CN103774193B - A kind of method of mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus - Google Patents

A kind of method of mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus Download PDF

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CN103774193B
CN103774193B CN201410004941.2A CN201410004941A CN103774193B CN 103774193 B CN103774193 B CN 103774193B CN 201410004941 A CN201410004941 A CN 201410004941A CN 103774193 B CN103774193 B CN 103774193B
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aluminium foil
deposition
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何业东
彭宁
梁力勃
宋洪洲
杨小飞
蔡小宇
熊传勇
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Xinjiang Guangtou Guidong Electronic Technology Co ltd
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Guangxi Hezhou Guidong Electronic Technology Co Ltd
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Abstract

A kind of method of mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus, comprising the steps: will be after homogenizing annealing processes, { 100} texture occupation rate is more than 95% in formation, surface is not enriched with Mn, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb element that electrode potential is higher than aluminum, purity is the mesohigh high-purity aluminum foil of 99.99%, carry out pretreatment and remove the oxide-film on surface, concurrently form new containing moisture film, use fast electrochemical deposition the most in the electrolytic solution, deposit the zinc nucleus of disperse at aluminium foil surface.The surface using the present invention deposited the mesohigh electric aluminum foil of disperse zinc nucleus, when electrolytic etching, zinc nucleus can effectively guide the corrosion hair engaging aperture of aluminium foil, improve the uniformity of Tunnel-hole distribution, reduce aluminium foil from corrosion thinning, thus ratio electric capacity and the warping resistance performance of aluminium foil can be significantly improved.

Description

A kind of method of mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus
Technical field
The present invention relates to aluminium electrolutic capacitor mesohigh anode aluminium foil and the manufacture field of etched foil, specifically a kind of mesohigh The method of aluminium foil surface electro-deposition disperse zinc nucleus.
Background technology
Along with the development of electronic product, based on the medium-high voltage aluminum electrolytic capacitor of components and parts certainly will have high power capacity and little The feature of type, to meet the development need of electronic product.The anode aluminium foil used in medium-high voltage aluminum electrolytic capacitor typically passes through The method of electrochemical corrosion generates substantial amounts of Tunnel-hole to expand its surface area at aluminium foil surface, thus carries high specific capacitance.In order to protect Card mesohigh electrode aluminium foil has required winding performance, and the aluminium foil after corrosion must also have certain hot strength and bending Performance, needs for this to keep the certain thickness aluminum layer not being corroded in the middle of corrosive aluminum foil.Therefore to after making corrosion Aluminium foil maximizing performance, mesohigh aluminium foil, in corrosion process, needs to improve the uniformity, as far as possible of aluminium foil surface pit distribution Certainly the corrosion of aluminium foil surface when avoiding the generation in also hole and reduce hair engaging aperture.
The technique of mesohigh aluminium foil corrosion specifically includes that pretreatment, hair engaging aperture process, expanding treatment before corrosion.During aluminium foil hair engaging aperture, The form in hole and distribution mode are mainly determined by the apparent condition of aluminium foil, and aluminium foil surface pretreatment relates to various physics and the place of chemistry Reason, including heat treatment, surface roughness control, oil removing cleaning, acid, alkali process, cathodic polarization process, anodized, Surface oxidation, deposition inert metal etc..At present, the performance improving mesohigh corrosive aluminum foil both at home and abroad is mainly by two kinds of approach Realize.The first approach: add the trace element such as Pb, Sn, In of ppm level in mesohigh aluminium foil, by annealing Heat treatment makes the trace element such as Pb, Sn, the In in aluminium foil be enriched with at aluminium foil surface, these Pb, Sn, In in the electrolyte Substantial amounts of corrosion micro cell is constituted with aluminum Deng trace element.During anode etching, this of aluminium foil surface existence is the most electric The uniformity of aluminium foil corrosion hair engaging aperture can be improved in pond, and its result is that the uniformity generating Tunnel-hole improves, but the corruption of simultaneously aluminium foil Losing thinning too increasing, the former makes the ratio electric capacity of aluminium foil be improved, and the mechanical performance that the latter makes corrosive aluminum foil declines.Second The approach of kind: improved the uniformity of aluminium foil hair engaging aperture by pretreatment further, even realize the ordered arrangement of Tunnel-hole, make to compare electric capacity It is significantly improved, suppresses the corrosion thinning of aluminium foil simultaneously.
