CN109208050A - A kind of surface treatment method improving electrolytic copper foil corrosion resistance - Google Patents
A kind of surface treatment method improving electrolytic copper foil corrosion resistance Download PDFInfo
- Publication number
- CN109208050A CN109208050A CN201811300168.9A CN201811300168A CN109208050A CN 109208050 A CN109208050 A CN 109208050A CN 201811300168 A CN201811300168 A CN 201811300168A CN 109208050 A CN109208050 A CN 109208050A
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- copper foil
- electrolytic copper
- corrosion resistance
- surface treatment
- treatment method
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
Abstract
The invention discloses a kind of surface treatment methods for improving electrolytic copper foil corrosion resistance, belong to electrolytic copper foil production technical field.The processing method includes foil pretreatment, solidification plating solution, Passivation Treatment, spraying coupling agent.After tested, the 12 μm of copper foil products prepared using present invention process, the performances such as inoxidizability, corrosion resistance, peel strength are reached application requirement, show good prospect and application value.
Description
Technical field
The invention belongs to electrolytic copper foil surface processing technology fields, and in particular to a kind of to improve electrolytic copper foil corrosion resistance
Surface treatment method.
Background technique
Basic material one of of the electrolytic copper foil as electronics industry, in electronics industry using very extensive, to entire
The development of electronics industry has highly important effect.Electrolytic copper foil is that suitable electrolyte solution is made in certain current density
Under, the metal copper deposits obtained by electro-deposition techniques are widely used in copper-clad plate (abbreviation CCL) and printed wiring board
The production of (abbreviation PCB).
The quality of electrolytic copper foil is not only related with foil matrix, also with the process for treating surface of copper foil it is closely bound up
1 ].Electrolytic copper foil can effectively improve the quality and performance of product, to have after the processing of suitable process of surface treatment
There are excellent heat resistance, corrosion resistance and higher peel strength, to meet industrial requirements at the higher level.
To adapt to electronics miniaturization, light-weighted functional requirement, 12 μm of slim copper foils or extra thin copper foil below
Using more and more extensively, there is preferable elongation percentage, flatness and high temperature resistant, anti-oxidant contour performance requirement for guarantee copper foil,
Traditional copper foil surface processing technique is insurmountable.Since copper foil will receive oxidation, corrosion during storage, transport etc.
Deng influence, thus copper foil need to be often surface-treated to prevent copper foil oxidative phenomena from occurring.Currently, traditional copper foil surface
Anti-oxidation processing method is deactivation method, i.e., chemical passivation or the electrolytic passivation under chromate, main mesh in chromic acid solution
Be copper foil surface formed " chromizing layer ", make copper foil and air exclusion, to achieve the effect that antirust antiplaque Anti- tarnishing.But just
The technical level of surface treating additive used at present and treatment process, treated copper foil is in inoxidizability, corrosion resistance
Energy aspect cannot still fully meet needs of production.
Summary of the invention
The main purpose of the present invention is to provide a kind of surface treatment methods for improving electrolytic copper foil corrosion resistance, pass through this method
After processing, the corrosion resistance and inoxidizability of copper foil are significantly improved.
The above goal of the invention is achieved through the following technical solutions, it is a kind of improve electrolytic copper foil corrosion resistance surface at
Reason method the following steps are included:
(1) foil pre-processes: after taking copper foil foil to utilize dehydrated alcohol oil removing, washing according to a conventional method, then with sulfuric acid removing oxidation
Film, then after washing, by roughening, then wash.
(2) solidify plating solution: carrying out solidification plating solution by pretreated copper foil for above-mentioned, solidify liquid includes salt zinc sulfate, sulphur
Sour nickel and additive and complexing agent.
Further, solidify liquid further includes catalyst modification titanium sulfate.
Further, additive includes sodium citrate, tartaric acid, N', dinethylformamide and boric acid, ammonium chloride.
Further, complexing agent is hydroxy ethylene diphosphonic acid sylvite.
Further, the composition of solidify liquid are as follows: 80~110g of zinc sulfate/L, 60~90g of nickel sulfate/L, ortho phosphorous acid
20~50g of sodium/L, 5~10 g of modifying titanium sulfate/L, 3~9 g of peaceful lemon acid sodium/L, 2~5 g of tartaric acid/L, N', N- bis-
Methylformamide 10~15 m L/L, 10~20 g of boric acid/L, 2~6 g of ammonium chloride/L, hydroxy ethylene diphosphonic acid sylvite 2
~10g/L.
