It is a kind of to use seven grades of middle-high voltage electrode foil manufacture methods of different hair engaging aperture conditions
Technical field
It is particularly a kind of using seven grades of mesohigh electrodes of different hair engaging aperture conditions the present invention relates to the manufacture method of electrode foil
Foil making method.
Background technology
Since reform and opening-up, national economy rapid growth, " scientific and technical innovation, autonomous innovation " has turned into current domestic industry hair
The main flow of exhibition, China's electronic industry is developed rapidly, especially the urgency in the machine product such as communication products, computer, household electrical appliances market
Play expands, and the development to aluminum electric pole foil industry has play a part of to add fuel to the flames.Simultaneously because the miniaturization of aluminium electrolutic capacitor, height
Performance-based, chip type requirement it is more and more urgent, the manufacturing industry to electrode foil it is also proposed technology and quality requirement higher.Electricity
Pole paper tinsel is the key raw material of aluminium electrolutic capacitor manufacture, and the quality of electrode foil will directly influence aluminium electrolutic capacitor
Functionality, quality and appealing design is poor.The conventional corrosion technology flow of currently manufactured electrode foil is pre-treatment-washing-Chemical cleaning-washing-pure water
Cleaning-dry, is main corrosive liquid with hydrochloric acid sulfuric acid or nitric acid, using direct current hair engaging aperture for several times, each corrosive liquid and electricity
Stream, temperature all same.Such as existing five-stage manufacturing method:Aluminium foil that first learn from else's experience excessive erosion, that purity is 99.99%, 90~
Impregnated 5~10 minutes in 100 DEG C of pure water, the water-soluble of 0.1~8% citric acid and 0.1~5% citrate is placed in after taking-up
It is then that one-level is melted into 8~15 points under conditions of 20mA/ (cm) 2, voltage is 140V in 70~95 DEG C, current density in liquid
Clock;Aluminium foil after one-level is melted into again is rinsed after taking out with water, then is placed in 0.1~5% azelaic acid and 0.1~5% nonyl two
It is two grades of changes under conditions of 20rriA/ (CIII) 2, voltage is 280V in 70~95 DEG C, current density in the aqueous solution of hydrochlorate
Into 8~15 minutes;Aluminium foil after two grades are melted into is placed in the water of 0.1~5% azelaic acid and 0.1~50/ azelate again
It is that three-level is melted into 8~15 minutes under conditions of 20mA/ (cm) 2, voltage is 450V in 70~95 DEG C, current density in solution;
Aluminium foil after the chemical conversion of special three-level is placed in the aqueous solution of 0.1~5% azelaic acid and 0.1~5% azelate again, 70~
95 DEG C, current density be 20mA/ (cm) 2, voltage be 580V under conditions of, level Four be melted into 8~15 minutes;After level Four is melted into
Aluminium foil is placed in the aqueous solution of 0.1~3% azelaic acid and 0.1~3% azelate again, in 70~95 DEG C, current density
Be 20mA/ (cm) 2, voltage be 620V under conditions of, Pyatyi be melted into 8~15 minutes;Aluminium foil after Pyatyi is melted into is from electrolyte
Taken out in groove, carry out 500 DEG C of high-temperature heat treatment 3~4 minutes;0.1~3% azelaic acid and 0.1~3% nonyl two are placed in again
It is under conditions of 20mA/ (cm) 2, voltage is 620V, to be melted into 8~15 points in 70~95 DEG C, current density in the aqueous solution of hydrochlorate
Clock;Then processed with temperature as 50~80 DEG C in 1~8% phosphoric acid solution;Be placed in again 0.1~3% azelaic acid and
It is then that 20mA/ (cm) 2, voltage is 620V's in 70~95 DEG C, current density in the aqueous solution of 0.1~3% azelate
Under the conditions of, it is melted into 8~15 minutes;Finally take out, dry.The manufacturing process of electrode foil for aluminum electrolytic capacitors is also aluminium foil surface
The process that hole produces and grows, in generation and production process, the length change in aperture and hole can be because of the structure shape in hole itself in hole
State and it is different, and in existing manufacturing technology, hair engaging aperture condition is single, it is impossible to fully meet hole different phase pair in growth course
Required in the difference of etching condition, cause pore size distribution uneven or the problem that hole merges and reduces effective hole number occurs.In order to
This problem is solved, R&D institution and the technical staff of enterprise are explored constantly, research, it is desirable to find out a kind of more advanced
Method manufacture meets the electrode foil of market demands, although makes some progress, but is remained still in practice
The technical barrier not overcome.