Substantial amounts of research shows, at the sintered metal thin layer that aluminium foil surface sedimentation potential is more positive than aluminum, as Pb, In, Sn, Zn, Fe, Cu etc. so that it is be uniformly adhered to aluminium foil surface, the micro cell that these loose metallic films and the aluminium foil of deposition are constituted can change The uniformity of kind aluminium foil hair engaging aperture.But can accelerate simultaneously aluminium foil surface from corrosion, cause aluminium foil thinning (W.Lin, G.C.Tu, C.F.Lin and Y.M.Peng,The effects of lead impurity on the DC-etching behavior of aluminum for Electrolytic capacitor usage, Corrosion Science, Vol.38, No.6, (1996), pp.889-907.) (W.Lin, G.C.Tu, C.F.Lin and Y.M.Peng,The effects of indium impurity on the DC-etching behavior of aluminum for Electrolytic capacitor usage, Corrosion Science, Vol.39, No.9, (1997), and pp.1531-1543.) the most electric at this Chi Zhong, the metallic in the loose metallic film of deposition is negative electrode, and aluminium foil is anode, thereby increases aluminium foil surface and occurs The active site of corrosion, reduces the critical potential that pitting occurs, thus improves the uniformity of Tunnel-hole hair engaging aperture.But because these The surface density of the loose metallic in metallic film is the highest, defines substantial amounts of corrosion micro cell at aluminium foil surface, and its face is close Spend considerably beyond the surface density needing hair engaging aperture, thus accelerate aluminium foil surface corrosion certainly, cause aluminium foil the most thinning, be i.e. unfavorable for Increasing substantially of electric capacity of ratio, reduces again the utilization rate of aluminium foil and the mechanical property of etched foil.Therefore, at mesohigh aluminium foil table The technology of face deposition Pb, In, Sn, Zn, Fe, Cu isoelectric level calibration thin metal layer does not obtains so far in electric aluminum foil industry Must apply.
The method using quick electrodeposition deposits the stannum nucleus of disperse at aluminium foil surface, guides the corrosion hair engaging aperture of aluminium foil, obtains Preferable effect (the patent number of accepting: 201310302175.5).Zinc is as the current potential element more positive than aluminum, it is also possible to aluminum substrate Constitute local micro cell and guide the corrosion hair engaging aperture of aluminium foil, and the electrode potential of zinc is than the negative (Zn of stannum2+:-0.763V,Sn4+: + 0.05V), i.e. can guide the corrosion hair engaging aperture of aluminium foil, be not easy again to cause excessive erosion, the electricity ratio electricity that additionally electrodepositing zinc needs Deposition stannum is low, is conducive to improving the quality of aluminium foil hair engaging aperture and reducing production cost.
Owing to aluminum is the most active metal, its surface is very easy to generate the oxide-film of protectiveness.It is perpendicular to aluminium foil to generate Epontic Tunnel-hole, mesohigh electric aluminum foil must have that { 100} texture, { 100} texture, aluminium foil needs to exist in order to obtain 500-600 DEG C carries out long term annealing process.But, in this annealing process, the oxide-film of aluminium foil surface becomes more to cause Close, become the obstacle of follow-up electrolytic etching hair engaging aperture.Therefore, when traditional mesohigh aluminium foil electrolytic etching hair engaging aperture, it is necessary to carry out This layer of fine and close oxide-film is removed by pretreatment, forms the new thin film containing a large amount of defects and is beneficial to the formation of Tunnel-hole.At electricity During deposition zinc nucleus, owing to there is fine and close oxide-film through the aluminium foil surface of 500-600 DEG C of long term annealing, therefore can not be Its surface Direct precipitation goes out zinc nucleus.One of key technology of the present invention is exactly to remove the fine and close oxygen of aluminium foil surface through pretreatment Change film, then form new aqueous film.During electrodepositing zinc, zinc ion can pass through this layer of aqueous film, at aluminum Surface deposits zinc nucleus.
