.As a comparison, aluminum plastic film will be made without chemically treated original aluminium foil
Afterwards, two peeling forces of the aluminum plastic film are respectively 7.8N and 0N.Obviously, the bonding of the aluminium foil after above-mentioned chemical treatment and glue-line
Intensity is able to satisfy the requirement of soft bag lithium ionic cell safety compared to greatly promoting without above-mentioned chemically treated original aluminium foil.
Embodiment 2
The lye and acid solution of processing aluminium foil are prepared, lye is specially the K of KOH, 0.02mol/L containing 0.01mol/L2CO3
With the K of 0.02mol/L3PO4Aqueous solution, acid solution be specially the HNO containing 0.4mol/L3, 0.2mol/L H2SO4、0.4mol/L
HF aqueous solution, the additive of 0.02mol/L is also added in acid solution, which is FeCl3Aqueous solution.
It will adjust first to 50 DEG C of lye and be sprayed to aluminium foil to be processed（" O " state aluminium foil of model 8079）Surface is simultaneously protected
60s is held, is then rinsed well aluminium foil with 50 DEG C of deionized water, then 50 DEG C of acid solution is sprayed to the aluminium foil surface and is kept
40s is finally rinsed well with 50 DEG C of deionized water.It can be wherein spray or leaching with the mode that deionized water is rinsed well
Bubble.
It will dry by above-mentioned chemically treated aluminium foil and do morphology analysis.Fig. 3 is its optical microphotograph amplification picture, as
Comparison, Fig. 4 are the original aluminium foil without any processing（" O " state aluminium foil of model 8079）.Obviously, by above-mentioned chemical treatment
There is the pitting largely corroded in aluminium foil surface afterwards, and degree of roughness also significantly becomes larger, this is beneficial to promote itself and glue-line
Adhesion strength.
It is same as Example 1, tensile test is done to aluminum plastic film made of the aluminium foil after above-mentioned chemical treatment, is obtained
The peeling force of the aluminum plastic film is 12.0N, is 5.4N by peeling force of the aluminum plastic film after lithium-ion battery electrolytes impregnate.As
Comparison, after aluminum plastic film is made without chemically treated original aluminium foil, corresponding two peeling forces are respectively 7.5N and 0N.Obviously,
The adhesion strength of aluminium foil and glue-line after above-mentioned chemical treatment is greatly promoted, and soft bag lithium ionic cell peace is able to satisfy
The requirement of full property.
Embodiment 3
The lye and acid solution of processing aluminium foil are prepared, lye is specially the aqueous solution of the KOH containing 0.025mol/L, acid solution tool
Body is the HNO containing 3mol/L3Aqueous solution, the additive of 0.03mol/L is also added in acid solution, which is KMnO4Water
Solution.
Adjustment alkali liquid temperature first is to 40 DEG C, by above-mentioned aluminium foil to be processed（" O " state aluminium foil of model 8021）It is dipped to
In lye and 10s is kept, aluminium foil is then taken out from lye and is rinsed well with 60 DEG C of deionized water, then the aluminium foil is impregnated
In the acid solution for being 30 DEG C to temperature and 30s is kept, aluminium foil is finally taken out from acid solution and is rinsed well with 60 DEG C of deionized water.
It can be wherein spray or immersion with the mode that deionized water is rinsed well.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11N, then its peeling force is still 4.5N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 1.
Embodiment 4
The lye and acid solution of processing aluminium foil are prepared, lye is specially the K of KOH, 0.05mol/L containing 0.01mol/L3PO4
Aqueous solution, acid solution be specially the HNO containing 1.5mol/L3Aqueous solution, the additive of 0.02mol/L is also added in acid solution,
The additive is KClO4Aqueous solution.
Adjustment alkali liquid temperature first is to 35 DEG C, by above-mentioned aluminium foil to be processed（" O " state aluminium foil of model 8021）It is dipped to
In lye and 25s is kept, aluminium foil is then taken out from lye and is rinsed well with 50 DEG C of deionized water, then the aluminium foil is impregnated
In the acid solution for being 30 DEG C to temperature and 35s is kept, aluminium foil is finally taken out from acid solution and is rinsed well with 50 DEG C of deionized water.
