CN109161881A - The anti-oxidation liquid of a kind of Chrome-free of electrolytic copper foil and without washing anti-oxidation technique - Google Patents
The anti-oxidation liquid of a kind of Chrome-free of electrolytic copper foil and without washing anti-oxidation technique Download PDFInfo
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- CN109161881A CN109161881A CN201811101186.4A CN201811101186A CN109161881A CN 109161881 A CN109161881 A CN 109161881A CN 201811101186 A CN201811101186 A CN 201811101186A CN 109161881 A CN109161881 A CN 109161881A
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- oxidation
- chrome
- free
- copper foil
- oxidation liquid
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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
- C23C22/40—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 molybdates, tungstates or vanadates
- C23C22/42—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 molybdates, tungstates or vanadates containing also phosphates
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
Abstract
The present invention provides a kind of anti-oxidation liquid of the Chrome-free of electrolytic copper foil, include following components: sodium tungstate 5-9g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 1-3g/L, disodium ethylene diamine tetraacetate 4-7g/L and phosphatase 11-3ml/L.The anti-oxidation liquid of the Chrome-free without containing the chromium to human carcinogen and reduces the zinc simple substance of battery performance, and does not need to wash, contaminated wastewater environment will not be generated in the process, not only environmental protection but also has saved cost.The present invention also provides use the anti-oxidation liquid of the Chrome-free without washing anti-oxidation technique, the technique is formed by passivating film and is consistent, guarantee that electrolytic copper foil has good wellability and electric conductivity, and it is easy to operate, control is convenient, reduce the process of one of washing, energy saving, and the waste water of pollution environment will not be generated.
Description
Technical field
The present invention relates to the technical fields of electrolytic copper foil manufacture, more particularly, to a kind of anti-oxidation liquid of Chrome-free of electrolytic copper foil
I.e. without the anti-oxidation technique of washing.
Background technique
Traditional electrodeposited copper foil forming manufacturing process specifically includes that generation copper foil-copper foil removing-drying-is anti-oxidation
Drying-winding before processing-washing-water of compaction-winding.In anti-oxidation treatment process, existing antioxidant is generally
Acidic chromate, after metal is contacted with chromating agent, surface be partly dissolved and in the form of metal-chromated oxide again
Precipitating.
Easily there are the problem of appearance such as wrinkle, water spot, color difference when producing ultrathin electrolytic copper foil in this production process distance.
Moreover, using oxidation proof passivation liquid containing chromium, there is also following shortcoming and defect:
(1) chromium of human carcinogen can be damaged to operator's body by containing;(2) after use, some copper foil products
High temperature oven is needed to dry, and high temperature causes the winding room temperature of sealing especially high, is not suitable for personnel's operation;(3) it needs anti-
Anode plate is added in copper foil smooth surface and hair side in oxidation trough, and leads to certain electric current just and can guarantee anti-oxidation requirement;(4) some oxygen
Change in passivating solution and contain zinc, forms metallic zinc in copper foil surface after electro-deposition, zinc simple substance can form original under battery Inner electrolysis matter
Battery, reduces the capacity and charge-discharge performance of battery, or even sets off an explosion.
In addition, also need after carrying out anti-oxidation processing using the oxidation proof passivation liquid containing chromium by washing, and the dress of washing
It sets including 1 pump and 4 jet pipes, needs to expend a large amount of electric energy and industrial water, subsequent also to generate waste water, this is not only polluted
Environment, and will increase cost of water treatment.
For save the cost and protection environment, it is necessary to existing anti-oxidation passivator and washing process are optimized and
It improves.
Summary of the invention
In order to solve the above problems existing in the present technology, it the present invention provides a kind of anti-oxidation liquid of Chrome-free, is free of
There is the chromium to human carcinogen and reduce the zinc simple substance of battery performance, and do not need to wash, will not be generated in the process
Contaminated wastewater environment, not only environmental protection but also saved cost.The present invention also provides use the anti-oxidation liquid of the Chrome-free without washing oxygen
Chemical industry skill, the technique are formed by passivating film and are consistent, and guarantee that electrolytic copper foil has good wellability and electric conductivity, and
Easy to operate, control is convenient, reduces the process of one of washing, energy saving, and will not generate the waste water of pollution environment.
