CN100467673C - Removing process of residual copper on cathode foil surface for improved aluminium electrolyzing capacitor - Google Patents

Removing process of residual copper on cathode foil surface for improved aluminium electrolyzing capacitor Download PDF

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Publication number
CN100467673C
CN100467673C CNB2006100391725A CN200610039172A CN100467673C CN 100467673 C CN100467673 C CN 100467673C CN B2006100391725 A CNB2006100391725 A CN B2006100391725A CN 200610039172 A CN200610039172 A CN 200610039172A CN 100467673 C CN100467673 C CN 100467673C
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China
Prior art keywords
cathode foil
copper
scavenging solution
cleaning solution
nitric acid
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Expired - Fee Related
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CNB2006100391725A
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Chinese (zh)
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CN1861846A (en
Inventor
余建强
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K.TECH PRECISION TECHNOLOGY (JIANGSU) CO., LTD.
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JUNDA TRAFFIC ENVIRONMENT PROTECTION CO Ltd WUXI CITY
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Priority to CNB2006100391725A priority Critical patent/CN100467673C/en
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Abstract

This improvement method relates to removing of the residual copper on the surface of the cathode foil, it is used in the aluminum electrolytic capacitor. The cleaning solution is hydrogen nitrate, and there is buffer in the cleaning solution, the buffer is soluble salt which contains element of CrO4 2- or PO43- or peptide amine or six-methyl fouramine. The weight of the buffer is 0.1-8% of the cleaning solution, the concentration of hydrogen nitrate uses in cleaning solution is 50-75 wt %, the temperature of it is 25-40DEG C, the time of immersion is 30-45s. This method can remove the residual copper on the surface of cathode foil, which belongs to the hard or soft electrical aluminum foil and is experienced the corrosion treatment. It can reduce the content of the copper on the cathode foil below 3mg/m2. This method is simple and easy to produce continuously, it can not affect the specific volume and mechanical intensity of the cathode foil, and it increases the lifetime of the aluminum electrolytic capacitor. At last, it doesn't contain the extraction of copper in this method, so the cost can be controlled.

Description

The removal method of improved remaining copper on surface of cathode foil for aluminum electrolytic capacitors
Technical field
The present invention relates to a kind of method of removing remaining copper on surface of cathode foil for aluminum electrolytic capacitors.
Background technology
Chinese patent CN03150482.5 discloses a kind of " the aluminium electrolutic capacitor removal method of negative pole aluminium etched foil remaining copper on surface ", it adopts high density nitric acid to add copper ion complexing agent as scavenging solution in rinse bath, adopt electrochemical electrolysis to extract the device of copper, clean chlorion and remaining copper simultaneously, concentration of nitric acid is 20-60wt%, the nitric acid liquid temperature is 15-60 ℃, the time of embathing is 5-90s, also added the copper ion complexing agent of 100-600ppm in the solution, though this method can be reduced to 5mg/m to etched foil remaining copper on surface content effectively 2Below, but the deficiency that exists is also clearly, promptly is used as scavenging solution nitric acid and has severe corrosive, and the anticathode paper tinsel also constitutes damage in the process of removing cupric ion, has reduced the specific volume of Cathode Foil, and its electrical property and work-ing life are had a strong impact on; In addition, adopt copper ion complexing agent in order to extract copper in this method, because the copper of Cathode Foil remained on surface still is fewer, the copper content of hard attitude electric aluminum foil is 0.18-0.25%, the copper content of soft attitude electric aluminum foil is 0.06-0.12%, thickness is 15 μ m-60 μ m, the device that extracts copper in the method in fact not have many realistic meaning, increased facility investment running cost on the contrary; Moreover, though the technical parameter of controlling in this technology can reach the effect of removing cupric ion, but can not adapt to the continuous operation of big production, operation is after 12 to 16 hours approximately continuously, the remaining copper on surface of cathode foil ion content needs the new liquid of scavenging solution restock of removal 1/3rd could continue technology just more than or equal to 10mg/M2.
Summary of the invention
The present invention is just in order to overcome above-mentioned deficiency, the not removal method of the improved remaining copper on surface of cathode foil for aluminum electrolytic capacitors of loss of a kind of specific volume is provided, compare with background technology, improved the electrical property of Cathode Foil, reduced the impedance of electrolytic condenser, improved the life-span of aluminium electrolutic capacitor, the main improvement is to add inhibiter in the nitric acid scavenging solution, utilize the effect of inhibiter to prevent the corrosion-damaged of nitric acid anticathode sheet capacitance, specifically implement like this: the removal method of improved remaining copper on surface of cathode foil for aluminum electrolytic capacitors, with salpeter solution as scavenging solution, it is characterized in that being added with in the scavenging solution inhibiter, described inhibiter is to contain CrO 4 2-Soluble salt or contain PO 4 3-Soluble salt or polymorphic amine or hexamethylenetetramine, the add-on of inhibiter accounts for 0.1-8% in scavenging solution weight, the concentration of cleaning with nitric acid is 50-75wt%, the nitric acid temperature is 25-40 ℃, dipping time is 30-45s.
Aluminium is that copper can be replaced in the active metal, copper is deposited on the Cathode Foil surface, simultaneously because the dissolving of aluminium, the specific volume of Cathode Foil is descended, the present invention adds inhibiter in nitric acid, purpose is to hinder the replacement(metathesis)reaction of aluminium and copper, hinders the dissolving of aluminium, thereby reach the remaining copper of removing the Cathode Foil surface, guarantee that again the specific volume of Cathode Foil is unaffected.
Inhibiter as in the scavenging solution contains CrO 4 2-The add-on of soluble salt to account for 3-5wt% in scavenging solution be good, contain PO 4 3-The add-on of soluble salt to account for 5-8wt% in scavenging solution be good, polymorphic amine NH 2(CH 2CH 2NH) nCH 2CH 2NH 2Add-on to account for 0.5-1wt% in scavenging solution be good, the add-on of hexamethylenetetramine accounts for 0.1-5wt% in scavenging solution, be good with 0.1-0.3wt% especially.
Concentration of nitric acid as scavenging solution among the present invention is good with 65-72wt% then, as long as guarantee the concentration of nitric acid, this cleaning can realize continuous production, need not at centre pause more renewing liquid.
Present method can be removed hard attitude, the soft attitude electric aluminum foil remaining copper on surface of cathode foil through corrosion treatment, can be reduced to remaining copper on surface of cathode foil content below the 3mg/m2, method is easy and can realize serialization production, can not influence the specific volume and the physical strength of Cathode Foil, improved the life-span of aluminium electrolutic capacitor, and not setting the extraction of copper in the technology, cost also is under control.
Embodiment
Embodiment 1, the removal method of improved remaining copper on surface of cathode foil for aluminum electrolytic capacitors, and the salpeter solution that with concentration is 50-75wt% also adds (the NH that accounts for scavenging solution 3-5wt% as scavenging solution in the scavenging solution 4) 2CrO 4The salt inhibiter, the nitric acid temperature is 25-40 ℃ during cleaning, dipping time is 30-45s.
Embodiment 2, the removal method of improved remaining copper on surface of cathode foil for aluminum electrolytic capacitors, and the salpeter solution that with concentration is 65-72wt% also adds the NH that contains that accounts for scavenging solution 5-8wt% as scavenging solution in the scavenging solution 4H 2PO 4The salt inhibiter, the nitric acid temperature is 25-40 ℃ during cleaning, dipping time is 30-45s.
Embodiment 3, reference example 2, and the inhibiter that adds in the scavenging solution is polymorphic amine NH 2(CH 2CH 2NH) nCH 2CH 2NH 2, it accounts for 0.5-1wt% in scavenging solution.
Embodiment 4, reference example 2, and the inhibiter that adds in the scavenging solution is a hexamethylenetetramine, it accounts for 0.1-5wt% in scavenging solution.
Embodiment 5, reference example 2, and the inhibiter that adds in the scavenging solution is a hexamethylenetetramine, it accounts for 0.1-0.3wt% in scavenging solution.
The test data of the foregoing description is:
Copper content mg/M 2 Specific volume μ F/cm 2
Embodiment 1 2.79-2.98 310-370
Embodiment 2 2.80-2.89 320-368
Embodiment 3 1.95-2.40 331-388
Embodiment 4 1.90-2.01 398-427
Embodiment 5 1.66-1.72 415-449