It can be wherein spray or immersion with the mode that deionized water is rinsed well.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.4N, then its peeling force is still 4.8N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 1.
Embodiment 5
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.02mol/L containing 0.01mol/L
K2CO3, 0.04mol/L K3PO4Aqueous solution, acid solution be specially the HNO containing 0.45mol/L3, 0.05mol/L HF it is water-soluble
Liquid, the additive of 0.01mol/L is also added in acid solution, which is ZnSO4Aqueous solution.
Adjustment alkali liquid temperature first is to 10 DEG C, by aluminium foil to be processed（" O " state aluminium foil of model 8021）It is dipped to lye
In and keep 60s, then take out and aluminium foil and rinsed well with 50 DEG C of deionized water from lye, then the aluminium foil is dipped to temperature
In the acid solution that degree is 25 DEG C and 40s is kept, aluminium foil is finally taken out from acid solution and is rinsed well with 50 DEG C of deionized water.Wherein
It can be spray or immersion with the mode that deionized water is rinsed well.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 12.3N, then its peeling force is still 5.5N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 1.
Embodiment 6
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.02mol/L containing 0.01mol/L
K2CO3, 0.04mol/L K3PO4Aqueous solution, acid solution be specially the HNO containing 1.2mol/L3, 0.04mol/L HF it is water-soluble
Liquid, the additive of 0.01mol/L is also added in acid solution, which is TiCl4Aqueous solution.
It will adjust first to 60 DEG C of lye and be sprayed to aluminium foil to be processed（" O " state aluminium foil of model 8021）Surface is simultaneously protected
20s is held, is then rinsed well aluminium foil with 40 DEG C of deionized water, then 60 DEG C of acid solution is sprayed to the aluminium foil surface and is kept
40s is finally rinsed well with 40 DEG C of deionized water.It can be wherein spray or leaching with the mode that deionized water is rinsed well
Bubble.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.2N, then its peeling force is still 4.7N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 1.
Embodiment 7
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.01mol/L containing 0.01mol/L
K2CO3, 0.03mol/L K3PO4Aqueous solution, acid solution be specially the HNO containing 1.5mol/L3, 0.05mol/L HF it is water-soluble
Liquid, the additive of 0.02mol/L is also added in acid solution, which is FeCl3Aqueous solution.
It will adjust first to 50 DEG C of lye and be sprayed to aluminium foil to be processed（" O " state aluminium foil of model 8021）Surface is simultaneously protected
40s is held, is then rinsed well aluminium foil with 50 DEG C of deionized water, then 50 DEG C of acid solution is sprayed to the aluminium foil surface and is kept
50s is finally rinsed well with 50 DEG C of deionized water.It can be wherein spray or leaching with the mode that deionized water is rinsed well
Bubble.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.4N, then its peeling force is still 4.9N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 1.
Embodiment 8
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.02mol/L containing 0.01mol/L
K2CO3, 0.03mol/L K3PO4Aqueous solution, acid solution be specially the HNO containing 1mol/L3, 0.03mol/L HF aqueous solution,
The additive of 0.015mol/L is also added in acid solution, additive is respectively the KMnO of 0.01mol/L4With 0.005mol/L's
ZnF2。
It will adjust first to 30 DEG C of lye and be sprayed to aluminium foil to be processed（" O " state aluminium foil of model 8021）Surface is simultaneously protected
90s is held, is then rinsed well aluminium foil with 40 DEG C of deionized water, then 40 DEG C of acid solution is sprayed to the aluminium foil surface and is kept
70s is finally rinsed well with 40 DEG C of deionized water.It can be wherein spray or leaching with the mode that deionized water is rinsed well
Bubble.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.3N, then its peeling force is still 4.6N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 1.
Embodiment 9
The lye and acid solution of processing aluminium foil are prepared, lye is specially the aqueous solution of the KOH containing 0.1mol/L, and acid solution is specific
For the HNO containing 2mol/L3Aqueous solution, the additive of 0.03mol/L is also added in acid solution, which is KMnO4It is water-soluble
Liquid.