To achieve the goals above, the present invention provides the following technical scheme that
A kind of anti-oxidation liquid of the Chrome-free of electrolytic copper foil includes following components: sodium tungstate 5-9g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 1-3g/
L, disodium ethylene diamine tetraacetate 4-7g/L and phosphatase 11-3ml/L.
In the anti-oxidation liquid of the Chrome-free, the addition of sodium tungstate can improve the surface roughness of copper foil, make it anti-oxidation
In treatment process, uniform passivating film is formed.
1-hydroxy ethylidene-1,1-diphosphonic acid, referred to as HEDP are a kind of organic phosphorus acids anti-incrustation corrosion inhibitors, can be more with iron, copper, zinc etc.
Metal ion species form stable complex compound, can dissolve the oxide of metal surface.Studies have shown that HEDP is remained at 250 DEG C
Play the role of good corrosion-mitigation scale-inhibition, still very stable at a high ph, not facile hydrolysis is not easily decomposed under general light and heat condition.It is resistance to
Acid-base property, the more other organic phosphoric acids of chlorine-resistant oxidation susceptibility (salt) are good.HEDP can be formed with underwater gold category ion, especially calcium ion
Six annulus chelates, thus HEDP has preferable scale inhibition effect and has apparent threshold effect, when compound with other water treatment agents
In use, showing ideal synergistic effect.
Disodium ethylene diamine tetraacetate, referred to as EDTA-2Na are a kind of good compounding agents in chemistry, and there are six coordinations for it
Atom almost can form stable chelate with all metal ions.
The main function of phosphoric acid is the pH value adjusted in anti-oxidation liquid, plays anti-oxidation liquid under the condition of suitable pH anti-
Oxidative deactivation effect.
The present invention is by the selection to said components, and preferably its proportion, by sodium tungstate, 1-hydroxy ethylidene-1,1-diphosphonic acid, second two
Amine tetraacethyl disodium and phosphoric acid are formulated in same solution system, and are acted synergistically, and can be formed uniformly in electrolytic copper foil surface
Polymerization be complexed film, the passivation film in many solvents stablize and it is insoluble, have good anticorrosive protective effect.
It include following components: sodium tungstate 6g/L, 1-hydroxy ethylene-1,1-diphosphonic as further describing for technical solution of the present invention
Sour 2g/L, disodium ethylene diamine tetraacetate 5g/L and phosphoric acid 2ml/L.
As further describing for technical solution of the present invention, the pH of the anti-oxidation liquid of Chrome-free is 2-4, invention human hair
Existing, the pH of anti-oxidation liquid is controlled in 2-4, and the passivating film that copper foil surface is formed is uniform, and no color differnece.
The present invention also provides the use anti-oxidation liquid of above-mentioned Chrome-free without the anti-oxidation technique of washing, comprising the following steps:
(1) copper ion in electrolyte deposits to roller surface and forms copper foil;
Foil equipment includes the dress such as cathode roll, anode slot, transmission and control system, commutation system, conducting system and liquid feeding pipeline
It sets.Specific foil process is the cathode roller that a revolution is installed in electrolytic cell and the anode of insoluble material support, roller
In the electrolytic solution, after energization, the copper ion in solution deposits to roller surface and forms copper foil the leaching of cylinder bottom.
(2) copper foil is removed, and is dried before removing using hot-air drying unit, and effectively takes out acid gas.
Hot-air drying unit includes air-heater, hot air duct, discharge pipe and the gear acid mist shield equipped with exhausting interface, and energy is really
Copper foil not water content before removing is protected, acid gas is effectively detached.
(3) anti-oxidation processing: anti-oxidation Passivation Treatment is carried out using the above-mentioned anti-oxidation liquid of Chrome-free, the Chrome-free is anti-oxidation
Liquid, include following components: sodium tungstate 5-9g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 1-3g/L, disodium ethylene diamine tetraacetate 4-7g/L and
Phosphatase 11-3ml/L.
