CN109972183A - The preparation method of deposit cobalt on a kind of anodic oxidation aluminium formwork - Google Patents
The preparation method of deposit cobalt on a kind of anodic oxidation aluminium formwork Download PDFInfo
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- CN109972183A CN109972183A CN201910235622.5A CN201910235622A CN109972183A CN 109972183 A CN109972183 A CN 109972183A CN 201910235622 A CN201910235622 A CN 201910235622A CN 109972183 A CN109972183 A CN 109972183A
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- aluminium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/045—Anodisation of aluminium or alloys based thereon for forming AAO templates
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/12—Anodising more than once, e.g. in different baths
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/20—Electrolytic after-treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention belongs to the method and technology fields of deposit cobalt, and in particular to the preparation method of deposit cobalt on a kind of anodic oxidation aluminium formwork, this method specifically includes the following steps: (1) surface of pure aluminum is cleaned, oil removing, except film process；(2) fine aluminium is put into oxidation solution and carries out a constant pressure anodic oxidation；(3) rinse the aluminium after oxidation, by aluminium be immersed in by phosphoric acid, chromium trioxide, water form except carrying out film process in film liquid；(4) aluminium is taken out, carries out two-step anodization after the completion of cleaning；(5) aluminium after oxidation is put into reaming solution and carries out expanding treatment；(6) by treated, aluminium is put into deposit cobalt in cobalt salt solution.The deposition for the nanometer cobalt that the method for the present invention is prepared reaches maximization, and deposit cobalt is quality, and stability is high.
Description
Technical field
The invention belongs to the method and technology fields of deposit cobalt, and in particular to the system of deposit cobalt on a kind of anodic oxidation aluminium formwork
Preparation Method.
Background technique
With the development of social economy and continuing to bring out for various new technologies, anodic alumina films slowly enter the view of people
It is wild.Compared with other templates, anodic alumina films corrosion resistance, high temperature and pressure, in terms of have it is excellent
Performance, these special design features and its unique functional characteristic make it the master for preparing high-sequential nano material
Want template.
In in the past few decades, people have carried out a large amount of research to the key technology of electrodeposit metals.Mainly include
Oxidized portion and deposition fraction.The anodised aluminium porous structure of high-sequential in order to obtain, people are by controlling and improving certainly
Organizational process has carried out a large amount of research, such as oxidation voltage, oxidation current, electrolyte to the anodic oxidation condition of metallic aluminium
Type, concentration of electrolyte, temperature, pH value, surface preparation etc..
In the electrolytic solution, usually used acid is oxalic acid, sulfuric acid and phosphoric acid, as chromic acid, boric acid etc. are also used to prepare oxygen
Change aluminum alloy pattern plate, but the alumina formwork order prepared is not high.Sulphuric acid anodizing method is low in cost, and wastewater treatment is held
Easily, gained oxidation film transparency is high, and activity is high, is easy to colour, and has excellent corrosion resistance and wearability.Usually comprising
The oxalic acid of 2-3% carries out anodization using the method for logical direct current or alternating current.So obtain film layer usually compared with
Thickness, up to 60 μm.The oxalic acid oxidation film of clear pale yellow color has good light resistance, hardness, wearability and corrosion resistance, these are all
It is better than sulfuric acid film properties.But this method cost is excessively high, power consumption is larger.Therefore, it is straight that industrial oxalic acid, which aoxidizes common method,
Stream superposition electrolysis method.Remove oxalic acid, the anodic oxidation in other organic carboxyl acid solution is more rare, this probably with organic carboxyl acid sheet
The property of body is related.Compared with inorganic acid, the acidity of organic carboxyl acid is relatively low, and most carboxylic acids are insoluble in water.Therefore, although having
There are many machine carboxylic acid type, but are seldom suitable for anode oxidation process.
Summary of the invention
Invention broadly provides a kind of preparation methods of deposit cobalt on anodic oxidation aluminium formwork, to the deposition of nanometer cobalt
Reach maximization, deposit cobalt is quality, and stability is high.Its technical solution is as follows:
The preparation method of deposit cobalt on a kind of anodic oxidation aluminium formwork, comprising the following steps:
(1) surface of pure aluminum cleaned, oil removing, remove film process；
(2) fine aluminium is put into oxidation solution and carries out a constant pressure anodic oxidation；
(3) rinse the aluminium after oxidation, by aluminium be immersed in by phosphoric acid, chromium trioxide, water form except carrying out in film liquid
Go film process；
(4) aluminium is taken out, carries out two-step anodization after the completion of cleaning；
(5) aluminium after oxidation is put into reaming solution and carries out expanding treatment；
(6) by treated, aluminium is put into deposit cobalt in cobalt salt solution.
Preferably, film process is removed to surface of pure aluminum using lye in step (1).
