CN108878141A - A kind of preparation method of hydrochloric acid reaming high-field electrode foil - Google Patents
A kind of preparation method of hydrochloric acid reaming high-field electrode foil Download PDFInfo
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- CN108878141A CN108878141A CN201810453858.1A CN201810453858A CN108878141A CN 108878141 A CN108878141 A CN 108878141A CN 201810453858 A CN201810453858 A CN 201810453858A CN 108878141 A CN108878141 A CN 108878141A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000011888 foil Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000005030 aluminium foil Substances 0.000 claims abstract description 77
- 238000005406 washing Methods 0.000 claims abstract description 66
- 230000007797 corrosion Effects 0.000 claims abstract description 46
- 238000005260 corrosion Methods 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- 238000000866 electrolytic etching Methods 0.000 claims description 23
- 239000000654 additive Substances 0.000 claims description 18
- 230000000996 additive effect Effects 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 239000008399 tap water Substances 0.000 claims description 16
- 235000020679 tap water Nutrition 0.000 claims description 16
- 238000002203 pretreatment Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000012805 post-processing Methods 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 3
- 239000013543 active substance Substances 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 14
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 6
- 230000007812 deficiency Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002699 waste material Substances 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012851 eutrophication Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 208000012639 Balance disease Diseases 0.000 description 1
- 241001474374 Blennius Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 231100000880 dysequilibrium Toxicity 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Cell Electrode Carriers And Collectors (AREA)
- ing And Chemical Polishing (AREA)
Abstract
The invention discloses a kind of preparation method of hydrochloric acid reaming high-field electrode foil, aluminium foil is carried out three-level corrosion treatment and Pyatyi washing process by this method.Replace nitric acid using hydrochloric acid, realizes NO3 ‑Zero-emission;Overcoming ELNA technique hydrochloric acid, simultaneously hole, capacity are low, the deficiency that nitric acid process aperture is small, foil is crisp;Cl‑Replace NO3 ‑, realized by film recovery system and repeat to recycle, reduce purchasing of raw materials cost, realized the discharge of spent acid ammonia nitrogen no pollution, reduce the pollution to water body;By changing the technique of hair engaging aperture and reaming stage, realize that aperture is big, corrosion preparation of high capacity etched foil.
Description
Technical field
The invention belongs to electrode foils to corrode preparation field, and in particular to a kind of preparation side of hydrochloric acid reaming high-field electrode foil
Method.
Background technique
With the development of electronics industry, the military expansion with commercial market such as household electrical appliances, communication, aerospace, to electrode foil
The especially demand sharp increase of Fabrication of High Specific Capacitance electrode foil, thus increase the specific surface area of light foil, improve intensity, manufacture high-performance is rotten
Erosion foil falls over each other the direction of research at everybody.
Before 2008, the country adopt substantially Japan ELNA etching process, using hydrochloric acid carry out reaming, and hydrochloric acid from
The halogen characteristic of son causes aperture uneven, is easy to produce simultaneously hole, capacity is relatively low, can not meet the demand in market, therefore
It begins one's study after 2008, in industry and gradually has developed the technique for carrying out reaming with nitric acid, be correspondingly improved corrosion
Capacity.But nitric acid reaming speed is slow, etched foil is crisp, and capacity attenuation is big, is unfavorable for being melted into the production of line and the winding of Waste Acid From Hua Cheng Foil
And hacking.
Meanwhile nitric acid chambering process can generate a large amount of NO3 -Although how corrosion industry investment substantial contribution research and development separate back
NO3 -, effective processing scheme is not obtained but.NO3 -Emission treatment if not up to standard, it is exceeded to will cause water body ammonia nitrogen(It is also water
Main oxygen consumption pollutant in body), dissolved oxygen in ammonium oxidation decomposition and consumption water makes water body black smelly.In oxygen abundance
In the case where, ammonia nitrogen can be nitrite nitrogen by microbiological oxidation, and then be decomposed into nitrate nitrogen, nitrite nitrogen and protein
In conjunction with nitrosamine is generated, there is carcinogenic and teratogenesis, this is very unfavorable to water correction and protection.In addition, ammonia nitrogen can be algae
Class growth provides nutrient source, stimulates and accelerate the growth of water plant, if the raised growth of seaweed, water plant is bred, increases water body
Eutrophication odds leads to water ecology dysequilibrium.Harm based on the above ammonia nitrogen to water environment, ammonia nitrogen waste water pair
The influence of environment has caused the attention of environment protection field or even global range.Country reinforces the attention to environmental protection, nitric acid reaming at present
Technique has been unable to satisfy the requirement of environmental protection, will be gradually by market.
