CN104499029A - High-conversion-rate formed liquid, formed foil and forming method thereof - Google Patents

High-conversion-rate formed liquid, formed foil and forming method thereof Download PDF

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CN104499029A
CN104499029A CN201410831065.0A CN201410831065A CN104499029A CN 104499029 A CN104499029 A CN 104499029A CN 201410831065 A CN201410831065 A CN 201410831065A CN 104499029 A CN104499029 A CN 104499029A
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forming liquid
cent
water
raw material
citric acid
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CN104499029B (en
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李铁军
涂长新
蔡斌
韩苏额
沈向前
施忠裕
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SICHUAN RIKE ELECTRONIC Co Ltd
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SICHUAN RIKE ELECTRONIC Co Ltd
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Abstract

The invention belongs to the field of electronic processing, and specifically relates to a high-conversion-rate formed liquid, a formed foil and a forming method thereof. The technical problem to be solved is to provide a formed liquid having high forming efficiency and capable of enhancing electrostatic capacity and flex conversion rate. The formed liquid comprises the following raw materials by weight percent: 0.55% to 0.85% of ammonium pentaborate, 0.005% to 0.025% of azelaic acid, 0.01% to 0.04% of citric acid and the balance of water. The formed liquid and a formed foil product prepared by the forming method have enhanced electrostatic capacity conversion rate and flex conversion rate, so that the volume of a capacitor can be shortened under the same production capacity condition, and thus the heat released by the capacitor in work is reduced, the power consumption is reduced, and the occupied space of an electric appliance can be reduced. According to the high-conversion-rate formed liquid, the formed foil and the forming method thereof provided by the invention, the technical scheme is simple and easy to implement, the field process flow is convenient to improve, the feasibility is strong, the application prospect is wide, and a brand-new choice is provided for the public.

Description

The forming liquid of high conversion, Waste Acid From Hua Cheng Foil and chemical synthesizing method thereof
Technical field
The invention belongs to electronics manufacture field, be specifically related to a kind of forming liquid of high conversion, Waste Acid From Hua Cheng Foil and chemical synthesizing method thereof.
Background technology
Waste Acid From Hua Cheng Foil is mainly used in aluminium electrolutic capacitor.Formation process is as non-conductive medium at the oxide film of rafifinal Surface Creation one deck densification.Formation process generally comprises following steps: A) level Four changes into or Pyatyi changes into, B) thermal treatment, C) phosphoric acid process, D) after change into, E) aftertreatment, level Four changes into and comprises that the first step changes into, the second stage changes into, the third stage changes into, the fourth stage changes into, Pyatyi changes into except above-mentioned level Four changes into, and also comprises level V and changes into.Aluminium and forming liquid is realized under the electric field at its Surface Creation di-aluminium trioxide film by above-mentioned processing step.
Forming liquid is generally the mixing solutions of boric acid aqueous solution, ammonium adipate, aqueous citric acid solution or above-mentioned medicine.Often add ammoniacal liquor as forming liquid using boric acid in existing method, gained finished product electrostatic capacity low conversion rate, illustrates for the product of 560VF, is about 95 ~ 100%, and it is also on the low side that warpage transforms multiplying power, is only 1.5 ~ 2 times.
The present invention overcomes above defect for providing a kind of brand-new forming liquid, realizes formation efficiency high, strengthens the object of electrostatic capacity and warpage transformation efficiency.
Summary of the invention
It is high that technical problem solved by the invention is to provide a kind of formation efficiency, can strengthen the forming liquid of electrostatic capacity and warpage transformation efficiency.
For solving the problems of the technologies described above, forming liquid of the present invention comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.025%, citric acid 0.01% ~ 0.04%, and all the other are water.
Concrete, adopt above-mentioned forming liquid to be applied in the third stage when changing into, forming liquid comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.010% ~ 0.025%, citric acid 0.025% ~ 0.040%, and all the other are water.
Adopt above-mentioned forming liquid to be applied in the fourth stage when changing into, forming liquid comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, and all the other are water.
For improving formation effect, electrostatic capacity transformation efficiency is greater than 105%, and warpage transforms multiplying power and is greater than 2.45 times.