The content of the invention
It is an object of the invention to overcome the above not enough, there is provided a kind of using seven grades of mesohigh electrodes of different hair engaging aperture conditions
Foil making method.By changing the concentration of reaming corrosive liquid and the height of temperature, can effective controlling paper tinsel hole generation and production, it is accurate
The really increase of control hole area, reaches production Technology requirement, obtains high-quality middle-high voltage electrode foil, improves production efficiency.
The present invention solves the technical step that is used of its technical problem:Washing-paper tinsel the surface of pre-treatment-once is once straight
Stream hair engaging aperture treatment-paper tinsel surface second direct current hair engaging aperture treatment-paper tinsel surface three times direct current hair engaging aperture treatment-paper tinsel surface four times direct current hair
At the direct current hair engaging aperture treatment-paper tinsel surface seven times direct current hair engaging aperture of the direct current hair engaging aperture treatment-paper tinsel surface six times of hole treatment-paper tinsel surface five times
Reason-secondary washing-paper tinsel surface expanding treatment-tri- time washing-Chemical cleaning-tetra- time washing-pure water is cleaned-dried.
A kind of detailed process using seven grades of middle-high voltage electrode foil manufacture methods of different hair engaging aperture conditions is as follows:
1st step:Pre-treatment:Pre-treatment mixes the solution of 1%~10% hydrochloric acid using 8%~40% sulfuric acid solution,
At 30~70 DEG C, process 1~5 minute;
Second step:The direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% mixed in hydrochloric acid
Liquid, temperature is 50~90 DEG C, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2;
Third step:The treatment of paper tinsel surface second direct current hair engaging aperture:Corrosive liquid is 8~40% sulfuric acid and 1~10% mixed in hydrochloric acid
Liquid, temperature is 50~90 DEG C, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, this step
Sulfuric acid content is the 98% of step 2 sulfuric acid content in rapid, and remaining condition is identical with previous step;
4th step:The three direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% mixed in hydrochloric acid
Liquid, temperature is 50~90 DEG C, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, this step
Sulfuric acid content is 98% of sulfuric acid content in step 3 in rapid, and temperature increases by 0.3 DEG C compared with step 3, and remaining condition is identical with step 3;
5th step:The four direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% mixed in hydrochloric acid
Liquid, temperature is 50~90 DEG C, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, this step
Sulfuric acid content is 96% of sulfuric acid content in step 3 in rapid, and remaining condition is identical with step 3;
6th step:The five direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% mixed in hydrochloric acid
Liquid, temperature is 50~90 DEG C, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, this step
Sulfuric acid content is 96% of sulfuric acid content in step 3 in rapid, and temperature increases by 0.3 DEG C compared with step 3, and remaining condition is identical with step 3;
7th step:The six direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% mixed in hydrochloric acid
Liquid, temperature is 50~90 DEG C, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, this step
Sulfuric acid content is 94% of sulfuric acid content in step 3 in rapid, and remaining condition is identical with step 3;
8th step:The seven direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% mixed in hydrochloric acid
Liquid, temperature is 50~90 DEG C, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, this step
Sulfuric acid content is 94% of sulfuric acid content in step 3 in rapid, and temperature increases by 0.3 DEG C compared with step 3, and remaining condition is identical with step 3;
9th step:Paper tinsel surface expanding treatment:Corrosive liquid is 1~10% nitric acid, and temperature is 50~90 DEG C, process time
At 60 seconds~360 seconds, using direct current, electricity was 30~80C/cm for control2;
10th step:Chemical cleaning:Cleaning fluid is 1~10% nitric acid, and temperature is 30~70 DEG C, 1~5 point of scavenging period
Clock;
11st step:Under above-mentioned washing is normal temperature condition, clean 1~3 minute;
12nd step:Pure water is cleaned:Under normal temperature condition, clean 2~6 minutes;
13rd step:Dry:Under the conditions of 150~350 DEG C, dry 1~5 minute.
Beneficial effects of the present invention:By changing the concentration of reaming corrosive liquid and the height of temperature, can effective controlling paper tinsel hole
Generation and production, the increase of accurate control hole area reaches production Technology requirement, obtains high-quality middle-high voltage electrode foil,
Improve production efficiency.