Summary of the invention
It is an object of the invention to manufacture the corroding electrode foil with large aperture, high capacity, replaces nitric acid with hydrochloric acid, realize
NO3 -Zero-emission;Overcoming ELNA technique hydrochloric acid, simultaneously hole, capacity are low, the deficiency that nitric acid process aperture is small, foil is crisp;Cl-Replace NO3 -,
It is realized by film recovery system and repeats to recycle, reduce purchasing of raw materials cost, realize the discharge of spent acid ammonia nitrogen no pollution.Therefore originally
Invention provides a kind of preparation method of hydrochloric acid reaming high-field electrode foil, by changing the technique of hair engaging aperture and reaming stage, realizes
Aperture is big, high capacity etched foil corrosion preparation.
The present invention is achieved by the following technical solutions:
A kind of preparation method of hydrochloric acid reaming high-field electrode foil, includes the following steps:
Step 1)Pre-treatment and one-stage water wash:Aluminium foil is taken to be placed in impregnation in level-one corrosion overflowing liquid, it will treated aluminium foil
It is washed;
Step 2)Level-one corrosion is washed with second level:It will be through step 1)Treated, and aluminium foil is placed in the mixed solution of sulfuric acid and hydrochloric acid
In, electrolytic etching is carried out, the aluminium foil after electrolysis is washed;
Step 3)Hydrochloric acid pure chemistry reaming:It will be through step 2)Treated, and aluminium foil corrodes in overflowing liquid at dipping in secondary chambering
Reason;
Step 4)Secondary chambering corrosion is washed with three-level:It will be through step 3)Treated, and aluminium foil is placed in containing additive and hydrochloric acid
In mixed solution, electrolytic etching is carried out, the aluminium foil after electrolysis is washed;
Step 5)Three-level reaming corrosion and level Four are washed:It will be through step 4)Treated, and aluminium foil is placed in containing additive and hydrochloric acid
In mixed solution, electrolytic etching is carried out, the aluminium foil after electrolysis is washed;
Step 6)Post-processing is washed with Pyatyi:It will be through step 5)Treated, and aluminium foil is placed in sulfuric acid solution handles, then washing,
Drying, obtains the hydrochloric acid reaming high-field electrode foil.
Further, the washing temperature is room temperature;The one-stage water wash time is 1 ~ 2 min, using tap water;It is described
Second level, three-level and level Four washing time are 1 ~ 3 min, using tap water;The Pyatyi washing time is 4 ~ 6 min, is used
Deionized water.
Further, the level-one corrosion process is as follows:At 60 ~ 80 DEG C, apply 200 ~ 400 mA/cm2Direct current
Electricity, 50 ~ 85 s of electrolytic etching.
Further, the second level and three-level reaming corrosion process are as follows:At 60 ~ 90 DEG C, apply 25 ~ 55 mA/cm2
Direct current, 4 ~ 6 min of electrolytic etching.
Further, step 2)Sulfuric acid concentration is 20 ~ 40 % in the mixed solution, and concentration of hydrochloric acid is 2 ~ 8 %.
Further, the additive is the polystyrene type anion active agent of molecular weight 20000 ~ 100000.
Further, step 4)In the mixed solution concentration of additive be 0.01 ~ 0.5 mL/L, concentration of hydrochloric acid be 2 ~
10 %;Step 5)The concentration of additive is 0.01 ~ 0.5 mL/L in the mixed solution, and concentration of hydrochloric acid is 3 ~ 10 %.