The third stage changes into forming liquid used, preferably includes the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.01% ~ 0.025%, citric acid 0.030% ~ 0.040%, and all the other are water.
The fourth stage changes into forming liquid used, preferably includes the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.015% ~ 0.020%, citric acid 0.010% ~ 0.025%, and all the other are water.
For improving formation effect further, electrostatic capacity transformation efficiency can reach 106.9%, and warpage transforms multiplying power can reach 2.47 times.
The third stage changes into forming liquid used, most preferably comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.020%, citric acid 0.035%, and all the other are water.
The fourth stage changes into forming liquid used, most preferably comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.015%, citric acid 0.020%, and all the other are water.
Adopt above-mentioned forming liquid to be applied in level V when changing into, can adopt and change into identical forming liquid with the fourth stage.Forming liquid comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, and all the other are water.
The forming liquid that level V changes into, preferably includes the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.015% ~ 0.020%, citric acid 0.010% ~ 0.025%, and all the other are water.
The forming liquid that level V changes into, most preferably comprises the raw material of following weight per-cent: ammonium pentaborate 0.55 ~ 0.85%, nonane diacid 0.015%, citric acid 0.020%, and all the other are water.
Second technical problem solved by the invention is to provide and adopts forming liquid of the present invention to be applied to the chemical synthesizing method preparing Waste Acid From Hua Cheng Foil, and chemical synthesizing method of the present invention comprises the following steps: A) multistagely to change into; B) thermal treatment; C) phosphoric acid process; D) change into after; E) aftertreatment.
Wherein, steps A) multipolarity becomes level Four and to change into or Pyatyi changes into.
Steps A) when adopting level Four to change into:
The third stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.010% ~ 0.025%, citric acid 0.025% ~ 0.040%, and all the other are water.
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, and all the other are water.
Step B) thermal treatment, C) phosphoric acid process, D) after change into, E) aftertreatment adopt ordinary method.
Steps A) when adopting Pyatyi to change into, the third stage changes into and changes into forming liquid used with the fourth stage and change into level Four, level V changes into forming liquid used, comprise the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, all the other are water.
For improving formation effect, shorten hydration time, in technique scheme, steps A) in the first step change into forming liquid used, comprise the raw material of following weight per-cent: ammonium adipate 0.25% ~ 0.45%, citric acid 0.15% ~ 0.30%, reductive agent 0.002% ~ 0.004%, all the other are water; Or be ammonium adipate 0.25% ~ 0.45%, citric acid 0.15% ~ 0.30%, maleic acid 0.002% ~ 0.004%, reductive agent 0.002% ~ 0.004%, all the other are water; Wherein, described reductive agent is at least one in ortho phosphorous acid, inferior sodium phosphate, ortho phosphorous acid potassium, ammonium hypophosphite.
For improving formation effect, shorten hydration time, in technique scheme, steps A) in the second stage change into forming liquid used, comprise the raw material of following weight per-cent: ammonium adipate 0.12% ~ 0.20%, citric acid 0.10% ~ 0.20%, reductive agent 0.001 ~ 0.002%, all the other are water; Or be ammonium adipate 0.12% ~ 0.20%, citric acid 0.10% ~ 0.20%, maleic acid 0.001 ~ 0.003%, reductive agent 0.001 ~ 0.002%, all the other are water; Wherein, described reductive agent is at least one in ortho phosphorous acid, inferior sodium phosphate, ortho phosphorous acid potassium, ammonium hypophosphite.
In technique scheme, step C) described phosphoric acid process adopts routine to change into phosphoric acid process liquid, as employing by weight percentage, the aqueous solution of phosphoric acid 5.0-8.0%.
In technique scheme, step D) described after change into forming liquid used and can adopt conventional forming liquid, as comprised the raw material of following weight per-cent: boronic acid containing 5.0%-8.0%, the aqueous solution of ammonium pentaborate 0.25%-0.45%.
In technique scheme, step e) described aftertreatment solution adopts conventional post-treatment solution, as adopted by weight percentage, the aqueous solution of phosphoric acid ammonium dihydrogen 0.30-0.50%.