Preferably, oxidation solution described in step (2) is malonic acid, and malonic acid oxidation solution concentration is 1.0-2.0mol/L.
Preferably, oxidization time is 1-4h in step (2), and oxidizing temperature is 10-20 DEG C, oxidation voltage 60-140V.
Preferably, in step (3) every liter except 10-25g chromium trioxide, 10-35ml phosphoric acid is contained in film liquid, surplus is water,
Striping soaking time is 0.5-6h, and temperature is 50-90 DEG C.
Preferably, scavenging period is 5-10min, two-step anodization condition and an anodic oxidation condition in step (4)
It is identical.
Preferably, reaming solution is phosphoric acid solution in step (5), and pore-enlargement is less than 3min.
Preferably, the mixed solution that cobalt salt forms in step (6) for 0.4mol/L boric acid and 0.1-0.5mol/L cobalt acetate,
The sweep speed of deposit cobalt is 0.005-0.02V/S.
Malonic acid is applicable anode oxidation process in a small number of organic carboxyl acids.The growth voltage of its oxidation film is higher,
Can be up to 140V or so, and its unit size is larger, up to 300nm or so, is suitable for electrochemical deposition.
Using the above scheme, the invention has the following advantages that
Deposition step has still maintained the nano-porous structure of AAO film in the method for the present invention, and AAO film is relatively stable and sinks
Oxidation film after product is capable of providing the function of high electronics transfer, and the product of synthesis has higher stability, improves fiber table
Face pattern, it compensates for surface defect, and has certain decorative performance, can satisfy the technical requirements of many applications.
Malonic acid aperture is easy to deposit greatly, and multiple anodizing is used in certain density malonic acid solution, is big
The industrial application of aperture AAO template proposes a feasible approach.
Detailed description of the invention
Fig. 1, Fig. 2 are the deposit cobalt surface electron-microscope scanning figure that under different times mirrors prepared by embodiment 1；
Fig. 3 is the graph of pore diameter distribution of deposit cobalt sample prepared by embodiment 1.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material
Material is conventional biochemical reagent and material unless otherwise required.
Embodiment 1
On the present embodiment anodic oxidation aluminium formwork deposit cobalt the preparation method is as follows:
(1) surface of pure aluminum pretreatment process: fine aluminium material is successively cut out, is cleaned, oil removing, lye is except film process；
(2) by step (1) pretreated fine aluminium be put into configured mass fraction be 1.0mol/L malonic acid solution into
Row anodic oxidation, relevant parameter be time 4h, 10 DEG C of temperature, voltage 140V；
After the fine aluminium decompression of (3) anodizeds removes barrier layer, tap water is rinsed, and is cleaned by ultrasonic 5min,
Be immersed in later except in film liquid, except film liquid is made of phosphoric acid, chromium trioxide, wherein every liter except film liquid chromium trioxide containing 10g,
10mL phosphoric acid, surplus are water, soaking time 5h, and temperature 60 C carries out film process；
(4) after the aluminium flake of step (3) processing takes out, ultrasonic washing with clean water 10min；Fine aluminium after once oxidation carries out two
Secondary anodic oxidation, condition are identical as an anodic oxidation；
(5) by the aluminium after oxidation be put into reaming solution impregnate 1min carry out expanding treatment, with distilled water flushing and
Shady place is protected from light naturally dry；
(6) by the sweep speed of treated aluminium 0.02V/S in cobalt salt solution deposit cobalt.
Embodiment 2
On the present embodiment anodic oxidation aluminium formwork deposit cobalt the preparation method is as follows:
(1) surface of pure aluminum pretreatment process: fine aluminium material is successively cut out, is cleaned, oil removing, lye is except film process；
(2) by step (1) pretreated fine aluminium be put into configured mass fraction be 1.0mol/L malonic acid solution into
Row anodic oxidation, relevant parameter be time 1h, 20 DEG C of temperature, voltage 60V；
After the fine aluminium decompression of (3) anodizeds removes barrier layer, tap water is rinsed, and is cleaned by ultrasonic 5min,
Be immersed in later except in film liquid, except film liquid is made of phosphoric acid, chromium trioxide, wherein every liter except film liquid chromium trioxide containing 25g,
35mL phosphoric acid, surplus are water, and soaking time 6h, 90 DEG C of temperature carry out film process；
(4) after the aluminium flake of step (3) processing takes out, ultrasonic washing with clean water 5min；Fine aluminium after once oxidation carries out two
Secondary anodic oxidation, condition are identical as an anodic oxidation；
(5) by the aluminium after oxidation be put into reaming solution impregnate 1min carry out expanding treatment, with distilled water flushing and
Shady place is protected from light naturally dry；
(6) by the sweep speed of treated aluminium 0.005V/S in cobalt salt solution deposit cobalt.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (8)
1. the preparation method of deposit cobalt on a kind of anodic oxidation aluminium formwork, it is characterised in that: the following steps are included:
(1) surface of pure aluminum cleaned, oil removing, remove film process；
(2) fine aluminium is put into oxidation solution and carries out a constant pressure anodic oxidation；
(3) rinse the aluminium after oxidation, by aluminium be immersed in by phosphoric acid, chromium trioxide, water form except carrying out striping in film liquid
Processing；
(4) aluminium is taken out, carries out two-step anodization after the completion of cleaning；
(5) aluminium after oxidation is put into reaming solution and carries out expanding treatment；
(6) by treated, aluminium is put into deposit cobalt in cobalt salt solution.