Summary of the invention
A kind of method that it is an object of the invention to provide mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus, aluminium foil can be through Cross pretreatment and remove the fine and close oxide-film on its surface, and formed new containing moisture film.Electrodepositing zinc nucleus is out-of-date in the electrolytic solution, Zinc ion by this layer containing moisture film, thus can deposit the zinc nucleus of disperse at aluminium foil surface.
The present invention reaches above-mentioned purpose by the following technical solutions: a kind of mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus Method, comprises the steps: that { 100} texture occupation rate is more than 95%, and surface is or not formation by after homogenizing annealing processes Mn, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb element that enrichment electrode potential is higher than aluminum, purity It is the mesohigh high-purity aluminum foil of 99.99%, in high purity water or aqueous slkali or phosphoric acid solution or in salpeter solution, carries out pre-place Manage or carry out in sulphuric acid-sulfuric acid solution electrochemical polishing treatment, remove the oxide-film on surface, form new containing at aluminium foil surface Water thin film, then uses quick electrodeposition technology in the electrolyte of deposition zinc nucleus, and zinc ion can penetrate containing of aluminium foil surface Water thin film, deposits the zinc nucleus of disperse at aluminium foil surface.
Concrete operation step is: the mesohigh high-purity aluminum foil after homogenizing annealing processes is placed in the height that temperature is 60~100 DEG C Decocting in water 5~50 seconds in pure water, or temperature be 15~70 DEG C of concentration be 0.5~1.5mol/L aqueous slkali in process 5~30 seconds, or The phosphoric acid solution that 40~60 DEG C of concentration is 0.1~1mol/L processes 30~60 seconds, or temperature be 30~70 DEG C of concentration be 0.5~2 The salpeter solution of mol/L processes 10~40 seconds, or temperature be 40~70 DEG C containing 5~14mol/L phosphoric acid+5~10mol/L sulfur Carrying out electrobrightening process in acid+0.1~1mol/L glycerol mixed solution, polishing electric current density is 30~120mA/cm2, polishing Time is 10~60 seconds, removes the oxide-film on surface and is formed new containing moisture film.Afterwards, by above-mentioned handle well have aqueous thin The aluminium foil of film is placed in the electrolyte containing zinc ion and carries out electro-deposition, and electrolyte becomes: 0.01~0.5mol/L zinc oxide + 0.02~0.2mol/L sodium hydroxide;Temperature is 30~60 DEG C;With graphite as anode, form the new middle height containing moisture film with surface Jewelling paper tinsel is negative electrode;Aluminium foil charged entrance electrolyte during electro-deposition disperse stannum nucleus, wherein the electric current density of electro-deposition is 5~60 mA/cm2, electrodeposition time is 5~30 seconds.
The present invention is directed to aluminium foil problem present in the anode etching of the sintered metal thin layer of surface sedimentation potential calibration, send out Understand the new method being gone out disperse zinc nucleus on mesohigh high-purity aluminum foil surface by electrochemical deposition.The problem that former method exists is main For: although this loose thin metal layer can improve the uniformity of aluminium foil hair engaging aperture, but can strongly accelerate the corrosion certainly of aluminium foil surface, Cause the thinning of aluminium foil, not only bad for increasing substantially the ratio electric capacity of etched foil, and reduce utilization rate and the corrosion of aluminium foil The mechanical property of paper tinsel, in the present invention, slightly larger than needs hair engaging aperture by the surface density making disperse zinc nucleus that electro-deposition obtains Surface density solves the problems referred to above, and its principle and technical advantage are as follows:
1. constituting micro cell between disperse zinc nucleus and aluminium foil, during anode electrolysis, these micro cells become and preferentially produce tunnel The active position in hole, road, can control the density of hair engaging aperture, improves the uniformity of hair engaging aperture, reduces and the generation in hole, thus can show Write the ratio electric capacity improving corrosive aluminum foil.