In technique scheme, change into temperature, pressure, voltage, the time etc. of chemical synthesizing method of the present invention all adopt existing routine to change into parameter.
Chemical synthesizing method of the present invention is applicable to the production of different size Waste Acid From Hua Cheng Foil between 180 ~ 730VF, without the need to adjusting composition and the concentration of forming liquid, but is controlled by the input voltage of increase and decrease groove end at different levels.
3rd technical problem solved by the invention is to provide the Waste Acid From Hua Cheng Foil being prepared gained by above-mentioned chemical synthesizing method, has the advantage of Fabrication of High Specific Capacitance, high warpage.The aluminium electrolutic capacitor that the Waste Acid From Hua Cheng Foil adopting aforesaid method to prepare gained is made has good performance.
Beneficial effect of the present invention is as follows:
The present invention adopts ammonium pentaborate, nonane diacid, citric acid to make forming liquid, changes into and the fourth stage changes into for the third stage, can improve the electrostatic capacity transformation efficiency of gained Waste Acid From Hua Cheng Foil, tortuously transform multiplying power.Change into product for 560VF, prior art products obtained therefrom electrostatic capacity transformation efficiency is 95-100%, warpage transform multiplying power be 1.5-2 doubly; Adopt the static capacity transformation efficiency of products obtained therefrom of the present invention to be 102.5-107.0%, it is 2.35-2.70 times that warpage transforms multiplying power, and static capacity transformation efficiency and warpage transform multiplying power and significantly improve.Forming liquid provided by the invention and matching used chemical synthesizing method are that the public provides a kind of selection completely newly.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but it should be understood that and protection scope of the present invention be not limited in this embodiment.
With the production instance of 560VF product, explanation is further explained to the present invention below.
Embodiment 1
Aluminium foil is carried out A successively) first step changes into, the second stage changes into, the third stage changes into, the fourth stage changes into; B) phosphoric acid process; C) thermal treatment; D) change into after; E) aftertreatment; Process parameters such as temperature, pressure, time, voltage etc. all adopt the parameter of conventional chemical synthesizing method; Wherein:
The first step changes into the raw material that forming liquid used comprises following weight per-cent: ammonium adipate 0.35%, citric acid 0.20%, maleic acid 0.003%, inferior sodium phosphate 0.003%, and all the other are water;
The second stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium adipate 0.18%, citric acid _ 0.15%, maleic acid 0.002%, inferior sodium phosphate 0.002%, and all the other are water;
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.005%; Citric acid 0.025%, all the other are water;
B) phosphoric acid process solution used by weight percentage, the aqueous solution of phosphoric acid 5.0-8.0%;
D) forming liquid used is changed into after by weight percentage, boronic acid containing 5.0-8.0%, the aqueous solution of ammonium pentaborate 0.25-0.45%;
E) aftertreatment with solution by weight percentage, the aqueous solution of phosphoric acid ammonium dihydrogen 0.30-0.50%.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 102.80%, and it is 2.67 times that warpage transforms multiplying power.
Embodiment 2
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.005%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 102.50%, and it is 2.59 times that warpage transforms multiplying power.
Embodiment 3
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.005%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 103.20%, and it is 2.55 times that warpage transforms multiplying power.
Embodiment 4
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.025%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.005%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 103.50%, and it is 2.53 times that warpage transforms multiplying power.
Embodiment 5
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 102.90%, and it is 2.63 times that warpage transforms multiplying power.
Embodiment 6
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 103.20%, and it is 2.59 times that warpage transforms multiplying power.
Embodiment 7
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 103.50%, and it is 2.57 times that warpage transforms multiplying power.
Embodiment 8
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.025%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%; Citric acid 0.025%, all the other are water.Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 103.10%, and it is 2.61 times that warpage transforms multiplying power.
Embodiment 9
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%, citric acid 0.030%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.20%, and it is 2.55 times that warpage transforms multiplying power.
Embodiment 10
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.20%, and it is 2.52 times that warpage transforms multiplying power.
Embodiment 11
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.90%, and it is 2.47 times that warpage transforms multiplying power.
Embodiment 12
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.025%, citric acid 0.030%, and all the other are water
; The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.80%, and it is 2.45 times that warpage transforms multiplying power.