(4) anti-oxidation liquid is squeezed, liquid method is squeezed using self weight adding pressure type.
(5) it dries, wind and cuts, pass through packaging, factory after quality inspection qualification.
The devices such as the drying equipment before winding includes, baking oven, Far-infrared radiation heating pipe and tube-axial fan, above and below baking oven
Equipped with steam collection conduit, there is gold-plated reflective layer at the back side of Far-infrared radiation heating pipe to enhance the energy of far infrared radiation, uses
The drying before copper foil is wound.Winding uses small-sized inflatable roller, and rim charge is facilitated to dismantle.
As further describing for process technology scheme of the invention, the anti-oxidation Passivation Treatment time is 6s, temperature
It is 24-26 DEG C.
Using the technique that above-mentioned Chrome-free is anti-oxidation, the electrolytic copper foil anti-oxidation and passivation film for manufacturing out is uniform, and
And without washing i.e. can reach good oxidation-protective effect, prevented the generation of wastewater with chromium, reduce cost for wastewater treatment and
Discharge, realizes clean manufacturing, reduces the pollution to environment.
Based on above-mentioned technical solution, technical effect that the present invention obtains are as follows:
(1) the anti-oxidation liquid of the Chrome-free of electrolytic copper foil provided by the invention without containing the chromium to human carcinogen and reduces battery
The zinc simple substance of performance can form uniform polymerization complexing film in electrolytic copper foil surface, and the passivation film is steady in many solvents
It is fixed and insoluble, there is good anticorrosive protective effect.
(2) the anti-oxidation liquid of Chrome-free of the invention is used, anti-oxidation passivation is carried out to electrolytic copper foil, improves the appearance matter of copper foil
Amount, avoids the problem of appearance such as water spot, color difference, due to passivating film uniformity, maintains the higher wellability of electrolytic copper foil and leads
Electrically.
(3) the anti-oxidation technique of the anti-oxidation liquid of Chrome-free provided by the invention uses the above-mentioned Chrome-free by preferred ingredient
Anti-oxidation liquid reduces the procedure in electrolytic copper foil production process, has not only saved production cost without washing, but also
Chromate waste water is not generated, environmental protection is free from environmental pollution.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with specific embodiments to invention is more fully described.This
Invent the better embodiment given.But the invention can be realized in many different forms, however it is not limited to this paper institute
The embodiment of description.On the contrary, the purpose of providing these embodiments is that making to understand more the disclosure
It is thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
Embodiment 1
A kind of anti-oxidation liquid of the Chrome-free of electrolytic copper foil includes following components: sodium tungstate 6g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 2g/L, second
Edetate disodium 5g/L and phosphoric acid 2ml/L;Wherein, the pH of the anti-oxidation liquid of Chrome-free is 3.
The above-mentioned anti-oxidation liquid of Chrome-free without washing anti-oxidation technique, comprising the following steps:
(1) copper ion in electrolyte deposits to roller surface and forms copper foil;
(2) copper foil is removed, and is dried before removing using hot-air drying unit, and effectively takes out acid gas;
(3) anti-oxidation processing: anti-oxidation Passivation Treatment is carried out using the anti-oxidation liquid of above-mentioned Chrome-free, the processing time is 6s, temperature control
It is made as 25 DEG C;
(4) anti-oxidation liquid is squeezed;
(5) it dries, wind and cuts, pass through packaging, factory after quality inspection qualification.
Embodiment 2
A kind of anti-oxidation liquid of the Chrome-free of electrolytic copper foil includes following components: sodium tungstate 5g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 1g/L, second
Edetate disodium 4g/L and phosphatase 11 ml/L;Wherein, the pH of the anti-oxidation liquid of Chrome-free is 4.
The above-mentioned anti-oxidation liquid of Chrome-free without washing anti-oxidation technique, comprising the following steps:
(1) copper ion in electrolyte deposits to roller surface and forms copper foil;
(2) copper foil is removed, and is dried before removing using hot-air drying unit, and effectively takes out acid gas;
(3) anti-oxidation processing: anti-oxidation Passivation Treatment is carried out using the anti-oxidation liquid of above-mentioned Chrome-free, the processing time is 6s, temperature control
It is made as 24 DEG C;
(4) anti-oxidation liquid is squeezed;
(5) it dries, wind and cuts, pass through packaging, factory after quality inspection qualification.