2. owing to constituting the significantly decline of the quantity of the micro cell thin metal layer more loose than deposition between disperse zinc nucleus and aluminium foil, Causing in addition to hair engaging aperture position, the micro cell on other surface of aluminium foil is little, therefore in addition to hair engaging aperture position, and the corruption certainly on other surface of aluminium foil Erosion Reducing thickness declines, and is remarkably improved utilization rate and the mechanical performance of corrosive aluminum foil.
3. when the aluminium foil using the deposition disperse zinc nucleus of the present invention carries out anode etching, owing to aluminium foil overwhelming majority surface is Rafifinal, thus insensitive to the impurity of etchant solution, can allow in etchant solution containing higher impurity content, Bu Huizao Become significant aluminium foil from corrosion thinning, reduce the difficulty of aluminium foil corrosion solution Industry Control, foil industry corrosion products can be improved Quality.
4. the method for the deposition disperse zinc nucleus of the present invention can be as the last treatment technology of manufacture mesohigh electronics aluminium foil, system Make novel mesohigh electronics aluminium foil;Can also manufacture high-quality as the pretreatment technology of manufacture mesohigh electronics aluminum etched foil The mesohigh electronics aluminum etched foil of amount.
Accompanying drawing explanation
Fig. 1 is the aluminum using the method for heretofore described mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus to prepare The scanning electron microscope pattern of paper tinsel surface electro-deposition disperse zinc nucleus.
Detailed description of the invention
By the following examples technical scheme is further described.
Using the aluminium foil of the zinc nucleus that surface deposits disperse in the present invention to carry out hair engaging aperture corrosion, hair engaging aperture solution is 0.8mol/L hydrochloric acid The aluminum ions mixed solution of+3.6mol/L sulphuric acid+0.8mol/L, temperature is 75 DEG C, then carries out reaming corrosion, and reaming solution is The salpeter solution of 0.07mol/L, temperature is 70 DEG C, and post processing is salpeter solution, cleans, and dries, finally according to industry standard Carry out 520V chemical conversion.
Comparative example
Purity is 99.99%, and thickness is 120 μm, the height of the cubic texture occupancy rate surface enrichment micro lead element more than 95% Pure aluminum foil, uses traditional mixed acid pretreating process, and pretreatment fluid used is 1mol/L hydrochloric acid+3mol/L sulphuric acid, temperature Degree is 80 DEG C, is directly soaked 120 seconds by aluminium foil in pretreatment fluid, then carries out place after above-mentioned hair engaging aperture burn into reaming burn into Reason and 520V chemical conversion treatment.
Embodiment 1
Being 99.99% by purity, thickness is 110 μm, cubic texture occupancy rate more than 95% through homogenizing annealing rear surface Be not enriched with these electrode potentials of Mn, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb higher than aluminum in high Pressure high-purity aluminum foil is placed in decocting in water 30 seconds in 95 DEG C of boiling water, aluminium foil surface formed new containing moisture film after.Above-mentioned aluminium foil is placed in electricity Solving in liquid and carry out electrodepositing zinc nucleus process, the composition of electrolyte is: 0.3mol/L zinc oxide+0.1mol/L sodium hydroxide;With Graphite is anode, defines the new mesohigh aluminium foil containing moisture film with the above-mentioned surface through decocting in water as negative electrode, by charged for aluminium foil enter Entering in electrolyte, wherein the temperature of electrolyte is 40 DEG C, and the electric current density of electro-deposition is 25mA/cm2, electrodeposition time is 15 Second.
The above-mentioned aluminium foil obtaining disperse zinc nucleus by being electrodeposited in surface is carried out hair engaging aperture corrosion, and hair engaging aperture solution is 0.8 The mixed solution of mol/L hydrochloric acid+3.6mol/L sulphuric acid+0.8mol/L, temperature is 75 DEG C, then carries out the reaming identical with comparative example Corrosion, post processing and 520V chemical conversion treatment.
