CN108611676A - A kind of the electrochemical corrosion preparation method and its micropore copper foil of micropore battery copper foil - Google Patents
A kind of the electrochemical corrosion preparation method and its micropore copper foil of micropore battery copper foil Download PDFInfo
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- CN108611676A CN108611676A CN201810723105.8A CN201810723105A CN108611676A CN 108611676 A CN108611676 A CN 108611676A CN 201810723105 A CN201810723105 A CN 201810723105A CN 108611676 A CN108611676 A CN 108611676A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
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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
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/103—Other heavy metals copper or alloys of copper
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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
- C23G1/20—Other heavy metals
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Abstract
The present invention a kind of the electrochemical corrosion preparation method and its micropore copper foil of micropore battery copper foil, belong to the preparing technical field of battery copper foil, technical solution is：It carries out as steps described below：Surface clean is carried out to the battery copper foil after rolling and dispels lubricant；Battery copper foil after cleaning is totally immersed into chemical corrosion liquid：The chemical corrosion liquid includes the HCl of 0.5 1.5mol/L, the C of 0.5 2mol/L2H2O4, the NH of 0.1 0.5mol/L4Cl, the FeCl of 0.1 1mol/L3, 0.1 0.5mol/L AgCl2, using etching tank as cathode, battery copper foil is corroded as anode, additional 6 64V direct currents, and residence time of the battery copper foil in the corrosive liquid is in 20 ~ 120s；Battery copper foil after corrosion cleans remained on surface liquid, drying；The present invention can be widely applied to the manufacturing field of lithium battery micropore copper foil.
Description
Technical field
The present invention a kind of the electrochemical corrosion preparation method and its micropore copper foil of micropore battery copper foil, belong to battery copper foil
Preparing technical field.
Background technology
New material and clean energy resource are all the prior development directions of State-level, and lithium ion battery is in current energy storage technology
Most widely used energy storage battery core, it is the target that the whole world is pursued to improve battery core energy storage density, and battery core energy density carries
Height depends on the progress of its positive and negative electrode material, but is also bonded with the positive and negative anodes collector of lithium ion battery, positive and negative anodes
The progress of the materials such as agent, electrolyte and diaphragm is related.
The cathode of lithium ion battery is by copper foil and the negative electrode slurry being coated on（Graphite slurry, silicon-carbon slurry or metatitanic acid
Lithium slurry）It is formed.People are generally increased using the method for roughening copper foil surface viscous between copper foil and negative electrode slurry at present
Power is tied, but the technique can not reach desired effect.Negative electrode slurry and copper foil are when winding column battery and cycle charge-discharge
Can all occur separation problem in the process, and then lead to product qualification rate first mate reduction, service life first mate shortening and battery capacity
Decaying is apparent.
In order to improve the bond state between negative copper foil collector and negative electrode slurry, some enterprises of Japan and TaiWan, China
Industry develops micropore copper foil and micropore copper foil, be all prepared on both positive and negative anodes collector foils are every square centimeter nine it is logical
The diameter in hole, each through-hole is about 1mm.But the copper foil and copper foil prepared by them must automatically be produced using special battery
Line, reason are on original battery automatic assembly line, using such through-hole diameter in the copper foil or copper foil of 1mm, meeting
There is the back side and ooze slurry phenomenon, influences the coating of another side.
Invention content
Overcome the deficiencies in the prior art of the present invention, it is therefore an objective to it is rotten to provide a kind of electrochemistry of high-performance lithium battery micropore copper foil
Lose preparation method.
In order to solve the above technical problems, the technical solution adopted in the present invention is：
The first step carries out surface clean to the battery copper foil after rolling and dispels surface attachments.
