Summary of the invention
The problems referred to above to conventional art; The invention provides a kind of manufacturing approach of 100~150V low-pressure chemical synthesis foil; It has following advantage: can generate firm oxide-film simultaneously; Reduce follow-up changing into and formed the loss that specific area is brought, reach the comprehensive purpose that improves aluminium foil static capacity and water resistance for aluminium foil.
For this reason; Technical solution of the present invention is a kind of manufacturing approach of 100~150V low-pressure chemical synthesis foil; Comprise changing into processing through the aluminium foil of corrosion behind the expansion face is multistage; And said multistage change into processing before, soak into treatment step A earlier as follows: will in wetting dispersion liquid, soak into processing through the aluminium foil of corrosion behind the expansion face; This wetting dispersion liquid is hydrophilic lipophilic balance HLB at the aqueous solution of 11~15 non-ionic surface active agent.
Possibly bring the analysis of loss to find on the basis for preceding place hole that aluminium foil forms and specific area follow-up changing into; In order to reduce the problem that oxide-film due to the subsequent treatment blocks pore; The manufacturing approach of low-pressure chemical synthesis foil of the present invention is optimized before changing into step originally as follows in addition: etched foil carry out anodised change into processing before; The Ricinate that water oil equilibrium valve HLB prepares at 11~15 non-ionic surface active agent soaks into it; Embodiment of the invention measured data proves: method of the present invention can effectively reduce follow-up changing into for aluminium foil and form the loss that specific area is brought, reaches comprehensive raising aluminium foil specific volume and water-fast purpose of closing performance.
Measured data is improved fully to be proved; Method of the present invention has realized following improvement mechanism: moistening dispersion liquid can infiltrate in the existing hole drives away the bubble that possibly accumulate; Aluminium foil surface can also adhere to the layer of surface activating agent; Drop into aluminium foil to change in the subsequent treatment liquid again and wait when handling, under the fully stable prerequisite of the moistening dispersion liquid little interference subsequent treatment liquid of assurance, treatment fluid composition, effectively improve the aluminium foil interfacial tension; One can effectively eliminate the bubble in the corrosion hole; Thereby prevent that the opening part of a large amount of pores from forming the pore of oxide-film shutoff etched foil, two come the most of pore that enters into etched foil that subsequent treatment liquid just can be very fast to react, and are convenient to form firm oxide film dielectric layer in the inner surface of pore.
In order further to improve, stablize wetting dispersion liquid to through the improving effect, prevent that other unnecessary physics and chemistry from disturbing of the aluminium foil interfacial tension of corrosion behind the expansion face, manufacturing approach of the present invention also comprises following improvement:
Non-ionic surface active agent in the said wetting dispersion liquid is an APEO.
Non-ionic surface active agent molecular structure in the said wetting dispersion liquid is R (OCH
2CH
2)
nH, wherein n=9~12.
Concentration in the said wetting dispersion liquid is 0.1~1ml/L.
In order further to improve the efficient and the effect of wetting dispersion treatment, manufacturing approach of the present invention also comprises following improvement:
The temperature of wetting dispersion liquid is controlled to be 10~50 ℃ in the said steps A, and the infiltration processing time is 0.5~5min.
The temperature of wetting dispersion liquid is controlled to be 20~30 ℃ in the said steps A, and the infiltration processing time is 1~3min; The concentration of non-ionic surface active agent is 0.1~0.5ml/L.
To handle in order cooperating to soak into, further to consolidate static capacity and the resistance to water that improves aluminium foil from subsequent step, manufacturing approach of the present invention also comprises on the following subsequent step to be improved:
Step B: the aluminium foil that will soak into carries out the multistage processing that changes in ammonium adipate solution;
Step C: the aluminium foil after multistage the changing into is cleaned, in phosphoric acid solution, carry out Passivation Treatment then;
Step D: the aluminium foil after the passivation is cleaned, then heat treatment under air atmosphere.
Step e: place ammonium dihydrogen phosphate to become voltage to repair on the aluminium foil after the heat treatment and change into processing with the multistage maximum that changes into processing procedure;
Step F: the aluminium foil after repairing changed into cleans heat treatment once more under air atmosphere then once more;
Step G: the aluminium foil after the heat treatment places ammonium dihydrogen phosphate to carry out reprocessing once more;
Step H: the aluminium foil after the reprocessing is placed air oven dry, rolling.