Further, the purity of the aluminium foil is 99.99 %
Beneficial effects of the present invention are as follows:
(1)Pure chemistry reaming is used before secondary chambering corrosion, the Al that level-one corrosion can be made to generate3+、Cl-、SO4 2-、H+、
OH-Plasma is migrated out out of hole, eliminates SO4 2-Factor is paid no attention to reaming, is conducive to the increasing in hole when secondary chambering corrosion
Greatly.But temperature will control properly, temperature is low, and ion quantity of moving out is few in hole, is unfavorable for forming macropore, temperature is excessively high then
Aluminium foil, which is partly dissolved, to be kept foil gradually thinning and cannot generate any effect.
(2)The application electric current corroded with three-level reaming, time, temperature, concentration etc. can be corroded by adjusting secondary chambering
Ratio obtains different passes, to adapt to the preparation of Waste Acid From Hua Cheng Foil under different voltages, makes product system diversification.
(3)It cuts that foil amount is big, cuts 2 ~ 3 times that foil amount is equivalent to nitric acid process, reduce etched foil thickness, manufactured electricity can be made
Container miniaturization.
(4)Hair engaging aperture is uniform, pore size is consistent, and the light foil region of not formed hole is few even without can enhance corrosion
The flexibility of foil, conducive to the production and winding hacking of Waste Acid From Hua Cheng Foil.
(5)Hydrochloric acid replaces nitric acid, reduces purchase cost(Nitric acid unit price is about 10 times of hydrochloric acid currently on the market), realize
The discharge of ammonia nitrogen no pollution, reduces the pollution to water body.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of embodiment 1 ~ 3;
Fig. 2 is the electron microscope scanning figure on electrode foil surface prepared by embodiment 2;
Fig. 3 is the electron microscope scanning figure on electrode foil surface prepared by comparative example 1;
Fig. 4 is the electron microscope scanning figure on electrode foil surface prepared by comparative example 2.
Specific embodiment
The present invention is further elaborated with embodiment with reference to the accompanying drawing.
Embodiment 1
The preparation method flow chart of the present embodiment is as shown in Figure 1.
(1)Pre-treatment and one-stage water wash:The aluminium foil for taking 99.99 % of purity corrodes overflowing liquid in 50 DEG C of level-ones(This one
Grade corrodes overflowing liquid(2)The liquid of middle level-one corrosion is used further to after the mode of overflow recycles(1)In, overflow is in the industry
It allows the wastes secondary use such as spent acid, waste water, is save the cost and a kind of most commonly used mode, if level-one corrosion not yet starts,
Also it can be directly used(2)In corrosive liquid, similarly hereinafter)3 min of middle dipping, the aluminium foil after pre-treatment is washed(Originally
Water), washing temperature is room temperature, 2 min of washing time;
(2)Level-one corrosion is washed with second level:Aluminium foil after washing is placed in the sulfuric acid of 40 % and the hydrochloric acid mixed solution of 8 %,
At a temperature of 60 DEG C, apply 200 mA/cm2Direct current, 85 s of electrolytic etching;Aluminium foil after level-one is corroded is washed(From
Water), washing temperature is room temperature, 2 min of washing time;
(3)Hydrochloric acid pure chemistry reaming:Aluminium foil after second level is washed corrodes overflowing liquid in 40 DEG C of secondary chambering(Concept is same as above
It is described, if secondary chambering corrosion not yet starts, also can be directly used(4)In corrosive liquid, similarly hereinafter)3 min of middle dipping;
(4)Secondary chambering corrosion is washed with three-level:Aluminium foil after hydrochloric acid pure chemistry reaming is placed in containing 0.01 mL/L additive
(The additive uses the polystyrene type anion active agent of molecular weight 20000 ~ 100000, similarly hereinafter)It is molten with the hydrochloric acid of 2 %
In liquid, at 90 DEG C, apply 55 mA/cm2Direct current, 4 min of electrolytic etching, aluminium foil after secondary chambering is corroded carries out
Washing(Tap water), washing temperature is room temperature, 2 min of washing time;
(5)Three-level reaming corrosion and level Four are washed:Aluminium foil after three-level is washed is placed in containing 0.5 mL/L additive and 10 %
Hydrochloric acid solution in, at 60 DEG C, apply 25 mA/cm2Direct current, 6 min of electrolytic etching, by three-level reaming corrosion after
Aluminium foil is washed(Tap water), washing temperature is room temperature, 2 min of washing time;
(6)Post-processing:Aluminium foil after level Four is washed is placed in the sulfuric acid solution of 5 %, and temperature is 70 DEG C, and the processing time is 1
min;
(7)Pyatyi washing:Aluminium foil after post treatment is washed(Deionized water), washing temperature is room temperature, washing time 4
~6 min;
(8)It is dried:Aluminium foil after Pyatyi is washed carries out 2 min drying and processings at 180 DEG C.