Battery copper foil after cleaning is totally immersed into chemical corrosion liquid by second step：The corrosive agent includes following mole
The solution of concentration：The C of the HCl of 0.5-1.5mol/L, 0.5-2mol/L2H2O4, the NH of 0.1-0.5mol/L4Cl, 0.1-1mol/L
FeCl3, 0.1-0.5mol/L AgCl2, using etching tank as cathode, battery copper foil as anode, additional 6-64V direct currents into
Row corrosion, residence time of the battery copper foil in the corrosive liquid is in 20 ~ 120s.
Third walks, and remained on surface liquid is cleaned to the battery copper foil after corrosion.
4th step, drying.
It is provided between third step and the 4th step：Brightening processing step.
Brightening processing brightening liquid include：The CrO of 2-5g/L3, 1-7g/L Na2Cr2O7•2H2O, 0.1-1.5g/L
NaF。
Cleaning solution in the first step includes the Na of NaOH, 10-70g/L of 5-30g/L2CO3, 10-40g/L
Na3PO4, time >=6s in cleaning solution.
Third step in cleaning solution include：The formula of cleaning solution：The Na of 0.4 ~ 0.8kg2SO4, 0.5 ~ 1kg CaSO4、0.1
The citric acid of ~ 0.3kg, which is dissolved in 1L water, to be configured.
It is cleaned after brightening processing, the formula of cleaning solution：The Na of 0.4 ~ 0.8kg2SO4, 0.5 ~ 1kg CaSO4、0.1~
The citric acid of 0.3kg, which is dissolved in 1L water, to be configured.
In second step, battery copper foil upper and lower surface is immersed in corrosive liquid simultaneously, the type of flow for making corrosive liquid to recycle
It is flowed in copper foil upper and lower surface, keeps upper and lower surface corrosion uniform to reach.
The micropore copper foil prepared using the electrochemical corrosion preparation method.On the micropore copper foil is every square centimeter
There is blind hole of 500 ~ 3000 diameters in 1 ~ 20 μm of through-hole and 10 ~ 100 diameters at 10 ~ 50 μm；And in the upper following table of copper foil
Face is uniform-distribution with deep 1 ~ 3 μm, wide 1 ~ 5 μm and long tens microns of erosion trace, and the adherency of negative electrode slurry and copper foil can be solved perfectly
Power problem makes micropore copper foil surface smoothness higher, without overlap, burr, and hole due to the hole and indentation of particular size
It is irregular arc transition with copper foil surface junction, 90 ° of right angles is not present, Li dendrite in charge and discharge process can be effectively prevent
Appearance, extend the service life of battery；In addition, micro-pore shape is also different, the micropore copper foil obtained by electrochemical erosion method
On hole be in irregular shape, aperture size changes in a certain range, and the diameter of each hole also has in different directions
Changed, the hole of this irregular shape is more advantageous to the cohesive force improved between copper foil and negative electrode slurry.
The copper that the main component of copper foil is 99.98%, remaining is impurity.In terms of microcosmic angle, in the process of copper foil sintering
In, numerous fine copper particles forms a large amount of nucleus of crystal.When they develop into crystal grain and gradually grow up to when meeting with regard to shape
At crystal boundary, distribution of the impurity on copper foil is concentrated on crystal boundary, during corroding to copper foil, HCl's
It is acid stronger, in conjunction with C2H2O4Selectivity corrodes the impurity element being enriched on crystal boundary in advance, due to the process in corrosion impurity
In, a part of hydrogen ion is consumed, so, when further corroding to copper particle, the aperture of generation is more small, corrosion
NH in liquid4Cl ingredients generate gas during corrosion, take away the partial impurities in copper foil, make the copper foil purity after corrosion
Higher coordinates villaumite to improve electric conductivity in corrosive agent, reconciles acid ingredient therein, makes the aperture corroded on copper foil
It is more various, and through-hole and blind hole are produced simultaneously, keep finally formed micropore copper foil stronger as the performance of cathode, corrosive agent
In contain a certain amount of villaumite, can buffered etch entirety corrosive nature, keep the aperture edge of corrosion more mellow and full；Ag is to hand over
Boundary's acid, therefore the solution containing Ag is aobvious weakly acidic, the corrosivity by forming gradient can make copper foil when corroding to copper foil
The aperture of upper standby corrosion and shape are more diversified, in addition to the formation of micropore and blind hole, have been formed simultaneously the quarter of irregular shape
Trace.Using the method for galvano-cautery, using etching tank as cathode, battery copper foil carries out rotten as anode, additional 6-64V direct currents
Erosion keeps the consistency of performance of product more preferable convenient for control product quality and speed of production, meet it is various under the conditions of production.It is rotten
Micropore battery copper foil after erosion can be used as negative electrode of lithium ion battery collector.