Embodiment 13
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.010%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.40%, and it is 2.51 times that warpage transforms multiplying power.
Embodiment 14
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.50%, and it is 2.47 times that warpage transforms multiplying power.
Embodiment 15
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.20%, and it is 2.45 times that warpage transforms multiplying power.
Embodiment 16
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.025%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.70%, and it is 2.37 times that warpage transforms multiplying power.
Embodiment 17
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.025%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.010%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 104.50%, and it is 2.55 times that warpage transforms multiplying power.
Embodiment 18
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.010%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 104.90%, and it is 2.50 times that warpage transforms multiplying power.
Embodiment 19
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.035%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.010%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.80%, and it is 2.47 times that warpage transforms multiplying power.
Embodiment 20
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.040%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.010%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.70%, and it is 2.45 times that warpage transforms multiplying power.
Embodiment 21
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.025%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.015%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.90%, and it is 2.53 times that warpage transforms multiplying power.
Embodiment 22
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.015%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.20%, and it is 2.49 times that warpage transforms multiplying power.
Embodiment 23
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.035%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.015%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.40%, and it is 2.46 times that warpage transforms multiplying power.
Embodiment 24
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.040%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.015%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.10%, and it is 2.46 times that warpage transforms multiplying power.
Embodiment 25
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.025%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.020%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.30%, and it is 2.54 times that warpage transforms multiplying power.
Embodiment 26
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.020%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.50%, and it is 2.51 times that warpage transforms multiplying power.
Embodiment 27
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.035%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.020%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.90%, and it is 2.47 times that warpage transforms multiplying power.
Embodiment 28
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.040%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.020%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 106.50%, and it is 2.47 times that warpage transforms multiplying power.
Embodiment 29
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.025%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.90%, and it is 2.45 times that warpage transforms multiplying power.
Embodiment 30
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.030%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.60%, and it is 2.42 times that warpage transforms multiplying power.
Embodiment 31
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.035%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.80%, and it is 2.40 times that warpage transforms multiplying power.
Embodiment 32
Chemical synthesizing method is identical with embodiment 1 method, and difference is that the third stage changes into and changes into forming liquid used with the fourth stage:
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.020%, citric acid 0.040%, and all the other are water;
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium pentaborate 0.65%, nonane diacid 0.015%; Citric acid 0.025%, all the other are water.
Gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency is 105.20%, and it is 2.37 times that warpage transforms multiplying power.
Table 1 embodiment 1-32 prepares the performance perameter of gained Waste Acid From Hua Cheng Foil
Embodiment is numbered Electrostatic capacity transformation efficiency Warpage transforms multiplying power
Embodiment 1 102.80% 2.67 doubly
Embodiment 2 102.50% 2.59 doubly
Embodiment 3 103.20% 2.55 doubly
Embodiment 4 103.50% 2.53 doubly
Embodiment 5 102.90% 2.63 doubly
Embodiment 6 103.20% 2.59 doubly
Embodiment 7 103.50% 2.57 doubly
Embodiment 8 103.10% 2.61 doubly
Embodiment 9 105.20% 2.55 doubly
Embodiment 10 105.20% 2.52 doubly
Embodiment 11 105.90% 2.47 doubly
Embodiment 12 105.80% 2.45 doubly
Embodiment 13 105.40% 2.51 doubly
Embodiment 14 105.50% 2.47 doubly
Embodiment 15 105.20% 2.45 doubly
Embodiment 16 105.70% 2.37 doubly
Embodiment 17 104.50% 2.55 doubly
Embodiment 18 104.90% 2.50 doubly
Embodiment 19 106.80% 2.47 doubly
Embodiment 20 106.70% 2.45 doubly
Embodiment 21 105.90% 2.53 doubly
Embodiment 22 106.20% 2.49 doubly
Embodiment 23 106.40% 2.46 doubly
Embodiment 24 106.10% 2.46 doubly
Embodiment 25 106.30% 2.54 doubly
Embodiment 26 106.50% 2.51 doubly
Embodiment 27 106.90% 2.47 doubly
Embodiment 28 106.50% 2.47 doubly
Embodiment 29 105.90% 2.45 doubly
Embodiment 30 105.60% 2.42 doubly
Embodiment 31 105.80% 2.40 doubly
Embodiment 32 105.20% 2.37 doubly
Analyze can obtain according to embodiment 1-32: in third stage forming liquid, nonane diacid content controls 0.01% ~ 0.025%, citric acid content controls 0.030% ~ 0.040%, in level Four forming liquid, nonane diacid content controls 0.015% ~ 0.020%, citric acid content controls 0.010% ~ 0.025%, the parameter changing into out is ideal: the electrostatic capacity transformation efficiency of 560VF product is greater than 105%, and warpage transforms multiplying power and is greater than 2.45 times.