2. the preparation method of deposit cobalt on anodic oxidation aluminium formwork according to claim 1, it is characterised in that: step (1)
It is middle that film process is removed to surface of pure aluminum using lye.
3. the preparation method of deposit cobalt on anodic oxidation aluminium formwork according to claim 1, it is characterised in that: step (2)
Described in oxidation solution be malonic acid, malonic acid oxidation solution concentration be 1.0-2.0mol/L.
4. the preparation method of deposit cobalt on anodic oxidation aluminium formwork according to claim 1, it is characterised in that: step (2)
Middle oxidization time is 1-4h, and oxidizing temperature is 10-20 DEG C, oxidation voltage 60-140V.
5. the preparation method of deposit cobalt on anodic oxidation aluminium formwork according to claim 1, it is characterised in that: step (3)
In every liter except 10-25g chromium trioxide, 10-35ml phosphoric acid is contained in film liquid, surplus is water, and striping soaking time is 0.5-6h, temperature
Degree is 50-90 DEG C.
6. the preparation method of deposit cobalt on anodic oxidation aluminium formwork according to claim 1, it is characterised in that: step (4)
Middle scavenging period is 5-10min, and two-step anodization condition is identical as an anodic oxidation condition.
7. the preparation method of deposit cobalt on anodic oxidation aluminium formwork according to claim 1, it is characterised in that: step (5)
Middle reaming solution is phosphoric acid solution, and pore-enlargement is less than 3min.
8. the preparation method of deposit cobalt on anodic oxidation aluminium formwork according to claim 1, it is characterised in that: step (6)
Middle cobalt salt is the mixed solution that 0.4mol/L boric acid and 0.1-0.5mol/L cobalt acetate form, and the sweep speed of deposit cobalt is
0.005-0.02V/S。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139511A (en) * | 2020-01-20 | 2020-05-12 | 烟台大学 | Cobaltosic oxide nanotube array assembled by anodic oxidation method and method |
Citations (4)
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| CN101838835A (en) * | 2010-03-30 | 2010-09-22 | 同济大学 | Ordered porous alumina template capable of being directly applied to electrochemical deposition and preparation method thereof |
| CN103225096A (en) * | 2013-05-17 | 2013-07-31 | 江苏理工学院 | Preparation method of porous anodic aluminum oxide film |
| US20140272280A1 (en) * | 2013-03-18 | 2014-09-18 | Asian Institute Of Technology | Anodized aluminum oxide nanoporous membrane integrated with micro-channel and method of formation thereof |
| CN106115800A (en) * | 2016-06-17 | 2016-11-16 | 南开大学 | A kind of tufted cobalt hydroxide nanometer sheet and preparation method thereof |
-
2019
- 2019-03-27 CN CN201910235622.5A patent/CN109972183A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838835A (en) * | 2010-03-30 | 2010-09-22 | 同济大学 | Ordered porous alumina template capable of being directly applied to electrochemical deposition and preparation method thereof |
| US20140272280A1 (en) * | 2013-03-18 | 2014-09-18 | Asian Institute Of Technology | Anodized aluminum oxide nanoporous membrane integrated with micro-channel and method of formation thereof |
| CN103225096A (en) * | 2013-05-17 | 2013-07-31 | 江苏理工学院 | Preparation method of porous anodic aluminum oxide film |
| CN106115800A (en) * | 2016-06-17 | 2016-11-16 | 南开大学 | A kind of tufted cobalt hydroxide nanometer sheet and preparation method thereof |
Non-Patent Citations (4)
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| F. HEKMAT B等: "Growth of the cobalt nanowires using AC electrochemical deposition on anodized aluminum oxide templates", 《J NANOSTRUCT CHEM》 * |
| SACHIKO ONO等: "Self-ordering of anodic porous alumina formed in organic acid electrolytes", 《ELECTROCHIMICA ACTA 》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139511A (en) * | 2020-01-20 | 2020-05-12 | 烟台大学 | Cobaltosic oxide nanotube array assembled by anodic oxidation method and method |
| CN111139511B (en) * | 2020-01-20 | 2021-06-29 | 烟台大学 | Cobaltosic oxide nanotube array assembled by anodic oxidation method and method |
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