Compared with prior art the invention has the advantages that：
Chemical mordant of the present invention is the corrosion being specifically applied to as cathode of lithium battery copper foil, for the microcosmic of negative copper foil
Structure, the chemical mordant combine the ratio of strong acid, middle strong acid, weakly acidic salt and villaumite in proportioning, break crystalline substance
The influence of boundary's surface impurity enrichment forms aperture in copper foil surface and shape is more various on the basis of reconciling corrosive nature
The hole and slight crack of change make the copper foil surface adhesion strength after corrosion significantly improve, and compared with primary battery copper foil, micropore copper foil resists
Tensile strength is close with the tensile strength of native copper foil；The resistivity of micropore copper foil also has almost no change, but makes lithium-ion electric simultaneously
The capacity in pond improves 8-10%.
Using micropore copper foil as cathode of lithium battery collector, the negative electrode slurry being coated on is not easily to fall off, meanwhile, make
Two surfaces, can be by lithium particle both not completely through or without completely isolated inside and outside micropore copper foil, and prevents other particles
Or particle passes through, and after lithium ion is by negative current collector, can move about in entire lithium battery, improves lithium ion activity, improves
Battery capacity, integral with copper foil coated in negative material above, adhesive force significantly improves.
It is gradient acid solutions different from general acid ＆ alkali liquid corrosive liquid, being used in caustic solution of the present invention that the present invention, which uses,
Coordinate chloride salt compound as corrosive liquid, can achieve the effect that during corrosion the higher copper foil of corrosion strength and
The degree of energy control corrosion rate, extent of reaction relaxation combine, and copper surface is made to form the microcellular structure of multiple aperture and shape, corrosive liquid
In silver ion or mercury ion, on the one hand to corrode its reconcile facilitation, on the other hand these ions can enter perforated membrane in
It is fixed in the follow-up process, plays a part of improvement to copper surface property.
There are 500 ~ 3000 diameters in 1 ~ 20 μm of through-hole and 10 ~ 100 on micropore copper foil of the invention is every square centimeter
Blind hole of the diameter at 10 ~ 50 μm；And it is uniform-distribution with deep 1 ~ 3 μm, wide 1 ~ 5 μm and tens microns long in the upper and lower surface of copper foil
Trace is lost, the adhesion strength problem of negative electrode slurry and copper foil can be solved perfectly, due to the hole and indentation of particular size, make micropore copper foil
Surface flatness higher is irregular arc transition without overlap, burr, and hole and copper foil surface junction, is not present 90 °
Right angle can effectively prevent the appearance of Li dendrite in charge and discharge process, extend the service life of battery；In addition, micro-pore shape
Different, the hole on micropore copper foil obtained by electrochemical erosion method is in irregular shape, and aperture size is in a certain range
Variation, the diameter of each hole are also varied from different directions, and the hole of this irregular shape is more advantageous to raising copper
Cohesive force between foil and negative electrode slurry.And existing production technology is varied without, easy to spread, it is not only suitable for single side coating
Suitable for dual coating.
Description of the drawings
Fig. 1 is the micro image after corrosion cell copper foil of the present invention.
Fig. 2 is the stress strain curve figure after corrosion cell copper foil of the present invention.