Adjustment alkali liquid temperature first is to 30 DEG C, by aluminium foil to be processed（" O " state aluminium foil of model 8079）It is dipped to lye
In and keep 35s, then take out and aluminium foil and rinsed well with 50 DEG C of deionized water from lye, then the aluminium foil is dipped to temperature
In the acid solution that degree is 10 DEG C and 60s is kept, aluminium foil is finally taken out from acid solution and is rinsed well with 50 DEG C of deionized water.Wherein
It can be spray or immersion with the mode that deionized water is rinsed well.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.8N, then its peeling force is still 5.0N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 2.
Embodiment 10
The lye and acid solution of processing aluminium foil are prepared, lye is specially the K of KOH, 0.05mol/L containing 0.01mol/L3PO4
Aqueous solution, acid solution be specially the HNO containing 1.5mol/L3Aqueous solution, the additive of 0.02mol/L is also added in acid solution,
The additive is KClO4Aqueous solution.
Adjustment alkali liquid temperature first is to 35 DEG C, by aluminium foil to be processed（" O " state aluminium foil of model 8079）It is dipped to lye
In and keep 30s, then take out and aluminium foil and rinsed well with 50 DEG C of deionized water from lye, then the aluminium foil is dipped to temperature
In the acid solution that degree is 40 DEG C and 10s is kept, aluminium foil is finally taken out from acid solution and is rinsed well with 50 DEG C of deionized water.Wherein
It can be spray or immersion with the mode that deionized water is rinsed well.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.9N, then its peeling force is still 4.9N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 2.
Embodiment 11
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.02mol/L containing 0.01mol/L
K2CO3, 0.04mol/L K3PO4Aqueous solution, acid solution be specially the HNO containing 1mol/L3, 0.05mol/L HF aqueous solution,
The additive of 0.005mol/L is also added in acid solution, which is ZnSO4Aqueous solution.
Adjustment alkali liquid temperature first is to 25 DEG C, by aluminium foil to be processed（" O " state aluminium foil of model 8079）It is dipped to lye
In and keep 35s, then taken out from lye and aluminium foil and use room temperature（15℃）Deionized water under state is rinsed well, then should
Aluminium foil is dipped in the acid solution that temperature is 25 DEG C and keeps 40s, and aluminium foil is finally taken out from acid solution and uses room temperature（15℃）State
Under deionized water rinse well.It can be wherein spray or immersion with the mode that deionized water is rinsed well.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 12.4N, then its peeling force is still 5.4N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 2.
Embodiment 12
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.02mol/L containing 0.01mol/L
K2CO3, 0.04mol/L K3PO4Aqueous solution, acid solution be specially the HNO containing 1.2mol/L3, 0.04mol/L HF it is water-soluble
Liquid, the additive of 0.01mol/L is also added in acid solution, which is TiCl4Aqueous solution.
It will adjust first to 60 DEG C of lye and be sprayed to aluminium foil to be processed（" O " state aluminium foil of model 8079）Surface is simultaneously protected
30s is held, is then rinsed well aluminium foil with 50 DEG C of deionized water, then 60 DEG C of acid solution is sprayed to the aluminium foil surface and is kept
20s is finally rinsed well with 50 DEG C of deionized water.It can be wherein spray or leaching with the mode that deionized water is rinsed well
Bubble.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.1N, then its peeling force is still 4.5N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 2.
Embodiment 13
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.01mol/L containing 0.01mol/L
K2CO3, 0.03mol/L K3PO4Aqueous solution, acid solution be specially the H containing 1.5mol/L2SO4, 0.05mol/L HF it is water-soluble
Liquid, the additive of 0.02mol/L is also added in acid solution, which is FeCl3Aqueous solution.
It will adjust first to 50 DEG C of lye and be sprayed to aluminium foil to be processed（" O " state aluminium foil of model 8079）Surface is simultaneously protected
45s is held, is then rinsed well aluminium foil with 50 DEG C of deionized water, then 50 DEG C of acid solution is sprayed to the aluminium foil surface and is kept
60s is finally rinsed well with 50 DEG C of deionized water.It can be wherein spray or leaching with the mode that deionized water is rinsed well
Bubble.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.5N, then its peeling force is still 4.9N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 2.
Embodiment 14
The lye and acid solution of processing aluminium foil are prepared, lye is specially KOH, 0.02mol/L containing 0.01mol/L
K2CO3, 0.03mol/L K3PO4Aqueous solution, acid solution be specially HCl, 0.03mol/L containing 2mol/L HF aqueous solution,
The additive of 0.01mol/L is also added in acid solution, which is ZnF2Aqueous solution.