Embodiment 2
Being 99.99% by purity, thickness is 110 μm, cubic texture occupancy rate more than 95% through homogenizing annealing rear surface Be not enriched with these electrode potentials of Mn, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb higher than aluminum in high Pressure high-purity aluminum foil be placed in temperature be 60 DEG C of concentration be 1mol/L aqueous slkali in process 15 seconds, formed new aqueous at aluminium foil surface After film.Being placed in electrolyte by above-mentioned aluminium foil and carry out electrodepositing zinc nucleus process, the composition of electrolyte is: 0.3mol/L zinc oxide + 0.1mol/L sodium hydroxide;With graphite as anode, define the new mesohigh aluminum containing moisture film with the above-mentioned surface through decocting in water Paper tinsel is negative electrode, and by charged for aluminium foil entrance electrolyte, wherein the temperature of electrolyte is 40 DEG C, and the electric current density of electro-deposition is 25 mA/cm2, electrodeposition time is 15 seconds.
The above-mentioned aluminium foil obtaining disperse zinc nucleus by being electrodeposited in surface is carried out hair engaging aperture corrosion, and hair engaging aperture solution is 0.8 The mixed solution of mol/L hydrochloric acid+3.6mol/L sulphuric acid+0.8mol/L, temperature is 75 DEG C, then carries out the reaming identical with comparative example Corrosion, post processing and 520V chemical conversion treatment.
Embodiment 3
Being 99.99% by purity, thickness is 110 μm, cubic texture occupancy rate more than 95% through homogenizing annealing rear surface Be not enriched with these electrode potentials of Mn, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb higher than aluminum in high Pressure high-purity aluminum foil is placed in the phosphoric acid solution that 60 DEG C of concentration is 0.5mol/L and processes 30~60 seconds, forms new containing at aluminium foil surface Moisture film.Being placed in electrolyte by above-mentioned aluminium foil and carry out electrodepositing zinc nucleus process, the composition of electrolyte is: 0.3mol/L zinc oxide + 0.1mol/L sodium hydroxide;With graphite as anode, define the new mesohigh aluminum containing moisture film with the above-mentioned surface through decocting in water Paper tinsel is negative electrode, and by charged for aluminium foil entrance electrolyte, wherein the temperature of electrolyte is 40 DEG C, and the electric current density of electro-deposition is 25 mA/cm2, electrodeposition time is 15 seconds.
The above-mentioned aluminium foil obtaining disperse zinc nucleus by being electrodeposited in surface is carried out hair engaging aperture corrosion, and hair engaging aperture solution is 0.8 The mixed solution of mol/L hydrochloric acid+3.6mol/L sulphuric acid+0.8mol/L, temperature is 75 DEG C, then carries out the reaming identical with comparative example Corrosion, post processing and 520V chemical conversion treatment.
Embodiment 4
Being 99.99% by purity, thickness is 110 μm, cubic texture occupancy rate more than 95% through homogenizing annealing rear surface Be not enriched with these electrode potentials of Mn, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb higher than aluminum in high Pressure high-purity aluminum foil is placed in the salpeter solution that 60 DEG C of concentration is 1mol/L and processes the oxide-film removing surface for 30 seconds, at aluminium foil surface Formed new containing moisture film.Being placed in electrolyte by above-mentioned aluminium foil and carry out electrodepositing zinc nucleus process, the composition of electrolyte is: 0.3 Mol/L zinc oxide+0.1mol/L sodium hydroxide;With graphite as anode, define new containing moisture film with the above-mentioned surface through decocting in water Mesohigh aluminium foil be negative electrode, by charged for aluminium foil entrance electrolyte, wherein the temperature of electrolyte is 40 DEG C, the electric current of electro-deposition Density is 25mA/cm2, electrodeposition time is 15 seconds.
The above-mentioned aluminium foil obtaining disperse zinc nucleus by being electrodeposited in surface is carried out hair engaging aperture corrosion, and hair engaging aperture solution is 0.8 The mixed solution of mol/L hydrochloric acid+3.6mol/L sulphuric acid+0.8mol/L, temperature is 75 DEG C, then carries out the reaming identical with comparative example Corrosion, post processing and 520V chemical conversion treatment.