Said step B adopts three grades and changes into processing, adopts maximum to become 40% ± 3%, 70% ± 3%, 100% change into of voltage successively; Saidly change into that handle to use ammonium adipate solution concentration be 0.2~0.5mol/L, temperature is 70~90 ℃, the constant voltage time 5~15min that change at different levels.
Among the said step C, phosphoric acid solution concentration is that 0.2~0.4mol/L, temperature are 40~60 ℃, soak time 1~3min.
The heat treatment of said step D is after the aluminium foil of handling through phosphoric acid is cleaned with pure water, directly to place 400~450 ℃ air atmosphere to handle 1~5min without other process; The heat treatment of said step F is after aluminium foil cleaned with pure water after repairing was changed into, in 500~580 ℃ air atmosphere, to handle 2~6min.
The inventive method experiment effect discloses: tradition is handled with phosphoric acid changing into the paper tinsel list; Can only open the blocked hole of aluminium foil surface; And before phosphoric acid is handled, with 400~450 ℃ temperature aluminium foil is heat-treated; The inner blocked hole of aluminium foil is opened, and the air that is wrapped in the hole also is released out, then aluminium foil remake to repair and change into processing and then can in the hole of opening, form oxide-film again; Finally reach and improve the aluminium foil static capacity, coating mass is also better guaranteed.
Measured data proves that the manufacturing approach of low-pressure chemical synthesis foil of the present invention can improve the about 4-9% of static capacity, significantly improve water resistance etc., and is remarkable for the certain effect of whole premium properties that realizes low-pressure chemical synthesis foil.
Below in conjunction with specific embodiment the present invention is further specified.
Embodiment
Embodiment 1:
Making operating voltage according to method of the present invention is the aluminium foil of 80V, sets maximum and becomes voltage (formation voltage) to be 105V, specific as follows:
1) will place 25 ℃ through the aluminium foil of corrosion behind the expansion face, concentration is to soak into 2min in the wetting dispersion liquid of APES OP-10 of 0.1ml/L, and its HLB value is 13.3~14.5;
2) will soak into aluminium foil after handling and in 80 ℃, 0.4mol/L ammonium adipate solution, carry out one-level and change into, boost to constant voltage 5min behind the 42V;
3) aluminium foil after one-level is changed into carries out secondary and changes in 80 ℃, 0.4mol/L ammonium adipate solution, boosts to constant voltage 5min behind the 74V;
4) aluminium foil after secondary is changed into carries out three grades and changes in 80 ℃, 0.4mol/L ammonium adipate solution, boosts to constant voltage 8min behind the 105V;
5) aluminium foil after three grades are changed into cleans and in 50 ℃, 0.3mol/L phosphoric acid solution, soaks passivation 2min;
6) aluminium foil after the Passivation Treatment is cleaned and in air atmosphere, heat-treats, 420 ℃ of temperature, time 2min;
7) the constant voltage 5min under 105V of the aluminium foil after the heat treatment is repaired change into processing, used solution is 80 ℃, 0.2mol/L ammonium dihydrogen phosphate;
8) aluminium foil after repairing is changed into cleans and in air atmosphere, carries out heat treatment once more, 520 ℃ of temperature, time 2min;
9) will be once more aluminium foil after the heat treatment place aftertreatment fluid to carry out reprocessing, aftertreatment fluid is 80 ℃, the ammonium dihydrogen phosphate of 0.2mol/l, soaks 2min;
10) aluminium foil after the reprocessing is cleaned once more and under air atmosphere with 150 ℃ of hot blast drying aluminium foils, rolling gets final product.
Adopt same comparative sample to handle according to traditional processing technology, its maximum becomes voltage still to be 105V.Respectively two kinds of finished products are tested, method of testing is undertaken by SJ/T 11140 standards, and test result is listed in the table 1.