When in third stage forming liquid, nonane diacid content controls 0.020%, citric acid content controls 0.035%, in level Four forming liquid, nonane diacid content controls 0.015%, citric acid content controls 0.020%, the parameter changing into out is ideal: the electrostatic capacity transformation efficiency of 560VF product can reach 106.9%, and warpage transforms multiplying power can reach 2.47 times.
Following examples investigate the first step to change into the impact of the forming liquid in changing into the second stage on chemical synthesizing method.
Embodiment 33
Chemical synthesizing method is identical with embodiment 1 method, and difference is that level Four changes into forming liquid used:
The first step changes into the raw material that forming liquid used comprises following weight per-cent: boric acid 2.5%, ammoniacal liquor 0.35%, inferior sodium phosphate 0.003%, and all the other are water.
The second stage changes into the raw material that forming liquid used comprises following weight per-cent: boric acid 2.5%, ammoniacal liquor 0.25%, inferior sodium phosphate 0.002%, and all the other are water.
The third stage changes into the raw material that forming liquid used comprises following weight per-cent: boric acid 6.5%, ammonium pentaborate 0.35%, and all the other are water.
The fourth stage changes into the raw material that forming liquid used comprises following weight per-cent: boric acid 6.5%, ammonium pentaborate 0.35 ~ 0.45%, and all the other are water.
Embodiment 34
Chemical synthesizing method is identical with embodiment 19 method, and difference is that the first step changes into and changes into forming liquid used with the second stage:
The first step changes into the raw material that forming liquid used comprises following weight per-cent: boric acid 2.5%, ammoniacal liquor 0.35%, inferior sodium phosphate 0.003%, and all the other are water.
The second stage changes into the raw material that forming liquid used comprises following weight per-cent: boric acid 2.5%, ammoniacal liquor 0.25%, inferior sodium phosphate 0.002%, and all the other are water.
Embodiment 35
Chemical synthesizing method is identical with embodiment 19 method, and difference is that the first step changes into and changes into forming liquid used with the second stage:
The first step changes into the raw material that forming liquid used comprises following weight per-cent: ammonium adipate 0.35%, citric acid 0.20%, inferior sodium phosphate 0.003%, and all the other are water.
The second stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium adipate 0.18%, citric acid _ 0.15%, inferior sodium phosphate 0.002%, and all the other are water.
Embodiment 36
Chemical synthesizing method is identical with embodiment 19 method, and difference is that the first step changes into and changes into forming liquid used with the second stage:
The first step changes into the raw material that forming liquid used comprises following weight per-cent: ammonium adipate 0.35%, citric acid 0.20%, maleic acid 0.003%, inferior sodium phosphate 0.003%, and all the other are water.
The second stage changes into the raw material that forming liquid used comprises following weight per-cent: ammonium adipate 0.18%, citric acid _ 0.15%, maleic acid 0.002%, inferior sodium phosphate 0.002%, and all the other are water.
Table 2
From embodiment 33-36, embodiment 34,35,36 adopts the condition being different from the conventional forming liquid of embodiment 33, the Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiency obtained and warpage transform multiplying power and can significantly improve, and the hydration time of embodiment 35,36 comparatively embodiment 33 obviously shorten, shorten 9s and 26s respectively.It is suitable that embodiment 34 .35,36 gained Waste Acid From Hua Cheng Foil electrostatic capacity transformation efficiencys and warpage transform multiplying power, but embodiment 36 hydration time obviously shortens, adopt maleic acid to be applied to the first step as can be seen here to change into when changing into the second stage and significantly can shorten hydration time, and multiplying power is transformed almost without impact to electrostatic capacity transformation efficiency and warpage.