It will adjust first to 40 DEG C of lye and be sprayed to aluminium foil to be processed（" O " state aluminium foil of model 8079）Surface is simultaneously protected
60s is held, room temperature is then used（15℃）Deionized water under state rinses aluminium foil well, then 30 DEG C of acid solution is sprayed to the aluminium
Foil surface simultaneously keeps 90s, finally uses room temperature（15℃）Deionized water under state is rinsed well.It is wherein rinsed with deionized water dry
Net mode can be spray or immersion.
Aluminum plastic film will be made and do tensile test by above-mentioned chemically treated aluminium foil, and obtain the peeling force of the aluminum plastic film
For 11.2N, then its peeling force is still 4.7N after lithium-ion battery electrolytes impregnate by the aluminum plastic film.
Other embodiment in the present embodiment is the same as embodiment 2.
In short, the foregoing is merely presently preferred embodiments of the present invention, made by all ranges according to the present patent application patent
Deng variation and modification, it is all covered by the present invention.
Claims (1)
1. the environment protection chemical surface treatment method of aluminium foil in lithium battery flexible packaging aluminum plastic film, it is characterised in that：Including following step
Suddenly：
（1）Base extraction：Aluminium foil is handled with lye, make aluminium foil surface degreasing and removes the oxidation film of aluminium foil surface,
The solute of the lye is KOH, K2CO3、K3PO4In any two more than mixture, the concentration of the lye is
0.025~0.1mol/L；The mode of the base extraction is immersion treatment or spray process, the lye temperature of the immersion treatment
Degree is 10 ~ 40 DEG C, and soaking time is 10 ~ 60s, and the alkali liquid temperature of the spray process is 30 ~ 60 DEG C, spray time is 20 ~
90s；
（2）Aluminium foil after base extraction is washed down with clear water, the mode that the clear water washes down is spray or impregnates, described
The water temperature of clear water is room temperature ~ 60 DEG C；
（3）Acid solution processing：Aluminium foil is handled with acid solution, improve the roughness of aluminium foil surface and is formed in aluminium foil surface hydrogen resistant
The stabilization passivating film of fluoric acid corrosion, the solute of the acid solution are HNO3、HCl、H2SO4, more than any two in HF mixing
Object, the concentration of the acid solution are 0.5 ~ 3mol/L, also include additive in the acid solution, the concentration of the additive
0.005 ~ 0.03mol/L, the additive are KMnO4、KClO4、K2S2O8、TiCl4、FeCl3、ZnCl2、ZnSO4、ZnF2In
Any or more than any two mixture；The mode of the acid solution processing is immersion treatment or spray process, the leaching
The acid liquor temperature of bubble processing is 10 ~ 40 DEG C, and soaking time is 10 ~ 60s, and the acid liquor temperature of the spray process is 30 ~ 60 DEG C, spray
The leaching time is 20 ~ 90s；
（4）Will by acid solution, treated that aluminium foil is washed down with clear water, the mode that the clear water washes down is spray or impregnates, described
The water temperature of clear water is room temperature ~ 60 DEG C.
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| CN107699894B (en) * | 2017-10-09 | 2020-09-29 | 山西沃特海默新材料科技股份有限公司 | Chemical corrosion preparation method of microporous battery aluminum foil |
| CN108613919A (en) * | 2018-04-28 | 2018-10-02 | 东莞市卓越新材料科技有限公司 | A kind of test method of aluminum plastic film electrolyte resistance corrosion |
| CN109897565A (en) * | 2018-12-19 | 2019-06-18 | 上海奥威科技开发有限公司 | The anti-battery aluminum plastic film for crossing envelope |
| JP7183395B2 (en) * | 2019-03-29 | 2022-12-05 | 富士フイルム株式会社 | Aluminum foil, method for producing aluminum foil, current collector, lithium ion capacitor, and lithium ion battery |
| CN113381102A (en) * | 2021-05-07 | 2021-09-10 | 厦门大学 | Aluminum plastic film with excellent heat dissipation performance for battery packaging and preparation method thereof |
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