Embodiment 5
Being 99.99% by purity, thickness is 110 μm, cubic texture occupancy rate more than 95% through homogenizing annealing rear surface Be not enriched with these electrode potentials of Mn, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb higher than aluminum in high Pressure high-purity aluminum foil is placed in polishing fluid and carries out electrochemical polishing treatment, and the composition of polishing fluid is: 12mol/L phosphoric acid+7.6mol/L Sulphuric acid+0.2mol/L glycerol mixed solution;Polishing electric current density when being polished is 60mA/cm2, polishing time is 30 seconds, Formed new containing moisture film at aluminium foil surface.Above-mentioned aluminium foil is placed in electrolyte and carries out electrodepositing zinc nucleus process, the one-tenth of electrolyte It is divided into: 0.3mol/L zinc oxide+0.1mol/L sodium hydroxide;With graphite as anode, define with the above-mentioned surface through decocting in water The new mesohigh aluminium foil containing moisture film is negative electrode, and by charged for aluminium foil entrance electrolyte, wherein the temperature of electrolyte is 40 DEG C, electricity The electric current density of deposition is 25mA/cm2, electrodeposition time is 15 seconds.
The above-mentioned aluminium foil obtaining disperse zinc nucleus by being electrodeposited in surface is carried out hair engaging aperture corrosion, and hair engaging aperture solution is 0.8 The mixed solution of mol/L hydrochloric acid+3.6mol/L sulphuric acid+0.8mol/L, temperature is 75 DEG C, then carries out the reaming identical with comparative example Corrosion, post processing and 520V chemical conversion treatment.
Table 1 is to use surface of the present invention to deposit the aluminium foil of disperse zinc nucleus in anode etching and change in comparative example and embodiment Cheng Hou, the corrosion thinning amount of aluminium foil, ratio electric capacity and bending times, it can be seen that use surface of the present invention to deposit the zinc crystalline substance of disperse The aluminium foil of core, corrosion thinning reduces 1-3mm, improves more than 5% than electric capacity, and bending times improves about 15%. The aluminium foil corrosion Reducing thickness of table 1 comparative example and embodiment, than electric capacity and bending times
Sample Corrosion thinning amount Than electric capacity (μ F/cm2) Bending times
Comparative example 5μm 0.736 17
Embodiment 1 3μm 0.778 21
Embodiment 2 4μm 0.760 20
Embodiment 3 4μm 0.770 20
Embodiment 4 2μm 0.795 21
Embodiment 5 3μm 0.783 20

Claims (4)

1. a method for mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus, is characterized in that, comprise the steps: warp Cross after homogenizing annealing processes, formed 100} texture occupation rate more than 95%, and surface be not enriched with the electrode potential Mn higher than aluminum, Fe, Co, Ni, Cu, Zn, Cd, Ga, Ge, In, Sn, Pb element, purity is the mesohigh high-purity aluminum foil of 99.99%, High purity water or aqueous slkali or phosphoric acid solution or salpeter solution carry out carrying out in pretreatment, or phosphorus acid-sulfur acid mixed solution Electrochemical polish pretreatment, to remove the oxide-film on surface, is formed new containing moisture film at aluminium foil surface simultaneously;Then at deposition zinc The electrolyte of nucleus uses fast electrochemical deposition zinc nucleus technology, deposits the zinc nucleus of disperse at aluminium foil surface.
The method of electro-deposition disperse zinc nucleus in mesohigh electric aluminum foil surface the most according to claim 1, is characterized in that: institute State and carry out pretreatment in high purity water or aqueous slkali or phosphoric acid solution or salpeter solution, be will to process through homogenizing annealing After mesohigh high-purity aluminum foil process 5~50 seconds in 60~100 DEG C of high purity waters;Or at 15~70 DEG C, concentration is 0.5~1.5mol/L Aqueous slkali in process 5~30 seconds;Or at 40~60 DEG C, concentration be 0.1~1mol/L phosphoric acid solution in process 30~60 seconds, Or at 30~70 DEG C, concentration be 0.5~2mol/L salpeter solution in process 10~40 seconds;Remove the oxide-film of aluminium foil surface, water Wash, formed at aluminium foil surface new containing moisture film.