The technology of the present invention and the electrode foil performance comparison table made by prior art
|
Comparative example |
Embodiment |
Bending (returning) |
60 |
65 |
Specific volume (μ F/cm2) |
0.57(640vf) |
0.59(640vf) |
Embodiment
(1) pre-treatment:Pre-treatment mixes the solution of 1%~10% hydrochloric acid, 30 using 8%~40% sulfuric acid solution
At~70 DEG C, process 1~5 minute;
(2) wash:Under normal temperature condition, clean 1~3 minute;
(3) the direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2;
(4) paper tinsel surface second direct current hair engaging aperture treatment:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is the 98% of step 3 sulfuric acid content, and remaining condition is identical with previous step;
(5) the three direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is 98% of sulfuric acid content in step 3, and temperature increases by 0.3 DEG C compared with step 3, and remaining condition is identical with step 3;
(6) the four direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is 96% of sulfuric acid content in step 3, and remaining condition is identical with step 3;
(7) the five direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is 96% of sulfuric acid content in step 3, and temperature increases by 0.3 DEG C compared with step 3, and remaining condition is identical with step 3;
(8) the six direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is 94% of sulfuric acid content in step 3, and remaining condition is identical with step 3;
(9) the seven direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is 94% of sulfuric acid content in step 3, and temperature increases by 0.3 DEG C compared with step 3, and remaining condition is identical with step 3;
(10) wash:Under normal temperature condition, clean 1~3 minute;
(11) paper tinsel surface expanding treatment:Corrosive liquid is 1~10% nitric acid, and temperature is 50~90 DEG C, process time control
At 60 seconds~360 seconds, using direct current, electricity was 30~80C/cm2;
(12) wash:Under normal temperature condition, clean 1~3 minute;
(13) Chemical cleaning:Cleaning fluid is 1~10% nitric acid, and temperature is 30~70 DEG C, scavenging period 1~5 minute;
(14) wash:Under normal temperature condition, clean 1~3 minute;
(15) pure water cleaning:Under normal temperature condition, clean 2~6 minutes;
(16) dry:Under the conditions of 150~350 DEG C, dry 1~5 minute;
Comparative example
(1) pre-treatment:Pre-treatment mixes the solution of 1%~10% hydrochloric acid, 30 using 8%~40% sulfuric acid solution
At~70 DEG C, process 1~5 minute;
(2) wash:Under normal temperature condition, clean 1~3 minute;
(3) the direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2;
(4) paper tinsel surface second direct current hair engaging aperture treatment:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is the 98% of step 3 sulfuric acid content, and remaining condition is identical with previous step;
(5) the three direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is 98% of sulfuric acid content in step 3, and temperature increases by 0.3 DEG C compared with step 3, and remaining condition is identical with step 3;
(6) the four direct current hair engaging aperture treatment in paper tinsel surface:Corrosive liquid is 8~40% sulfuric acid and 1~10% hydrochloric acid mixed solution, temperature
It is 50~90 DEG C to spend, and process time is controlled at 30 seconds~120 seconds, and using direct current, electricity is 5~15C/cm2, sulphur in this step
Acid content is 96% of sulfuric acid content in step 3, and remaining condition is identical with step 3;
(7) wash:Under normal temperature condition, clean 1~3 minute;
(8) paper tinsel surface expanding treatment:Corrosive liquid is 1~10% nitric acid, and temperature is 50~90 DEG C, and process time control exists
60 seconds~360 seconds, using direct current, electricity was 30~80C/cm2;
(9) wash:Under normal temperature condition, clean 1~3 minute;
(10) Chemical cleaning:Cleaning fluid is 1~10% nitric acid, and temperature is 30~70 DEG C, scavenging period 1~5 minute;
(11) wash:Under normal temperature condition, clean 1~3 minute;
(12) pure water cleaning:Under normal temperature condition, clean 2~6 minutes;
(13) dry:Under the conditions of 150~350 DEG C, dry 1~5 minute;
As shown by data that embodiments of the invention and comparative example draw, by the concentration and temperature that change reaming corrosive liquid
Just, specific volume increases to 0.59 (640vf), and bending (returning) is 65, can effective controlling paper tinsel hole generation and production, accurate control hole
The increase of area, reaches production Technology requirement, obtains high-quality middle-high voltage electrode foil, improves production efficiency.