Embodiment 3
A kind of anti-oxidation liquid of the Chrome-free of electrolytic copper foil includes following components: sodium tungstate 9g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 3g/L, second
Edetate disodium 7g/L and phosphoric acid 3ml/L;Wherein, the pH of the anti-oxidation liquid of Chrome-free is 2.
The above-mentioned anti-oxidation liquid of Chrome-free without washing anti-oxidation technique, comprising the following steps:
(1) copper ion in electrolyte deposits to roller surface and forms copper foil;
(2) copper foil is removed, and is dried before removing using hot-air drying unit, and effectively takes out acid gas;
(3) anti-oxidation processing: anti-oxidation Passivation Treatment is carried out using the anti-oxidation liquid of above-mentioned Chrome-free, the processing time is 6s, temperature control
It is made as 26 DEG C;
(4) anti-oxidation liquid is squeezed;
(5) it dries, wind and cuts, pass through packaging, factory after quality inspection qualification.
Embodiment 4
A kind of anti-oxidation liquid of the Chrome-free of electrolytic copper foil includes following components: sodium tungstate 7g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 2g/L, second
Edetate disodium 5g/L and phosphoric acid 2ml/L;Wherein, the pH of the anti-oxidation liquid of Chrome-free is 3.
The above-mentioned anti-oxidation liquid of Chrome-free without washing anti-oxidation technique, comprising the following steps:
(1) copper ion in electrolyte deposits to roller surface and forms copper foil;
(2) copper foil is removed, and is dried before removing using hot-air drying unit, and effectively takes out acid gas;
(3) anti-oxidation processing: anti-oxidation Passivation Treatment is carried out using the anti-oxidation liquid of above-mentioned Chrome-free, the processing time is 6s, temperature control
It is made as 25 DEG C;
(4) anti-oxidation liquid is squeezed;
(5) it dries, wind and cuts, pass through packaging, factory after quality inspection qualification.
Comparative example
Electrolytic copper foil enters the oxidation proof passivation liquid for containing only disodium ethylene diamine tetraacetate 5g/L through deflector roll after copper foil removing
In, wherein temperature control is 25 DEG C, and the processing time is 6s, is wound after high temperature is dried.
The product of embodiment 1- embodiment 4 and comparative example is subjected to anti-oxidation test, test result is as follows:
The copper foil product of 1 embodiment 1- embodiment 4 of table and comparative example carries out anti-oxidation test result
The oxidation proof passivation liquid that disodium ethylene diamine tetraacetate is only used it can be seen from the test result of table 1, almost to copper
Foil unprotect effect, and the copper foil of the anti-oxidation liquid of above-mentioned Chrome-free is used, oxidation-protective effect is good, and reason is mainly embodiment 1- real
Sodium tungstate, 1-hydroxy ethylidene-1,1-diphosphonic acid, disodium ethylene diamine tetraacetate and phosphoric acid are formulated in same solution body by the anti-oxidation liquid for applying example 4
It in system, and acts synergistically, uniform polymerization complexing film can be formed in electrolytic copper foil surface, the passivation film is in many solvents
Middle stabilization and insoluble, has good anticorrosive protective effect.
The above content is only structure example and explanation of the invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these obviously replace shape
Formula all belongs to the scope of protection of the present invention.
Claims (5)
1. a kind of anti-oxidation liquid of the Chrome-free of electrolytic copper foil, which is characterized in that include following components: sodium tungstate 5-9g/L, hydroxyl second
Pitch di 2 ethylhexyl phosphonic acid 1-3g/L, disodium ethylene diamine tetraacetate 4-7g/L and phosphatase 11-3ml/L.
2. the anti-oxidation liquid of the Chrome-free of electrolytic copper foil according to claim 1, which is characterized in that include following components: wolframic acid
Sodium 6g/L, 1-hydroxy ethylidene-1,1-diphosphonic acid 2g/L, disodium ethylene diamine tetraacetate 5g/L and phosphoric acid 2ml/L.