The preparation method of the modifying titanium sulfate: the deionized water dissolving of a certain amount of Ti (SO4) 2 is weighed, then will be certain
The La2O3 of amount dissolves in wherein, 100 DEG C of dryings, cold by solids respectively at 400~500 DEG C of temperature calcination 4h in Muffle furnace
But it is saved backup under mill-drying environment after.
Curing process condition: 2~3A/dm of cathode-current density2, temperature is room temperature, and anode is stereotype, wherein when plating
Between 16~20 s.
(3) Passivation Treatment, passivating solution are commercial product, are passivated under the conditions of 8.0~11.0,40~50 DEG C of pH value
Processing, preferably Passivation Treatment 5s；
(4) coupling agent is sprayed, is sprayed and is soaked in electrolytic copper foil surface using KBE-903 silane coupling agent.
Rare earth modified solid acid is made through high-temperature roasting after the titanium doped La2O3 of sulfuric acid, rare earth member is introduced in solid acid
Element, modified solid acid not only have a better surface acidity, and content of rare earth is few, settles fast, easily separated after reaction and returns
Receive, it is reusable repeatedly, the advantages that regenerating easily, and it is colourless, limpid to enormously simplify the aftertreatment technology of reaction, product
It is transparent.Solid acid after rare earth modified is a kind of environment-friendly catalyst.
Further to verify modifying titanium sulfate as solidifying work of the solution additive in terms of improving electrolytic copper foil corrosion resistance
With our company has made following tests:
12 μm of high-purity electrolytic copper foils that experiment is produced using our company are cut copper foil by 5 cm × 10cm size,
Two pieces are cut into, is surface-treated respectively with test group solidify liquid and control group solidify liquid, corrosion resistant is carried out with the hair side to copper foil
Corrosion research.
Test group: the group of solidify liquid becomes zinc sulfate 100g/L, nickel sulfate 80g/L, sodium hypophosphite 35g/L, modified
8 g of titanium sulfate/L, 6 g of peaceful lemon acid sodium/L, tartaric acid 3g/L, N', dinethylformamide 12 m L/L, 15 g of boric acid/
L, 4 g of ammonium chloride/L, hydroxy ethylene diphosphonic acid sylvite 6g/L.
Control group: other ingredients of solidify liquid are completely the same with test group, are intended only as the modification sulfuric acid of one of additive
Titanium changes titanium sulfate into.
In cathode-current density 3A/dm2, temperature is room temperature, and anode is stereotype, wherein 20 s of plating time.
Test result: the copper foil being surface-treated by test group and control group is placed in climatic chamber simultaneously, 100
DEG C, under 80% damp condition, carry out corrosive nature test, the results showed that, it is existing that 48 h of test group copper foil does not show oxidation stain
As；Then significantly there is oxidation stain phenomenon in control group.3343 type universal testing machine of Instron is used simultaneously, to electrolysis
The peel strength of copper foil is detected, and as a result test group is 1.18N/mm, and control group is 1.06 N/mm, test group performance
Preferable peel strength performance out.
Beneficial effects of the present invention: titanium sulfate is modified to the surface that electrolytic copper foil is used for as the additive of solidify liquid
There is not been reported for processing, and rare earth modified solid acid especially is made through high-temperature roasting again with La2O3 modifying titanium sulfate and is used as raising
Copper foil corrosion resistance is not shown in technical report.Compared with prior art, electrolytic copper foil surface processing of the present invention is using modified sulfuric acid
Titanium can enhance the covering power of electrolytic copper foil as additive, profile peak height and peak valley can plate one layer it is uniform fine
Alloying pellet roughened layer makes the very low-profile electrolytic copper foil produced reach crystallite effect, enhances copper foil anti-stripping on base material
From intensity, and make coating compact crystallization, enhances coating corrosion resistance.Meanwhile the technique is without the harmful elements such as Pb, As, tool
There is good environmental protection characteristic.After tested, using present invention process prepare 12 μm of copper foil products, inoxidizability, corrosion resistance,
The performances such as peel strength reach application requirement, show good prospect and application value.
Specific embodiment
Embodiment one: it is a kind of improve electrolytic copper foil corrosion resistance surface treatment method the following steps are included:
(1) foil pre-processes: after taking copper foil foil to utilize dehydrated alcohol oil removing, washing according to a conventional method, then with sulfuric acid removing oxidation
Film, then after washing, by roughening, then wash.
