CN103966624B - A kind of method preparing electrochemical electrolysis electrode - Google Patents
A kind of method preparing electrochemical electrolysis electrode Download PDFInfo
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- CN103966624B CN103966624B CN201410178770.5A CN201410178770A CN103966624B CN 103966624 B CN103966624 B CN 103966624B CN 201410178770 A CN201410178770 A CN 201410178770A CN 103966624 B CN103966624 B CN 103966624B
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- metallic foil
- aluminum metallic
- aluminum
- negative electrode
- acid solution
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Abstract
The embodiment of the invention discloses a kind of method preparing electrochemical electrolysis electrode, including: aluminum metallic foil is immersed at the first temperature the immersion very first time in strong acid solution；From strong acid solution, take out aluminum metallic foil, clean with abluent, and be dried；Dried aluminum metallic foil is immersed in deionized water, the second time of water-bath at the second temperature；Aluminum metallic foil after cooling dry water-bath.Method according to embodiments of the present invention, uses the aluminum metallic foil of concentrated sulphuric acid or concentrated nitric acid passivation as negative electrode, on the one hand electrolysis cost will be made to greatly reduce, and the most not reduce the cathode function of electrolysis simultaneously.And it addition, the aluminum negative electrode after Dun Hua is less susceptible to adhere to spot than traditional Pt negative electrode in an experiment.
Description
Technical field
The present invention relates to electrochemical field, especially relate to a kind of method preparing electrochemical electrolysis electrode.
Background technology
Electrochemistry is the science that research chemical energy is mutually changed with electric energy, and this conversion is real by redox reaction
Existing.Electrochemistry is generally used in every field, and the knowledge of different field be intertwined to form alloy electrochemistry,
Multiple branches such as semiconductor electrochemistry, organic semiconductor electrochemistry, spectroelectrochemistry and bio electrochemistry.Electrochemistry is rotten at metal
Lose and find broad application from the different direction such as protection, cell reaction, chemical cell.
Electrochemistry, especially cell reaction have obtained important utilization in scientific research and commercial production.Along with Grims group first
Propose and successfully prepare TiO by anodised method2Since nanotube, electrochemical etching method is preparing nano structural material
Field is widely adopted.During conventional electrochemical anodic oxidation, generally use nanostructured to be prepared metal forming or
Person's sputtering has the backing material of respective metal thin film as anode, uses and makees mixed with acid or alkaline electrolyte mixed solution
For electrolyte, cathode material the most often uses platinum or graphite.
Platinum cathode usually uses high-purity (99.99%) platinized platinum, but owing to Pt electrode is expensive, is electrolysed simultaneously
Cheng Zhonghui has black attachment to produce frequently to be needed with HF acid ultrasonic cleaning.So using Pt negative electrode relatively costly, and need
The attachment dirt of ultrasonic cleaning in time.
When graphite is as negative electrode, although its stable chemical nature and cheap, but owing to graphite-structure is loose porous, cause
Easily infiltrate into electrolyte solution inside it, so not easy cleaning, easily cause reaction after repeatedly using and pollute.Additionally, dredge
The graphite material of pine is difficult to prepare negative electrode that is solid durable and that have multiple appearance structure.
Additionally, currently used electrolysis electrode all uses the plate electrode or columnar electrode that single-ended wire accesses.Due to gold
Belong to and have certain resistance value, so the distribution that electromotive force is on this negative electrode is not approximation isoelectric level, but with accessing conductor spacing
The most remote, electromotive force lands successively.Thus can not higher degree ground approximate simulation experiment required for equipotential face.In anodic oxidation
Cheng Zhong, non-equipotential plane easily causes metallic foil anode oxide etch certain sequencing, causes and reacts on sheet metal
Degree is uneven, causes film quality to decline.
Summary of the invention
An object of the present invention is to provide a kind of method preparing electrochemical electrolysis electrode, and the electrode that it is prepared is on the one hand
Electrolysis cost will be made to greatly reduce, the most do not reduce the cathode function of electrolysis simultaneously.
An object of the present invention is to provide a kind of method preparing electrochemical electrolysis electrode, and its electrode prepared has many
Individual (at least two) is electrically accessed a little, overcomes traditional electrode Potential Distributing uneven and be difficult to the defect of simulation experiment demand.
Technical scheme disclosed by the invention includes:
Provide a kind of method preparing electrochemical electrolysis electrode, it is characterised in that including: by aluminum metallic foil in the first temperature
The lower immersion in strong acid solution of degree is soaked the very first time；From described strong acid solution, take out described aluminum metallic foil, clean with abluent,
And be dried；Dried described aluminum metallic foil is immersed in deionized water, the second time of water-bath at the second temperature；Cool down and do
Described aluminum metallic foil after dry water-bath.