Following examples are Waste Acid From Hua Cheng Foil impacts on product performance that investigation forming liquid of the present invention prepares different size.
Adopt chemical synthesizing method of the present invention to prepare the product of different size respectively, carry out contrast as following table 3 with ordinary method products obtained therefrom.
Wherein, ordinary method preparation condition, see embodiment 33, only adjusts the conditions such as voltage, electric current, reaction times according to specification requirement.The inventive method preparation condition, see embodiment 36, only adjusts the conditions such as voltage, electric current, reaction times according to specification requirement.
Table 3
As can be seen from Table 3, the Waste Acid From Hua Cheng Foil product of different voltage end, adopts the present invention to improve the electrostatic capacity transformation efficiency of gained Waste Acid From Hua Cheng Foil product after chemical synthesizing method and warpage and transforms multiplying power and all improve significantly than the performance perameter of ordinary method gained Waste Acid From Hua Cheng Foil product.
To sum up, adopt the lifting of forming liquid of the present invention and chemical synthesizing method gained Waste Acid From Hua Cheng Foil product electrostatic capacity transformation efficiency to be conducive to improving the capacity of miniaturization aluminium electrolutic capacitor, in the capacitor product of identical capacity, anode and the cathode area of producing electric capacity can be reduced.Warpage transforms the lifting of multiplying power, and electrical condenser can use little capacitor core, as originally used diameter for 2.0mm, can replace after lifting with 1.0mm.By the lifting of above-mentioned two parameters, the volume of electrical condenser under the condition of equivalent production capacity, can be reduced, and then the heat discharged when reducing electrical condenser work, reduce power consumption, and the occupation of land space of electrical equipment can be reduced.Technical solution of the present invention is simple, and site technique workflow reengineering is convenient, and feasibility is strong, and application prospect is wide, for the public provides a kind of selection completely newly.

Claims (10)

1. forming liquid, is characterized in that, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.025%, citric acid 0.01% ~ 0.04%, and all the other are water.
2. forming liquid according to claim 1, is characterized in that, forming liquid is applied in the third stage when changing into, comprise the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.010% ~ 0.025%, citric acid 0.025% ~ 0.040%, all the other are water;
Preferably, forming liquid is applied in the third stage when changing into, and comprise the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.01% ~ 0.025%, citric acid 0.030% ~ 0.040%, all the other are water;
Most preferably, forming liquid is applied in the third stage when changing into, and comprise the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.020%, citric acid 0.035%, all the other are water.
3. forming liquid according to claim 1 and 2, it is characterized in that, forming liquid be applied in the fourth stage change into or level V changes into time, comprise the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, all the other are water;
Preferably, forming liquid be applied in the fourth stage change into or level V changes into time, comprise the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.015% ~ 0.020%, citric acid 0.010% ~ 0.025%, all the other are water;
Most preferably, forming liquid be applied in the fourth stage change into or level V changes into time, comprise the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.015%, citric acid 0.020%, all the other are water.
4. adopt the chemical synthesizing method of the forming liquid described in any one of claim 1-3, comprise the following steps: A) multistagely to change into; B) thermal treatment; C) phosphoric acid process; D) change into after; E) aftertreatment; It is characterized in that:
Wherein, steps A) multipolarity becomes level Four and to change into or Pyatyi changes into;
Steps A) when adopting level Four to change into:
The third stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.010% ~ 0.025%, citric acid 0.025% ~ 0.040%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, and all the other are water;
Steps A) when adopting Pyatyi to change into:
The third stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.010% ~ 0.025%, citric acid 0.025% ~ 0.040%, and all the other are water;
The fourth stage changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, and all the other are water;
Level V changes into forming liquid used, comprises the raw material of following weight per-cent: ammonium pentaborate 0.55% ~ 0.85%, nonane diacid 0.005% ~ 0.020%, citric acid 0.015% ~ 0.025%, and all the other are water.