Specific implementation mode
Embodiment 1
A kind of electrochemical corrosion preparation method of high-performance lithium battery micropore copper foil, follows the steps below：
1）Surface clean is carried out to the battery copper foil after rolling and dispels lubricant：The composition of first cleaning solution is 10g/L
The Na of NaOH, 10g/L2CO3, 40g/L Na3PO4, by the copper foil after rolling by the first cleaning solution, in the first cleaning solution
The time of holding is 8s.
2）The copper foil cleaned is pressed into chemical corrosion liquid：The composition of chemical corrosion liquid is：1.5mol/L HCl、1mol/L
C2H2O4、0.1mol/L NH4Cl、1mol/L FeCl3, 0.1mol/L AgCl2Using etching tank as cathode, copper foil as anode,
Additional 48V direct currents are corroded.Residence time of the copper foil in the corrosive agent in 45s, in this stage, it is ensured that following table on copper foil
Face is immersed in corrosive liquid simultaneously, and the type of flow for making corrosive liquid to recycle is flowed in copper foil upper and lower surface, is made with reaching
Upper and lower surface corrosion is uniform.
3）Copper foil after corrosion is cleaned：The composition of second cleaning solution is the Na for taking 0.4kg2SO4, 0.8kg
CaSO4, 0.1kg citric acid, be dissolved in the water of 1L and being formed jointly, copper foil upper and lower surface use nozzle sprinkling second cleaning
Liquid is cleaned.
4）Brightization processing：The composition of brightening liquid is the CrO of 2g/L3, 1g/L Na2Cr2O7•2H2O, the NaF of 0.5g/L,
Surface brightening processing is carried out to the copper foil after cleaning.
5）Copper foil after brightening is cleaned again：The copper foil after brightening is cleaned again using the second cleaning solution.
6）Drying and processing：The copper foil cleaned again is dried, temperature is 250 DEG C.
7）Finished product is wound.
Embodiment 2
1）Surface cleaning processing is carried out to battery copper foil：Rolling battery copper foil surface has attachment, they have not copper foil pore-forming
Profit influences, and need to clean copper foil by the first cleaning solution.First cleaning solution is by 15g/L NaOH, 15g/L
Na2CO3、15g/L Na3PO4Composition.By the copper foil after rolling by the first cleaning solution, the time kept in the first cleaning solution
It is 7s.
2）Copper foil after cleaning is totally immersed into the chemical corrosion liquid, makes corrosive liquid with the type of flow that recycles in copper
Foil upper and lower surface flows, and keeps upper and lower surface corrosion uniform to reach.Using etching tank as cathode, copper foil is as anode, additional 6V
Direct current is corroded, and direct current can also be set as to the safe voltages such as 36V, 64V, and etching time 20s can will also corrode
Time is set as 60s, 100s, 120s；It is 1.5mol/L HCl, 1.2mol/L that the chemical corrosion liquid, which contains molar concentration,
C2H2O4、0.3mol/L NH4Cl、1mol/L FeCl3, 0.5mol/L AgCl2。
3）Remained on surface liquid is cleaned to the copper foil after corrosion, the cleaning solution that when cleaning selects is by 0.6kg Na2SO4、
0.6kg CaSO4, 0.2kg citric acids be dissolved in 1L water, be formulated.
4）Surface-brightening processing is carried out to the copper foil after cleaning, the brightening liquid of brightening processing includes：The CrO of 5g/L3、
The Na of 5g/L2Cr2O7•2H2O, the NaF of 0.4g/L.
5）It is cleaned after brightening processing, the cleaning solution that when cleaning selects is by 0.6kg Na2SO4、0.6kg CaSO4、
0.2kg citric acids are dissolved in 1L water, are formulated.
6）The temperature of drying and processing, drying is 300 DEG C.