Embodiment 2
The preparation method flow chart of the present embodiment is as shown in Figure 1.
(1)Pre-treatment and one-stage water wash:The aluminium foil for taking 99.99 % of purity impregnates in 90 DEG C of level-one corrosion overflowing liquid
1 min washes the aluminium foil after pre-treatment(Tap water), washing temperature is room temperature, 2 min of washing time;
(2)Level-one corrosion is washed with second level:Aluminium foil after washing is placed in the sulfuric acid of 20 % and the hydrochloric acid mixed solution of 2 %,
At a temperature of 80 DEG C, apply 400 mA/cm2Direct current, 50 s of electrolytic etching;Aluminium foil after level-one is corroded is washed(From
Water), washing temperature is room temperature, 2 min of washing time;
(3)Hydrochloric acid pure chemistry reaming:Aluminium foil after second level is washed impregnates 1 in 70 DEG C of secondary chambering corrosion overflowing liquid
min;
(4)Secondary chambering corrosion is washed with three-level:Aluminium foil after hydrochloric acid pure chemistry reaming is placed in containing 0.5 mL/L additive
In the hydrochloric acid solution of 10 %, at 60 DEG C, apply 25 mA/cm2Direct current, 6 min of electrolytic etching, by secondary chambering corruption
Aluminium foil after erosion is washed(Tap water), washing temperature is room temperature, 2 min of washing time;
(5)Three-level reaming corrosion and level Four are washed:Aluminium foil after three-level is washed is placed in containing 0.01 mL/L additive and 3 %
Hydrochloric acid solution in, at 90 DEG C, apply 55 mA/cm2Direct current, 4 min of electrolytic etching, by three-level reaming corrosion after
Aluminium foil is washed(Tap water), washing temperature is room temperature, 2 min of washing time;
(6)Post-processing:Aluminium foil after level Four is washed is placed in the sulfuric acid solution of 10 %, and temperature is 40 DEG C, and the processing time is 3
min;
(7)Pyatyi washing:Aluminium foil after post treatment is washed(Deionized water), washing temperature is room temperature, washing time 5
min;
(8)It is dried:Aluminium foil after Pyatyi is washed carries out 2 min drying and processings at 180 DEG C.
The electrode foil SEM figure prepared is as shown in Fig. 2, its pore size is more consistent, and 1.8 ~ 2.1 μm, hole distribution is equal
It is even, do not occur the light foil region of not formed hole.
Embodiment 3
The preparation method flow chart of the present embodiment is as shown in Figure 1.
(1)Pre-treatment and one-stage water wash:The aluminium foil for taking 99.99 % of purity impregnates in 70 DEG C of level-one corrosion overflowing liquid
2 min wash the aluminium foil after pre-treatment(Tap water), washing temperature is room temperature, 2 min of washing time;
(2)Level-one corrosion is washed with second level:Aluminium foil after washing is placed in the sulfuric acid of 30 % and the hydrochloric acid mixed solution of 5 %,
At a temperature of 70 DEG C, apply 300 mA/cm2Direct current, 70 s of electrolytic etching;Aluminium foil after level-one is corroded is washed(From
Water), washing temperature is room temperature, 2 min of washing time;
(3)Hydrochloric acid pure chemistry reaming:Aluminium foil after second level is washed impregnates 2 in 55 DEG C of secondary chambering corrosion overflowing liquid
min;
(4)Secondary chambering corrosion is washed with three-level:Aluminium foil after hydrochloric acid pure chemistry reaming is placed in containing 0.3 mL/L additive
In the hydrochloric acid solution of 6 %, at 80 DEG C, apply 40 mA/cm2Direct current, 5 min of electrolytic etching, by secondary chambering corruption
Aluminium foil after erosion is washed(Tap water), washing temperature is room temperature, 2 min of washing time;
(5)Three-level reaming corrosion and level Four are washed:Aluminium foil after three-level is washed is placed in containing 0.3 mL/L additive and 6 %
In hydrochloric acid solution, at 80 DEG C, apply 40 mA/cm2Direct current, 5 min of electrolytic etching, by three-level reaming corrosion after aluminium
Foil is washed(Tap water), washing temperature is room temperature, 2 min of washing time;
(6)Post-processing:Aluminium foil after level Four is washed is placed in the sulfuric acid solution of 8 %, and temperature is 60 DEG C, and the processing time is 2
min;
(7)Pyatyi washing:Aluminium foil after post treatment is washed(Deionized water), washing temperature is room temperature, washing time 5
min;
(8)It is dried:Aluminium foil after Pyatyi is washed carries out 2 min drying and processings at 180 DEG C.