(2) solidify plating solution: carrying out solidification plating solution, the composition of solidify liquid are as follows: zinc sulfate by pretreated copper foil for above-mentioned
100g/L, nickel sulfate 80g/L, sodium hypophosphite 35g/L, 8 g of modifying titanium sulfate/L, 6 g of peaceful lemon acid sodium/L, tartaric acid 3
G/L, N', dinethylformamide 12 m L/L, 15 g of boric acid/L, 4 g of ammonium chloride/L, hydroxy ethylene diphosphonic acid sylvite
6g/L。
Curing process condition: cathode-current density 2A/dm2, temperature is room temperature, and anode is stereotype, wherein plating time
16 s。
(3) Passivation Treatment, passivating solution are commercial product, are passivated place under the conditions of 8.0~11.0,45 DEG C of pH value
Reason, preferably Passivation Treatment 5s；
(4) coupling agent is sprayed, is sprayed and is soaked in electrolytic copper foil surface using KBE-903 silane coupling agent.
The electrolytic copper foil obtained by above-mentioned processing method, is placed in climatic chamber, in temperature 70 C, the item of humidity 80%
Under part, 48 h do not show oxidation stain phenomenon.
Embodiment two: it is a kind of improve electrolytic copper foil corrosion resistance surface treatment method the following steps are included:
(1) foil pre-processes: after taking copper foil foil to utilize dehydrated alcohol oil removing, washing according to a conventional method, then with sulfuric acid removing oxidation
Film, then after washing, by roughening, then wash.
(2) solidify plating solution: carrying out solidification plating solution, the composition of solidify liquid are as follows: zinc sulfate by pretreated copper foil for above-mentioned
80g/L, nickel sulfate 60g/L, sodium hypophosphite 20g/L, 10 g of modifying titanium sulfate/L, 9 g of peaceful lemon acid sodium/L, tartaric acid 2
G/L, N', dinethylformamide 10 m L/L, 20 g of boric acid/L, ammonium chloride 2g/L, hydroxy ethylene diphosphonic acid sylvite
10g/L。
Curing process condition: cathode-current density 3A/dm2, temperature is room temperature, and anode is stereotype, wherein plating time
20 s。
(3) Passivation Treatment, passivating solution are commercial product, are passivated place under the conditions of 8.0~11.0,40 DEG C of pH value
Reason, preferably Passivation Treatment 5s；
(4) coupling agent is sprayed, is sprayed and is soaked in electrolytic copper foil surface using KBE-903 silane coupling agent.
The electrolytic copper foil obtained by above-mentioned processing method, is placed in climatic chamber, in 120 DEG C of temperature, humidity 80%
Under the conditions of, 48 h do not show oxidation stain phenomenon.
Embodiment three: it is a kind of improve electrolytic copper foil corrosion resistance surface treatment method the following steps are included:
(1) foil pre-processes: after taking copper foil foil to utilize dehydrated alcohol oil removing, washing according to a conventional method, then with sulfuric acid removing oxidation
Film, then after washing, by roughening, then wash.
(2) solidify plating solution: carrying out solidification plating solution, the composition of solidify liquid are as follows: zinc sulfate by pretreated copper foil for above-mentioned
110g/L, nickel sulfate 90g/L, sodium hypophosphite 50g/L, modifying titanium sulfate 5g/L, 3 g of peaceful lemon acid sodium/L, tartaric acid 5
G/L, N', dinethylformamide 15 m L/L, 10 g of boric acid/L, ammonium chloride 6g/L, hydroxy ethylene diphosphonic acid sylvite
2g/L。
Curing process condition: cathode-current density 3A/dm2, temperature is room temperature, and anode is stereotype, wherein plating time
20 s。
(3) Passivation Treatment, passivating solution are commercial product, are passivated place under the conditions of 8.0~11.0,40 DEG C of pH value
Reason, preferably Passivation Treatment 5s；
(4) coupling agent is sprayed, is sprayed and is soaked in electrolytic copper foil surface using KBE-903 silane coupling agent.
The electrolytic copper foil obtained by above-mentioned processing method, performance indexes is as follows after tested:
The electrolytic copper foil obtained by above-mentioned processing method, is placed in climatic chamber, in 150 DEG C of temperature, the condition of humidity 80%
Under, 48 h do not show oxidation stain phenomenon.