Fig. 1 is the micro image after corrosion cell copper foil of the present invention, from Fig. 1 as can be seen that micropore copper foil inside and outside two
Surface is not both completely through or without completely isolated, adhesive force integral coated in positive electrode above and copper foil
It significantly improves.
Fig. 2 is the stress strain curve figure after corrosion cell copper foil of the present invention, and curve 1 is that the stretching of primary battery copper foil is bent in figure
Line, curve 2 are the stress strain curve of micropore copper foil, and the micropore copper foil after electrochemical corrosion, tensile property is compared with primary battery copper
Foil is close instead or increase there is no reducing.
Compared with primary battery copper foil, the tensile strength of micropore copper foil is close with the tensile strength of native copper foil；Micropore copper foil
Resistivity is increased only can make the capacity of lithium ion battery improve 8-10% less than 3%.Since micropore copper foil makes copper foil two sides
Negative material is connected as an entirety, and the uniformity of the performances such as capacity and the charge-discharge characteristics of battery can be made obviously to be improved,
Battery production yield rate improves 15-20%.
In above-mentioned second step, chemical mordant can also be following several formulas：
The third：The C of the HCl of 0.5mol/L, 1.5mol/L2H2O4, the NH of 0.3mol/L4The FeCl of Cl, 0.6mol/L3,
The AgCl of 0.3mol/L2。
4th kind：The C of the HCl of 1.5mol/L, 0.5mol/L2H2O4, the NH of 0.5mol/L4The FeCl of Cl, 0.5mol/L3,
The AgCl of 0.4mol/L2。
5th kind：The C of the HCl of 1mol/L, 1.5mol/L2H2O4, the NH of 0.1mol/L4The FeCl of Cl, 0.1mol/L3,
The AgCl of 0.4mol/L2。
6th kind：The C of the HCl of 1mol/L, 1.5mol/L2H2O4, the NH of 0.2mol/L4The FeCl of Cl, 0.5mol/L3,
0.1mol/L AgCl2。
7th kind：The C of the HCl of 1.5mol/L, 0.5mol/L2H2O4, the NH of 0.5mol/L4The FeCl of Cl, 0.5mol/L3,
The AgCl of 0.5mol/L2。
8th kind：The C of the HCl of 1mol/L, 1.5mol/L2H2O4, the NH of 0.1mol/L4The FeCl of Cl, 0.1mol/L3,
The AgCl of 0.2mol/L2。
The caustic solution and embodiment of above eight kinds of corrosive agent are same or like.
Table 1 is being compared as follows for micropore copper foil and native copper foil resistivity：
The above content is combine specific preferred embodiment to the further description of the invention done, and it cannot be said that this hair
Bright specific implementation mode is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, is not departing from this
Under the premise of invention, several simple deduction or replace can also be made, all shall be regarded as belonging to the power of the invention by being submitted
Sharp claim determines scope of patent protection.
Claims (8)
1. a kind of electrochemical corrosion preparation method of micropore battery copper foil, it is characterised in that carry out as steps described below：
The first step carries out surface clean to the battery copper foil after rolling and dispels surface attachments；
Battery copper foil after cleaning is totally immersed into chemical corrosion liquid by second step：The corrosive agent includes following molar concentration
Solution：The C of the HCl of 0.5-1.5mol/L, 0.5-2mol/L2H2O4, the NH of 0.1-0.5mol/L4Cl, 0.1-1mol/L's
FeCl3, 0.1-0.5mol/L AgCl2Using etching tank as cathode, battery copper foil is carried out as anode, additional 6-64V direct currents
Corrosion, residence time of the battery copper foil in the corrosive liquid is in 20 ~ 120s；
Third walks, and remained on surface liquid is cleaned to the battery copper foil after corrosion；
4th step, drying.
2. a kind of electrochemical corrosion preparation method of micropore battery copper foil according to claim 1, it is characterised in that in institute
It states and is provided between third step and the 4th step：Brightening processing step.