In one embodiment of the present of invention, described strong acid solution is concentrated sulphuric acid.
In one embodiment of the present of invention, the concentration of described concentrated sulphuric acid is 98%, and described first temperature is less than 30 degrees Celsius,
The described very first time is 30 minutes.
In one embodiment of the present of invention, described strong acid solution is concentrated nitric acid.
In one embodiment of the present of invention, the concentration of described concentrated nitric acid is 65%, and described first temperature is less than 10 degrees Celsius,
The described very first time is 30 minutes.
In one embodiment of the present of invention, described second temperature is 100 degrees Celsius, and described second time is 30 minutes.
In one embodiment of the present of invention, it is characterised in that also include: in the position that at least two separates by described aluminum
Metal forming is connected to conduct electricity on wire frame, thus forms what at least two separated between described aluminum metallic foil and described conduction wire frame
Be electrically connected contact.
In one embodiment of the present of invention, described conduction wire frame includes: first annular end；Second annular end；At least two
Connecting portion, described at least two connecting portion connects described first annular end and described second annular end；Wherein said aluminum metallic foil
It is connected on the outer surface of described at least two connecting portion.
In one embodiment of the present of invention, described conduction wire frame includes: the first conductiving metal strip；Wherein said aluminum metallic foil
The position that at least two on described first conductiving metal strip separates is connected to described first conductiving metal strip.
In one embodiment of the present of invention, described conduction wire frame includes: the first conductiving metal strip；Second conductiving metal strip,
Described second conductiving metal strip is connected with each other with described first conductiving metal strip；Wherein said aluminum metallic foil is conducted electricity described first
At least one position on bonding jumper is connected to described first conductiving metal strip, and on described second conductiving metal strip
At least one position is connected on described second conductiving metal strip.
Method according to embodiments of the present invention, use concentrated sulphuric acid or concentrated nitric acid passivation aluminum metallic foil as negative electrode, a side
Face will make electrolysis cost greatly reduce, and the most not reduce the cathode function of electrolysis simultaneously.And it addition, the aluminum negative electrode after Dun Hua exists
Experiment is less susceptible to adhere to spot than traditional Pt negative electrode.
And, method according to embodiments of the present invention, aluminum metallic foil negative electrode has multiple (at least two) and is electrically accessed a little, gram
Take traditional electrode Potential Distributing uneven and be difficult to the defect of simulation experiment demand.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method preparing electrochemical electrolysis electrode of one embodiment of the invention.
Fig. 2 and Fig. 3 is the aluminum metallic foil schematic diagram with the connection of conduction wire frame of one embodiment of the invention.
Fig. 4 is the aluminum metallic foil schematic diagram with the connection of conduction wire frame of another embodiment of the present invention.
Detailed description of the invention
The method preparing electrochemical electrolysis electrode concrete of embodiments of the invention is described in detail below in conjunction with accompanying drawing
Step.
Fig. 1 is the schematic flow sheet of the method preparing electrochemical electrolysis electrode of one embodiment of the invention, below with reference to
Each step of method in this embodiment is described in detail by Fig. 1.
In embodiments of the invention, in step 10, first obtain aluminum metallic foil, then aluminum metallic foil can be immersed strong
Acid solution is passivated process, for example, it is possible to aluminum metallic foil immersed time strong acid solution soaks first at the first temperature
Between.
In embodiments of the invention, the material of aluminum metallic foil and size can set as required.Such as, an embodiment
In, it is possible to use purity is the aluminum metallic foil of 99.99%, a size of 10mm × 10mm × 0.4mm.
In one embodiment of the present of invention, strong acid solution here can be concentrated sulphuric acid, such as concentration be the dense sulfur of 98%
Acid, now, aforesaid first temperature can be less than the temperature of 30 degrees Celsius, and the aforesaid very first time can be 30 minutes.
When aluminum metallic foil is soaked in concentrated sulfuric acid, its surface can occur following approximate reverse to answer:
Aluminium sesquioxide (the Al that reaction generates2O3) in aluminum metallic foil, one layer of passivating film of formation is as barrier layer, in stoping
The aluminium foil of layer continues oxidation.According to embodiments of the invention, when aluminum metallic foil soaks 30 minutes in concentrated sulfuric acid, have best
Passivation effect.
In an alternative embodiment of the invention, strong acid solution here can be concentrated nitric acid, such as concentration be the dense nitre of 65%
Acid, now, aforesaid first temperature can be less than the temperature of 10 degrees Celsius, and the aforesaid very first time can be 30 minutes.
Similar with the situation that aforesaid aluminum metallic foil enters in concentrated sulphuric acid, in aluminum metallic foil immerses concentrated nitric acid situation
Under, aluminum metallic foil surface also can form Al2O3Passivating film as barrier layer, stop the aluminium foil of internal layer to continue oxidation.According to this
Bright embodiment, when aluminum metallic foil soaks 30 minutes in concentrated sulfuric acid, has best passivation effect, because now Al2O3Stop
The thickness of layer reaches maximum.