Embodiment 2:
Making operating voltage according to method of the present invention is the aluminium foil of 100V, sets maximum and becomes voltage (formation voltage) to be 132V, specific as follows:
1) will place 30 ℃ through the aluminium foil of corrosion behind the expansion face, concentration is to soak into 3min in the wetting dispersion liquid of NPE NP-7 of 0.1ml/L; Its HLB value is 11.7~12;
2) will soak into aluminium foil after handling and in 80 ℃, 0.4mol/L ammonium adipate solution, carry out one-level and change into, boost to constant voltage 8min behind the 53V;
3) aluminium foil after one-level is changed into carries out secondary and changes in 80 ℃, 0.4mol/L ammonium adipate solution, boosts to constant voltage 8min behind the 93V;
4) aluminium foil after secondary is changed into carries out three grades and changes in 80 ℃, 0.4mol/L ammonium adipate solution, boosts to constant voltage 12min behind the 132V;
5) aluminium foil after three grades are changed into cleans and in 50 ℃, 0.3mol/L phosphoric acid solution, soaks passivation 2min;
6) aluminium foil after the Passivation Treatment is cleaned and in air atmosphere, heat-treats, 400 ℃ of temperature, time 4min;
7) the constant voltage 8min under 132V of the aluminium foil after the heat treatment is repaired change into processing, used solution is 80 ℃, 0.2mol/L ammonium dihydrogen phosphate;
8) aluminium foil after repairing is changed into cleans and in air atmosphere, carries out heat treatment once more, 520 ℃ of temperature, time 2min;
9) will be once more aluminium foil after the heat treatment place aftertreatment fluid to carry out reprocessing, aftertreatment fluid is 85 ℃, the ammonium dihydrogen phosphate of 0.2mol/l, soaks 2min;
10) aluminium foil after the reprocessing is cleaned once more and under air atmosphere with 150 ℃ of hot blast drying aluminium foils, rolling gets final product.
Adopt same comparative sample to handle according to traditional processing technology, its maximum becomes voltage still to be 132V.Respectively two kinds of finished products are tested, method of testing is undertaken by SJ/T 11140 standards, and test result is listed in the table 1.
Embodiment 3:
According to the aluminium foil that method system operating voltage of the present invention is 80V, set maximum and become voltage (formation voltage) to be 115V, specific as follows:
1) will place 25 ℃ through the aluminium foil of corrosion behind the expansion face, concentration is to soak into 2min in the wetting dispersion liquid of APES OP-10 of 0.3ml/L, and its HLB value is 13.3~14.5;
2) will soak into aluminium foil after handling and in 80 ℃, 0.4mol/L ammonium adipate solution, carry out one-level and change into, boost to constant voltage 7min behind the 46V;
3) aluminium foil after one-level is changed into carries out secondary and changes in 80 ℃, 0.4mol/L ammonium adipate solution, boosts to constant voltage 7min behind the 80V;
4) aluminium foil after secondary is changed into carries out three grades and changes in 80 ℃, 0.4mol/L ammonium adipate solution, boosts to constant voltage 10min behind the 115V;
5) aluminium foil after three grades are changed into cleans and in 50 ℃, 0.3mol/L phosphoric acid solution, soaks passivation 2min;
6) aluminium foil after the Passivation Treatment is cleaned and in air atmosphere, heat-treats, 420 ℃ of temperature, time 3min;
7) the constant voltage 7min under 115V of the aluminium foil after the heat treatment is repaired change into processing, used solution is 80 ℃, 0.2mol/L ammonium dihydrogen phosphate;
8) aluminium foil after repairing is changed into cleans and in air atmosphere, carries out heat treatment once more, 520 ℃ of temperature, time 2min;
9) will be again aluminium foil after the heat treatment place aftertreatment fluid to carry out reprocessing, aftertreatment fluid is 80 ℃, the ammonium dihydrogen phosphate of 0.3mol/l, soaks 2min;
10) aluminium foil after the reprocessing is cleaned once more and under air atmosphere with 150 ℃ of hot blast drying aluminium foils, rolling gets final product.
Adopt same comparative sample according to tradition production technology to be handled, its maximum becomes voltage still to be 115V.Respectively two kinds of finished products are tested, method of testing is undertaken by SJ/T 11140 standards, and test result is listed in the table 1.
Table 1
Contrast can know, the aluminium foil that adopts method of the present invention to make, and its static capacity is apparently higher than about the about 4-9% of traditional handicraft, and performances such as pressure rising time, oxide-film withstand voltage, resistance to water all are superior to traditional handicraft.