5. chemical synthesizing method according to claim 4, it is characterized in that: steps A) in the first step change into forming liquid used, comprise the raw material of following weight per-cent: ammonium adipate 0.25% ~ 0.45%, citric acid 0.15% ~ 0.30%, reductive agent 0.002% ~ 0.004%, all the other are water;
Or be ammonium adipate 0.25% ~ 0.45%, citric acid 0.15% ~ 0.30%, maleic acid 0.002% ~ 0.004%, reductive agent 0.002% ~ 0.004%, all the other are water;
Wherein, described reductive agent is at least one in ortho phosphorous acid, inferior sodium phosphate, ortho phosphorous acid potassium, ammonium hypophosphite.
6. chemical synthesizing method according to claim 4, it is characterized in that: steps A) in the second stage change into forming liquid used, comprise the raw material of following weight per-cent: ammonium adipate 0.12% ~ 0.20%, citric acid 0.10% ~ 0.20%, reductive agent 0.001 ~ 0.002%, all the other are water;
Or be ammonium adipate 0.12% ~ 0.20%, citric acid 0.10% ~ 0.20%, maleic acid 0.001 ~ 0.003%, reductive agent 0.001 ~ 0.002%, all the other are water;
Wherein, described reductive agent is at least one in ortho phosphorous acid, inferior sodium phosphate, ortho phosphorous acid potassium, ammonium hypophosphite.
7. chemical synthesizing method according to claim 4, is characterized in that: step C) described phosphoric acid process adopts by weight percentage, the aqueous solution of phosphoric acid 5.0-8.0%.
8. chemical synthesizing method according to claim 4, is characterized in that: step D) described after change into the raw material that forming liquid used comprises following weight per-cent: boronic acid containing 5.0-8.0%, the aqueous solution of ammonium pentaborate 0.25-0.45%.
9. chemical synthesizing method according to claim 4, is characterized in that: step e) described aftertreatment adopts by weight percentage, the aqueous solution of phosphoric acid ammonium dihydrogen 0.30-0.50%.
10. the Waste Acid From Hua Cheng Foil of chemical synthesizing method gained described in any one of claim 4-9;
Preferably, described Waste Acid From Hua Cheng Foil is for the preparation of aluminium electrolutic capacitor.
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CN108441919A (en) * 2018-03-22 2018-08-24 四川日科电子有限公司 The preparation method of full stress-strain acid aluminum electrolysis capacitor anode Waste Acid From Hua Cheng Foil forming liquid
CN110828184A (en) * 2019-11-26 2020-02-21 深圳市柏瑞凯电子科技有限公司 Formation method of solid aluminum capacitor
CN113026073A (en) * 2021-01-05 2021-06-25 南通海星电子股份有限公司 Formation method of extra-high voltage electrode foil
CN117373830A (en) * 2023-11-09 2024-01-09 江苏楷泓新材科技有限责任公司 Method for manufacturing anode foil of aluminum electrolytic capacitor with high dielectric constant composite film

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CN102610390A (en) * 2011-01-20 2012-07-25 严民 Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors

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CN1990914A (en) * 2005-12-30 2007-07-04 新疆众和股份有限公司 Forming technique for reducing voltage rising time of aluminum electrolytic capacitor anode foil
CN102011167A (en) * 2010-09-26 2011-04-13 广西贺州市桂东电子科技有限责任公司 Electron aluminum foil initial section formation liquid additive and adding method thereof
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CN108441919A (en) * 2018-03-22 2018-08-24 四川日科电子有限公司 The preparation method of full stress-strain acid aluminum electrolysis capacitor anode Waste Acid From Hua Cheng Foil forming liquid
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CN110828184B (en) * 2019-11-26 2022-05-10 深圳市柏瑞凯电子科技股份有限公司 Formation method of solid aluminum capacitor
CN113026073A (en) * 2021-01-05 2021-06-25 南通海星电子股份有限公司 Formation method of extra-high voltage electrode foil
CN117373830A (en) * 2023-11-09 2024-01-09 江苏楷泓新材科技有限责任公司 Method for manufacturing anode foil of aluminum electrolytic capacitor with high dielectric constant composite film

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