After Passivation Treatment in step 10 completes, in step 12, can by the aluminum metallic foil after Passivation Treatment from
Strong acid solution is removed, and cleans with abluent, be then dried.
Such as, in an embodiment, take out after aluminum metallic foil from strong acid solution, this aluminum metallic foil can be spent from
Sub-water is cleaned, then dries up with nitrogen or drying baker drying.
Then, at step 14, can this aluminum metallic foil dried be immersed in deionized water, water at the second temperature
Bathed for the second time.
In embodiments of the invention, the second temperature here can be 100 degrees Celsius, i.e. carries out water in the case of boiling water
Bath；Here the second time can be 30 minutes.
In embodiments of the invention, using boiling water bath to process is by the sky of the how empty shape aluminum oxide film membrane structure outside barrier layer
Hole seals.Under boiling water bath heating state, will occur to react as follows:
。
At high temperature heat, hydrone and aluminium sesquioxide generate boehmite(can also be expressed as (), simultaneous reactions afterproduct boehmite and original aluminium sesquioxide phase specific volume expand to 33% ~
100%, so can block the loose structure of original thin film, improve compactness and the decay resistance of aluminum metallic foil.
After water bath processing, in step 16, this aluminum metallic foil after water-bath can be cooled down and be dried.Such as, a reality
Execute in example, can dry up with pure nitrogen gas (purity 99.99%) after aluminum metallic foil natural cooling.
In embodiments of the invention, after the process of abovementioned steps, can be by this aluminum metallic foil at least two
The position separated is connected to (step 18) on conduction wire frame, constitutes the electrolysis electrode for electrochemical electrolysis.Here, this aluminium gold
Belong to and between paper tinsel and this conduction wire frame, form the contact that is electrically connected that at least two separates.
Fig. 2 and Fig. 3 is the aluminum metallic foil schematic diagram with the connection of conduction wire frame of one embodiment of the invention.
As shown in Figures 2 and 3, in the present embodiment, conduction wire frame 3 generally cylindrical shape, including first annular end 31, second
Annular end 32 and at least two connecting portion 33, this at least two connecting portion 33 connects first annular end 31 and the second annular end 32.
Aluminum metallic foil 5 after abovementioned steps processes connect (such as, welding) to the outer surface of this at least two connecting portion 33,
It is electrically connected to each other such that achieve aluminum metallic foil 5 with the position that separates at least two of conduction wire frame 3.Conduction wire frame 3 leads to
Cross wire 1 and external electrical connections.Wire 1 is outside is coated with cabinet 2.
Fig. 4 is the aluminum metallic foil schematic diagram with the connection of conduction wire frame of another embodiment of the present invention.
As shown in Figure 4, in the present embodiment, conduction wire frame can include the first conductiving metal strip 60 and the second conductiving metal strip
61, the second conductiving metal strip 61 is connected with each other with the first conductiving metal strip 60, such as, be connected with each other at junction point 67.Through front
Aluminum metallic foil 5 after stating step process at least one position on the first conductiving metal strip 60 is connected to this first conduction
Bonding jumper 60, such as, is connected to the first conductiving metal strip by the pad of pad 65,62,64 and/or other positions
60；Further, this aluminum metallic foil 5 also at least one position on the second conductiving metal strip 61 is connected to this second conducting metal
Bar 61, such as, is connected to the second conductiving metal strip 61 by the pad of pad 66,62,63 and/or other positions.
In embodiment in Fig. 4, conduction wire frame therein can be simplified.Such as, this conduction wire frame can only include
One conductiving metal strip 60, and through abovementioned steps process after aluminum metallic foil 5 on the first conductiving metal strip 60 at least
Two positions separated are connected to this first conductiving metal strip 60, such as, by pad 65,62,64 and other positions
Pad in any at least two be connected to the first conductiving metal strip 60.
Method according to embodiments of the present invention, employs aluminum (Al) metal forming of concentrated sulphuric acid or concentrated nitric acid passivation as negative electrode
Instead of traditional platinum (Pt) negative electrode.During due to aluminum metallic foil as negative electrode, electrochemical reaction can only obtain electronics and gone back
Former, it is impossible to lose electronics oxidized, and the aluminium sesquioxide that aluminum metallic foil cathode surface produces, it is by the Al element of strong metal
Constituting with the O element of strong oxidizing property, be difficult to anti-raw reduction reaction, the Al substrate of internal layer simultaneously to be corroded and oxidation must be occurred anti-
Should, so aluminum metallic foil negative electrode is not susceptible to the corrosion caused by redox reaction.