3. the anti-oxidation liquid of the Chrome-free of electrolytic copper foil according to claim 1, which is characterized in that the anti-oxidation liquid of Chrome-free
PH is 2-4.
4. it is a kind of using Chrome-free described in claim 1 anti-oxidation liquid without washing anti-oxidation technique, which is characterized in that including following
Step:
(1) copper ion in electrolyte deposits to roller surface and forms copper foil;
(2) copper foil is removed, and is dried before removing using hot-air drying unit, and effectively takes out acid gas;
(3) anti-oxidation Passivation Treatment anti-oxidation processing: is carried out using the anti-oxidation liquid of Chrome-free described in claim 1;
(4) anti-oxidation liquid is squeezed;
(5) it dries, wind and cuts, pass through packaging, factory after quality inspection qualification.
5. according to claim 4 without washing anti-oxidation technique, which is characterized in that the anti-oxidation Passivation Treatment time is
6s, temperature are 24-26 DEG C.
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CN201811101186.4A CN109161881B (en) | 2018-09-20 | 2018-09-20 | Chromium-free anti-oxidation liquid and washing-free anti-oxidation process for electrolytic copper foil |
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CN201811101186.4A CN109161881B (en) | 2018-09-20 | 2018-09-20 | Chromium-free anti-oxidation liquid and washing-free anti-oxidation process for electrolytic copper foil |
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Cited By (6)
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CN110344043A (en) * | 2019-07-05 | 2019-10-18 | 国工恒昌新材料沧州有限公司 | A kind of processing of lead frame copper strip plate curing means and maintenance process |
CN111472005A (en) * | 2020-04-27 | 2020-07-31 | 青海电子材料产业发展有限公司 | Acidic environment-friendly anti-oxidation process for electrolytic copper foil |
CN112095108A (en) * | 2020-08-11 | 2020-12-18 | 湖北工程学院 | Electrolytic copper foil antioxidant and anti-oxidation process using same |
CN113463078A (en) * | 2021-08-04 | 2021-10-01 | 武汉轻工大学 | Preparation method and application of anti-oxidation liquid containing polyhydroxy organic matter |
CN113564572A (en) * | 2021-08-04 | 2021-10-29 | 武汉轻工大学 | Preparation and application of novel electrolytic copper foil anti-oxidation liquid |
CN116333593A (en) * | 2023-03-22 | 2023-06-27 | 江苏铭丰电子材料科技有限公司 | Environment-friendly anti-oxidation liquid for electrolytic copper foil and anti-oxidation process thereof |
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CN107634228A (en) * | 2017-09-14 | 2018-01-26 | 江苏铭丰电子材料科技有限公司 | A kind of lithium ion battery electrolytic copper foil Chrome-free anti-oxidation technology |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN110344043A (en) * | 2019-07-05 | 2019-10-18 | 国工恒昌新材料沧州有限公司 | A kind of processing of lead frame copper strip plate curing means and maintenance process |
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CN111472005B (en) * | 2020-04-27 | 2022-05-24 | 青海电子材料产业发展有限公司 | Acidic environment-friendly anti-oxidation process for electrolytic copper foil |
CN112095108A (en) * | 2020-08-11 | 2020-12-18 | 湖北工程学院 | Electrolytic copper foil antioxidant and anti-oxidation process using same |
CN113463078A (en) * | 2021-08-04 | 2021-10-01 | 武汉轻工大学 | Preparation method and application of anti-oxidation liquid containing polyhydroxy organic matter |
CN113564572A (en) * | 2021-08-04 | 2021-10-29 | 武汉轻工大学 | Preparation and application of novel electrolytic copper foil anti-oxidation liquid |
CN113463078B (en) * | 2021-08-04 | 2023-10-27 | 武汉轻工大学 | Preparation method and application of antioxidant liquid containing polyhydroxy organic matters |
CN116333593A (en) * | 2023-03-22 | 2023-06-27 | 江苏铭丰电子材料科技有限公司 | Environment-friendly anti-oxidation liquid for electrolytic copper foil and anti-oxidation process thereof |
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