3. a kind of electrochemical corrosion preparation method of micropore battery copper foil according to claim 2, it is characterised in that brightening
The brightening liquid of processing includes：The CrO of 2-5g/L3, 1-7g/L Na2Cr2O7•2H2O, the NaF of 0.1-1.5g/L.
4. a kind of electrochemical corrosion preparation method of micropore battery copper foil according to claim 1, it is characterised in that first
Cleaning solution in step includes the Na of NaOH, 10-70g/L of 5-30g/L2CO3, 10-40g/L Na3PO4, when in cleaning solution
Between >=6s.
5. a kind of electrochemical corrosion preparation method of micropore battery copper foil according to claim 1, it is characterised in that third
Cleaning solution in step includes：The formula of cleaning solution：The Na of 0.4 ~ 0.8kg2SO4, 0.5 ~ 1kg CaSO4, 0.1 ~ 0.3kg lemon
Acid, which is dissolved in 1L water, to be configured.
6. a kind of electrochemical corrosion preparation method of micropore battery copper foil according to claim 2, it is characterised in that brightening
It is cleaned after processing, the formula of cleaning solution：The Na of 0.4 ~ 0.8kg2SO4, 0.5 ~ 1kg CaSO4, 0.1 ~ 0.3kg citric acid
It is dissolved in 1L water and configuring.
7. a kind of electrochemical corrosion preparation method of micropore battery copper foil according to claim 1, it is characterised in that：Second
In step, battery copper foil upper and lower surface is immersed in corrosive liquid simultaneously, the following table that makes corrosive liquid with the type of flow that recycles on copper foil
Surface current is dynamic, keeps upper and lower surface corrosion uniform to reach.
8. using a kind of micropore copper prepared by the electrochemical corrosion preparation method of micropore battery copper foil as described in claim 1
Foil.
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| CN201810723105.8A CN108611676A (en) | 2018-07-04 | 2018-07-04 | A kind of the electrochemical corrosion preparation method and its micropore copper foil of micropore battery copper foil |
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| CN201810723105.8A CN108611676A (en) | 2018-07-04 | 2018-07-04 | A kind of the electrochemical corrosion preparation method and its micropore copper foil of micropore battery copper foil |
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| CN103481583A (en) * | 2013-10-09 | 2014-01-01 | 北京科技大学 | Treated copper foil with porous structure on surface and preparation method thereof |
| CN104694939A (en) * | 2015-04-07 | 2015-06-10 | 河南红日铜箔科技有限公司 | Surface treatment technology for ultralow-surface-roughness copper foil |
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| CN107740099A (en) * | 2017-10-09 | 2018-02-27 | 山西沃特海默新材料科技股份有限公司 | A kind of chlorine salt corrosion agent for being used to prepare micropore aluminium foil |
| CN107740177A (en) * | 2017-10-09 | 2018-02-27 | 山西沃特海默新材料科技股份有限公司 | A kind of electrochemical heat corrosion preparation method of micropore battery aluminium foil |
| CN107768683A (en) * | 2017-10-09 | 2018-03-06 | 山西沃特海默新材料科技股份有限公司 | A kind of high-performance lithium battery plus plate current-collecting body and its preparation method and application |
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2018
- 2018-07-04 CN CN201810723105.8A patent/CN108611676A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6199700A (en) * | 1984-10-22 | 1986-05-17 | Hitachi Ltd | Structure of copper wiring board |
| CN103481583A (en) * | 2013-10-09 | 2014-01-01 | 北京科技大学 | Treated copper foil with porous structure on surface and preparation method thereof |
| CN104694939A (en) * | 2015-04-07 | 2015-06-10 | 河南红日铜箔科技有限公司 | Surface treatment technology for ultralow-surface-roughness copper foil |
| CN107740100A (en) * | 2017-10-09 | 2018-02-27 | 山西沃特海默新材料科技股份有限公司 | A kind of chemical mordant for being used to prepare micropore aluminium foil |
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