Comparative example 1
(1)Pre-treatment and one-stage water wash:The aluminium foil for taking 99.99 % of purity impregnates 1 in 90 DEG C of level-one corrosion overflowing liquid
Min washes the aluminium foil after pre-treatment(Tap water), washing temperature is room temperature, 2 min of washing time;
(2)Level-one corrosion is washed with second level:Aluminium foil after washing is placed in the sulfuric acid of 40 % and the hydrochloric acid mixed solution of 8 %,
At a temperature of 75 DEG C, apply 250 mA/cm2Direct current, 60 s of electrolytic etching;Aluminium foil after level-one is corroded is washed(From
Water), washing temperature is room temperature, 2 min of washing time;
(3)Secondary chambering corrosion is washed with three-level:Aluminium foil after second level is washed is placed in containing 0.3 mL/L additive and 6 %
In hydrochloric acid solution, at 85 DEG C, apply 50 mA/cm2Direct current, 8 min of electrolytic etching, the aluminium after secondary chambering is corroded
Foil is washed(Tap water), washing temperature is room temperature, 2 min of washing time;
(4)Post-processing:Aluminium foil after three-level is washed is placed in the nitric acid solution of 65 %, and temperature is 25 DEG C, and the processing time is 2
min;
(5)Level Four washing:Aluminium foil after post treatment is washed(Deionized water), washing temperature is room temperature, washing time 2
min;
(6)It is dried:Aluminium foil after Pyatyi is washed carries out 2 min drying and processings at 180 DEG C.
The electrode foil SEM prepared schemes have several places king-sized and hole as shown in figure 3, its pore size is different, and has big
Measure the light foil region of not formed hole.
Comparative example 2
(1)Pre-treatment and one-stage water wash:The aluminium foil for taking 99.99 % of purity impregnates 1 in 90 DEG C of level-one corrosion overflowing liquid
Min washes the aluminium foil after pre-treatment(Tap water), washing temperature is room temperature, 2 min of washing time;
(2)Level-one corrosion is washed with second level:Aluminium foil after washing is placed in the sulfuric acid of 40 % and the hydrochloric acid mixed solution of 8 %,
At a temperature of 75 DEG C, apply 250 mA/cm2Direct current, 60 s of electrolytic etching;Aluminium foil after level-one is corroded is washed(From
Water), washing temperature is room temperature, 2 min of washing time;
(3)Secondary chambering corrosion is washed with three-level:Aluminium foil after second level is washed is placed in containing 0.3 mL/L additive and 10 %
Nitric acid solution in, at 65 DEG C, apply 60 mA/cm2Direct current, 8 min of electrolytic etching, after secondary chambering is corroded
Aluminium foil is washed(Tap water), washing temperature is room temperature, 2 min of washing time;
(4)Post-processing:Aluminium foil after three-level is washed is placed in the nitric acid solution of 65 %, and temperature is 25 DEG C, and the processing time is 2
min;
(5)Level Four washing:Aluminium foil after post treatment is washed(Deionized water), washing temperature is room temperature, washing time 2
min;
(6)It is dried:Aluminium foil after Pyatyi is washed carries out 2 min drying and processings at 180 DEG C.
The electrode foil SEM figure prepared, less than 1.2 μm, there is the light of a large amount of not formed holes as shown in figure 4, its aperture is small
Foil region.