Al negative electrode after said process is passivated, is difficult to reaction in electrochemistry experiment.Experimental verification, uses this negative electrode
PrepareNano-tube film is close with the nano-tube film quality using Pt negative electrode, and Al negative electrode does not occur instead simultaneously
Should.
Method according to embodiments of the present invention, use concentrated sulphuric acid or concentrated nitric acid passivation aluminum metallic foil as negative electrode, a side
Face will make electrolysis cost greatly reduce, and the most not reduce the cathode function of electrolysis simultaneously.And it addition, the aluminum negative electrode after Dun Hua exists
Experiment is less susceptible to adhere to spot than traditional Pt negative electrode.
And, method according to embodiments of the present invention, aluminum metallic foil negative electrode has multiple (at least two) and is electrically accessed a little, gram
Take traditional electrode Potential Distributing uneven and be difficult to the defect of simulation experiment demand.
Describe the present invention above by specific embodiment, but the present invention is not limited to the enforcement that these are concrete
Example.It will be understood by those skilled in the art that and the present invention can also be made various amendment, equivalent, change etc., these conversion
Without departing from the spirit of the present invention, all should be within protection scope of the present invention.Additionally, " the reality described in above many places
Execute example " represent different embodiment, naturally it is also possible to it is completely or partially combined in one embodiment.
Claims (4)
1. the method preparing electrochemical electrolysis electrode, it is characterised in that including:
Aluminum metallic foil is immersed at the first temperature the immersion very first time in strong acid solution；
From described strong acid solution, take out described aluminum metallic foil, clean with abluent, and be dried；
Dried described aluminum metallic foil is immersed in deionized water, the second time of water-bath at the second temperature；
Described aluminum metallic foil after cooling dry water-bath；
Be connected to described aluminum metallic foil to conduct electricity on wire frame in the position that at least two separates, thus in described aluminum metallic foil and
The contact that is electrically connected that at least two separates is formed between described conduction wire frame；
Wherein, described conduction wire frame includes:
First annular end；
Second annular end；
At least two connecting portion, described at least two connecting portion connects described first annular end and described second annular end；
Wherein said aluminum metallic foil is connected on the outer surface of described at least two connecting portion.
2. the method for claim 1, it is characterised in that: described strong acid solution is concentrated sulphuric acid.
3. the method for claim 1, it is characterised in that: described strong acid solution is concentrated nitric acid.
4. the method for claim 1, it is characterised in that: described second temperature is 100 degrees Celsius, and described second time is
30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410178770.5A CN103966624B (en) | 2014-04-30 | 2014-04-30 | A kind of method preparing electrochemical electrolysis electrode |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410178770.5A CN103966624B (en) | 2014-04-30 | 2014-04-30 | A kind of method preparing electrochemical electrolysis electrode |
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| Publication Number | Publication Date |
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| CN103966624A CN103966624A (en) | 2014-08-06 |
| CN103966624B true CN103966624B (en) | 2017-01-04 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1860254A (en) * | 2003-10-14 | 2006-11-08 | 日本轻金属株式会社 | Corrosion-resistant aluminum conductive material and process for producing the same |
| CN101425393A (en) * | 2008-07-29 | 2009-05-06 | 东莞市东阳光电容器有限公司 | Cathode foil manufacturing method for aluminum electrolysis capacitor |
| CN201256082Y (en) * | 2008-08-27 | 2009-06-10 | 东莞市东阳光电容器有限公司 | Aluminum electrolysis capacitor |
| JP4308556B2 (en) * | 2002-09-26 | 2009-08-05 | 昭和電工株式会社 | Aluminum material for electrolytic capacitor electrode, method for producing electrolytic capacitor electrode material, and electrolytic capacitor |
-
2014
- 2014-04-30 CN CN201410178770.5A patent/CN103966624B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4308556B2 (en) * | 2002-09-26 | 2009-08-05 | 昭和電工株式会社 | Aluminum material for electrolytic capacitor electrode, method for producing electrolytic capacitor electrode material, and electrolytic capacitor |
| CN1860254A (en) * | 2003-10-14 | 2006-11-08 | 日本轻金属株式会社 | Corrosion-resistant aluminum conductive material and process for producing the same |
| CN101425393A (en) * | 2008-07-29 | 2009-05-06 | 东莞市东阳光电容器有限公司 | Cathode foil manufacturing method for aluminum electrolysis capacitor |
| CN201256082Y (en) * | 2008-08-27 | 2009-06-10 | 东莞市东阳光电容器有限公司 | Aluminum electrolysis capacitor |
Non-Patent Citations (1)
| Title |
|---|
| "铝电解电容器阴极箔的后处理和稳定化处理";邓福祥等;《电子元件与材料》;20000831;第19卷(第4期);正文第1页第1栏第3段 * |
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