Claims (6)
1. a kind of surface treatment method for improving electrolytic copper foil corrosion resistance, the processing method is the following steps are included: (1) foil
Pretreatment: after taking copper foil foil to utilize dehydrated alcohol oil removing, washing according to a conventional method, then with sulfuric acid oxide film dissolving, then after washing,
By roughening, then wash；(2) solidify plating solution: carrying out solidification plating solution by pretreated copper foil for above-mentioned, solidify liquid includes salt sulphur
Sour zinc, nickel sulfate and additive and complexing agent；(3) Passivation Treatment, passivating solution are commercial product, in pH value 8.0~11.0,40
Processing, preferably Passivation Treatment 5s are passivated under the conditions of~50 DEG C；(4) coupling agent is sprayed, it is silane coupled using KBE-903
Agent is sprayed in electrolytic copper foil surface and is soaked, it is characterised in that solidify liquid further includes catalyst modification titanium sulfate.
2. a kind of surface treatment method for improving electrolytic copper foil corrosion resistance as described in claim 1, it is characterised in that addition
Agent includes sodium citrate, tartaric acid, N', dinethylformamide and boric acid, ammonium chloride.
3. a kind of surface treatment method for improving electrolytic copper foil corrosion resistance as described in claim 1, it is characterised in that complexing
Agent is hydroxy ethylene diphosphonic acid sylvite.
4. a kind of surface treatment method for improving electrolytic copper foil corrosion resistance as described in claim 1, it is characterised in that solidification
The composition of liquid are as follows: 80~110g of zinc sulfate/L, 60~90g of nickel sulfate/L, 20~50g of sodium hypophosphite/L, modified sulfuric acid
5~10 g of titanium/L, 3~9 g of peaceful lemon acid sodium/L, 2~5 g of tartaric acid/L, N', 10~15 m L/ of dinethylformamide
L, 10~20 g of boric acid/L, 2~6 g of ammonium chloride/L, 2~10g/L of hydroxy ethylene diphosphonic acid sylvite.
5. a kind of surface treatment method for improving electrolytic copper foil corrosion resistance as described in claim 1, it is characterised in that described
The preparation method of modifying titanium sulfate: the deionized water dissolving of a certain amount of Ti (SO4) 2 is weighed, then a certain amount of La2O3 is dissolved in
Wherein, solids is distinguished 400~500 DEG C of temperature calcination 4h, mill-drying environment after cooling by 100 DEG C of dryings in Muffle furnace
Under save backup.
6. a kind of surface treatment method for improving electrolytic copper foil corrosion resistance as described in claim 1, it is characterised in that solidification
Process conditions: 2~3A/dm of cathode-current density2, temperature is room temperature, and anode is stereotype, wherein 16~20s of plating time.
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| CN201811300168.9A CN109208050B (en) | 2018-11-02 | 2018-11-02 | Surface treatment method for improving corrosion resistance of electrolytic copper foil |
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Cited By (4)
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| CN109518237A (en) * | 2019-01-24 | 2019-03-26 | 合鸿新材科技有限公司 | Zinc-nickel phosphorus electroplate liquid, preparation method and electro-plating method |
| CN110079840A (en) * | 2019-04-26 | 2019-08-02 | 山东金宝电子股份有限公司 | A kind of surface treatment additive package improving copper foil high-temp antioxidizing performance |
| CN111005045A (en) * | 2019-12-31 | 2020-04-14 | 西安西工大超晶科技发展有限责任公司 | Preparation method of titanium and titanium alloy surface coating |
| CN113943954A (en) * | 2021-12-01 | 2022-01-18 | 青海诺德新材料有限公司 | Preparation method of 2-3 micron pinhole-free carrier electrolytic copper foil |
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| CN110079840A (en) * | 2019-04-26 | 2019-08-02 | 山东金宝电子股份有限公司 | A kind of surface treatment additive package improving copper foil high-temp antioxidizing performance |
| CN111005045A (en) * | 2019-12-31 | 2020-04-14 | 西安西工大超晶科技发展有限责任公司 | Preparation method of titanium and titanium alloy surface coating |
| CN113943954A (en) * | 2021-12-01 | 2022-01-18 | 青海诺德新材料有限公司 | Preparation method of 2-3 micron pinhole-free carrier electrolytic copper foil |
| CN113943954B (en) * | 2021-12-01 | 2023-06-30 | 青海诺德新材料有限公司 | Preparation method of 2-3 micron pinhole-free carrier electrolytic copper foil |
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Denomination of invention: A surface treatment method for improving the corrosion resistance of electrolytic copper foil Effective date of registration: 20211018 Granted publication date: 20210330 Pledgee: Shandong Shengmu Tourism Development Co.,Ltd. Pledgor: SHANDONG JINSHENGYUAN ELECTRONIC MATERIAL Co.,Ltd. Registration number: Y2021980010790 |
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