Caustic solution of the present invention and traditional caustic solution comparative test result are as follows:
Comparison it is found that using the method for the present invention manufacture corroding electrode foil, specific volume, intensity, cut foil amount, loss be superior to tradition side
The corroding electrode foil of method manufacture, especially high voltage lower pass is bigger, and specific volume is higher.Simultaneously hydrochloric acid replace nitric acid, reduce buying at
This, realizes ammonia nitrogen zero-emission, avoid discharging it is exceeded after cause Water Eutrophication.
Claims (8)
1. a kind of preparation method of hydrochloric acid reaming high-field electrode foil, which is characterized in that include the following steps:
Step 1)Pre-treatment and one-stage water wash:Aluminium foil is taken to be placed in impregnation in level-one corrosion overflowing liquid, it will treated aluminium foil
It is washed;
Step 2)Level-one corrosion is washed with second level:It will be through step 1)Treated, and aluminium foil is placed in the mixed solution of sulfuric acid and hydrochloric acid
In, electrolytic etching is carried out, the aluminium foil after electrolysis is washed;
Step 3)Hydrochloric acid pure chemistry reaming:It will be through step 2)Treated, and aluminium foil corrodes in overflowing liquid at dipping in secondary chambering
Reason;
Step 4)Secondary chambering corrosion is washed with three-level:It will be through step 3)Treated, and aluminium foil is placed in containing additive and hydrochloric acid
In mixed solution, electrolytic etching is carried out, the aluminium foil after electrolysis is washed;
Step 5)Three-level reaming corrosion and level Four are washed:It will be through step 4)Treated, and aluminium foil is placed in containing additive and hydrochloric acid
In mixed solution, electrolytic etching is carried out, the aluminium foil after electrolysis is washed;
Step 6)Post-processing is washed with Pyatyi:It will be through step 5)Treated, and aluminium foil is placed in sulfuric acid solution handles, then washing,
Drying, obtains the hydrochloric acid reaming high-field electrode foil.
2. a kind of preparation method of hydrochloric acid reaming high-field electrode foil according to claim 1, which is characterized in that the washing
Temperature is room temperature;The one-stage water wash time is 1 ~ 2 min, using tap water;The second level, three-level and level Four washing time are equal
For 1 ~ 3 min, using tap water;The Pyatyi washing time is 4 ~ 6 min, using deionized water.
3. a kind of preparation method of hydrochloric acid reaming high-field electrode foil according to claim 1, which is characterized in that the level-one
Corrosion process is as follows:At 60 ~ 80 DEG C, apply 200 ~ 400 mA/cm2Direct current, 50 ~ 85 s of electrolytic etching.
4. a kind of preparation method of hydrochloric acid reaming high-field electrode foil according to claim 1, which is characterized in that the second level
It is as follows with three-level reaming corrosion process:At 60 ~ 90 DEG C, apply 25 ~ 55 mA/cm2Direct current, 4 ~ 6 min of electrolytic etching.
5. a kind of preparation method of hydrochloric acid reaming high-field electrode foil according to claim 1, which is characterized in that step 2)Institute
Stating sulfuric acid concentration in mixed solution is 20 ~ 40 %, and concentration of hydrochloric acid is 2 ~ 8 %.
6. a kind of preparation method of hydrochloric acid reaming high-field electrode foil according to claim 1, which is characterized in that the addition
Agent is the polystyrene type anion active agent of molecular weight 20000 ~ 100000.
7. a kind of preparation method of hydrochloric acid reaming high-field electrode foil according to claim 1, which is characterized in that step 4)Institute
The concentration for stating additive in mixed solution is 0.01 ~ 0.5 mL/L, and concentration of hydrochloric acid is 2 ~ 10 %;Step 5)In the mixed solution
The concentration of additive is 0.01 ~ 0.5 mL/L, and concentration of hydrochloric acid is 3 ~ 10 %.
8. a kind of preparation method of hydrochloric acid reaming high-field electrode foil according to claim 1, which is characterized in that the aluminium foil
Purity be 99.99 %.
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CN117612868A (en) * | 2024-01-18 | 2024-02-27 | 南通南辉电子材料股份有限公司 | Method for manufacturing medium-pressure corrosion foil |
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