The method of electro-deposition disperse zinc nucleus in mesohigh electric aluminum foil surface the most according to claim 1, is characterized in that: institute State in phosphorus acid-sulfur acid mixed solution, carry out electrochemical polish pretreatment, be by high-purity for the mesohigh after homogenizing annealing processes Aluminium foil, is 40~70 DEG C in temperature, molten containing 5~14mol/L phosphoric acid+5~10mol/L sulphuric acid+0.1~1mol/L glycerol mixing Carrying out electrobrightening process in liquid, wherein, polishing electric current density is 30~120mA/cm2, polishing time is 10~60 seconds, water Wash, formed at aluminium foil surface new containing moisture film.
4. according to the method for the mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus described in claim 1,2,3, its feature It is: described employing fast electrochemical deposition zinc nucleus technology in the electrolyte of deposition zinc nucleus, deposits disperse at aluminium foil surface Zinc nucleus, consisting of of its electro-deposition disperse zinc nucleus electrolyte: 0.01~0.5mol/L zinc oxide+0.02~0.2mol/L hydrogen-oxygen Changing sodium, temperature is 30~60 DEG C;With graphite cake as anode during deposition zinc nucleus, surface forms the new mesohigh aluminium foil containing moisture film For negative electrode, aluminium foil charged entrance electrolyte, the electric current density of electro-deposition is 5~60mA/cm2, electrodeposition time is 5~30 seconds.
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CN104357886B (en) * 2014-10-30 2017-10-17 广西贺州桂海铝业科技有限公司 The method that mesohigh anode deposits disperse tin, zinc nucleus with high-purity aluminum foil surface chemistry
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CN104733181B (en) * 2015-02-16 2017-06-06 广西正润新材料科技有限公司 Mesohigh anode deposits the method and device of disperse tin, zinc nucleus with high-purity aluminum foil surface spray
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100813142B1 (en) * 2006-11-03 2008-03-13 김현규 Reflective sheet and the method of preparing it
CN101752095A (en) * 2009-12-28 2010-06-23 广西贺州市桂东电子科技有限责任公司 Method for etching holes by corroding aluminum foil
CN103198925A (en) * 2013-04-28 2013-07-10 广西贺州市桂东电子科技有限责任公司 Method for controlling distribution of mesohigh electronic aluminum foil etching holes
CN103361692A (en) * 2013-07-15 2013-10-23 广西贺州市桂东电子科技有限责任公司 Medium-high voltage electronic aluminum foil diffused tin nucleus electro-deposition method
CN103451713A (en) * 2013-08-28 2013-12-18 广西贺州市桂东电子科技有限责任公司 Corrosion pretreatment method for anode oxidation deposited zinc/tin crystal nucleus of middle-high voltage electronic aluminum foil

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100813142B1 (en) * 2006-11-03 2008-03-13 김현규 Reflective sheet and the method of preparing it
CN101752095A (en) * 2009-12-28 2010-06-23 广西贺州市桂东电子科技有限责任公司 Method for etching holes by corroding aluminum foil
CN103198925A (en) * 2013-04-28 2013-07-10 广西贺州市桂东电子科技有限责任公司 Method for controlling distribution of mesohigh electronic aluminum foil etching holes
CN103361692A (en) * 2013-07-15 2013-10-23 广西贺州市桂东电子科技有限责任公司 Medium-high voltage electronic aluminum foil diffused tin nucleus electro-deposition method
CN103451713A (en) * 2013-08-28 2013-12-18 广西贺州市桂东电子科技有限责任公司 Corrosion pretreatment method for anode oxidation deposited zinc/tin crystal nucleus of middle-high voltage electronic aluminum foil

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"电沉积弥散锡晶核对高压阳极铝箔电解腐蚀特性的影响";彭宁等;《中国有色金属学报》;20131215;第23卷(第12期);第3368页左栏第3-5段,第3371页左栏第1段, *

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