Claims (3)

1. the removal method of improved remaining copper on surface of cathode foil for aluminum electrolytic capacitors, as scavenging solution, the concentration of cleaning with nitric acid is 50-75wt% with salpeter solution, the nitric acid temperature is 25-40 ℃, dipping time is 30-45s, is added with inhibiter in the scavenging solution, it is characterized in that inhibiter is to contain CrO 4 2-Soluble salt or contain PO 4 3-Soluble salt or polymorphic amine or hexamethylenetetramine, wherein, contain CrO 4 2-Soluble salt in scavenging solution, account for 3-5wt%, contain PO 4 3-Soluble salt in scavenging solution, account for 5-8wt%, polymorphic amine NH 2(CH 2CH 2NH) nCH 2CH 2NH 2Account for 0.5-1wt% in scavenging solution, hexamethylenetetramine accounts for 0.1-5wt% in scavenging solution.
2. removal method according to claim 1 is characterized in that hexamethylenetetramine accounts for 0.1-0.3wt% in scavenging solution.
3. removal method according to claim 1 is characterized in that concentration of nitric acid is 65-72wt%.
CNB2006100391725A 2006-03-27 2006-03-27 Removing process of residual copper on cathode foil surface for improved aluminium electrolyzing capacitor Expired - Fee Related CN100467673C (en)

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CN100467673C true CN100467673C (en) 2009-03-11

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649454B (en) * 2009-06-23 2010-12-08 吴江飞乐天和电子材料有限公司 Method for removing remaining copper on surface of cathode foil for aluminum electrolytic capacitors
CN101649458B (en) * 2009-06-23 2011-03-16 吴江飞乐天和电子材料有限公司 Method for reducing remaining copper on surface of cathode foil of aluminum electrolytic capacitor
CN103276435B (en) * 2013-05-21 2014-08-06 东莞劲胜精密组件股份有限公司 Micro-nano processing method for aluminum/aluminum alloy surface and aluminum/ aluminum alloy structure
CN108004547A (en) * 2017-11-20 2018-05-08 湖北富奕达电子科技有限公司 A kind of aluminium electrolytic capacitor cathode aluminium foil corrosion new process

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1489161A (en) * 2003-08-21 2004-04-14 上海交通大学 Method for removing residual copper of aluminium corroding foil surface of negative electrode for aluminium electrolytic capacitor

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1489161A (en) * 2003-08-21 2004-04-14 上海交通大学 Method for removing residual copper of aluminium corroding foil surface of negative electrode for aluminium electrolytic capacitor

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低表面附着铜含量的铝阴极箔研究. 任晓辉等.电子元件与材料,第23卷第2期. 2004
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