CN105350052B - A kind of preparation method of aluminium alloy golden yellow conductive oxide film - Google Patents
A kind of preparation method of aluminium alloy golden yellow conductive oxide film Download PDFInfo
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- CN105350052B CN105350052B CN201510843843.2A CN201510843843A CN105350052B CN 105350052 B CN105350052 B CN 105350052B CN 201510843843 A CN201510843843 A CN 201510843843A CN 105350052 B CN105350052 B CN 105350052B
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Abstract
The present invention relates to aluminium alloy electric conductive oxidation technical field of membrane, especially a kind of preparation method of aluminium alloy golden yellow conductive oxide film, pass through gasoline decontamination, sodium hydroxide solution soaks degreasing, rinse, salpeter solution soaks light extraction, rinse, anodic oxidation is carried out again, rinse, dyeing, rinse, dry up packaging and other steps, so that aluminum alloy material surface forms the diaphragm of one layer of compactness, the film forms oxide-film cavity, so that the surface color and polish of the aluminum alloy materials after dyeing processing is uniform, improve the uniformity to aluminum alloy materials dyeing, and its oxide-film into thickness be 0.005 0.008 microns, effectively enhance the corrosion resistance of aluminum alloy materials, it ensure that the electric conductivity of aluminum alloy materials is good to greatest extent, so that its surface contacted resistance is 21.7 22.1m Ω.
Description
Technical field
The present invention relates to aluminium alloy electric conductive oxidation technical field of membrane, especially a kind of aluminium alloy golden yellow conductive oxide film
Preparation method.
Background technology
Aluminium is the active metal of comparison, and its normal potential is -1.706V, corrosion-resistant in atmospheric environment.In aerospace industry
In production, it is the reinforcing effect for needing to add aluminum some minor metallic elements raising aluminum, increases the strong of aluminum
After degree, then as raw material use;But with the hardness increase of aluminum, its decay resistance substantially reduces, and then leads
Cause the service life of aluminum shorter, influence the performance of equipment, cause potential safety hazard.
At present, in order to ensure that aluminum alloy materials have under enough intensity, there is higher corrosion resistance again, then need
Oxidation processes are carried out to aluminum alloy materials.
It is divided into chemical oxidation treatment and electrochemicial oxidation for the oxidation processes of aluminium alloy in the prior art;And for
The aluminum alloy materials applied in aerospace industry are, it is necessary to obtain aluminium alloy conductive protection, that is to say, that so that the film layer after processing is
Have conductivity, again in golden yellow, and color and luster needs uniformity.
But come according to prior art and oxidized aluminum alloy processing producer's technology used and the product produced
See, its be by aluminum alloy surface carry out chemical oxidation treatment after so that the color and luster of film surface is rendered as irised
Film layer;And also there is researcher by using electrochemicial oxidation to aluminum alloy surface, then carried out dyeing processing, but by
Raw material is chosen in handling process and the restriction of parameter is inaccurate, cause the surface effect of alloy product that obtains compared with
Difference, especially color and luster are poor so that need again aluminum alloy material surface be processed into golden yellow conductive film layer difficulty it is larger.
In addition, oxidized aluminum alloy of the prior art, dyeing processing, it is due in oxidized aluminum alloy processing procedure
Handle it is incorrect, cause aluminum alloy surface formed oxide-film thickness it is larger, and then cause aluminum alloy surface resistance compared with
Greatly so that level off to state of insulation, lose aluminium alloy electric conductivity;Moreover, oxide-film of the prior art treats
Cheng Zhong, due to not having the dense porous state for forming uniformity in aluminium alloy protective layer, cause in dyeing course,
It is difficult to form the color of uniformity on surface, and then causes the color that a plurality of color bands are formed in aluminum alloy material surface, drops
Aluminum alloy surface after low dyeing processing it is attractive in appearance.
Based on this, this researcher combines long-term exploration practice and continuously attempted to, and passes through electrochemicial oxidation mode
Use, and to before electrochemicial oxidation, processing in, processing after physical and chemical parameter condition limitation so that the aluminium after processing
Alloy surface reduces the difficulty for the conducting film that golden yellow is prepared into aluminum alloy material surface, is in golden yellow conducting film
Aluminum alloy material surface conductive protection provides a kind of new approaches.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides a kind of aluminium alloy golden yellow conductive oxygen
Change the preparation method of film.
It is achieved particular by following technical scheme:
Gasoline decontamination, sodium hydroxide solution immersion degreasing, rinse, salpeter solution immersion light extraction, rinse, carry out anodic oxygen again
Change, rinse, dyeing, rinse, drying packaging;
It is that the greasy dirt of aluminum alloy surface is purged as cleaning agent using 120# gasoline in journey is treated
After processing;Again by it in the sodium hydroxide solution that mass-volume concentration is 60~65g/l, it is 60- to control sodium hydroxide temperature
After 70 DEG C of processing 0.5-1min, then the clear water of flowing is used to clean up;It is placed on again in salpeter solution and soaks 0.5-1min
Afterwards, cleaned up using the clear water of flowing;Again as anode, and electrolytic oxidation process is carried out, electrolyte is quality volume
Concentration is 180-200g/l sulfuric acid solution, and the temperature of electrolyte is 13-15 DEG C, the current density in electrolytic process for (0.5~
0.8)A/dm2, voltage 13-15V, electrolytic processing time 4-6min;After electrolysis terminates, it is drawn off, using the clear of flowing
Water is rinsed well;Dyeing processing is carried out again, and the temperature of dyeing liquor is 55-60 DEG C, processing time 1-2min, and dyeing is completed
Afterwards, rinsed well using the clear water of flowing, then used compressed air to dry up surface, packed, you can.Compressed air is blown out
The speed come is 1.5-3.7m3/h。
The above-mentioned salpeter solution used is for 1: 1 mixed solution mixed by nitric acid and water according to mass ratio.
Above-mentioned dyeing liquor is the madder that the alizarin yellow for using concentration as 0.25~0.3g/l is 0.1~0.15g/l with concentration
Mixed solution after the red mass mixing according to grade of element;Described dyeing puts the anode aluminium alloy material flitch for being electrolysed completion when handling
Enter immersion treatment in dyeing liquor.
During the electrochemicial oxidation of aluminum alloy materials is carried out, the substantially life of the oxide-film of aluminum alloy surface
Into the process with dissolving, in the moment that is powered, because oxygen and aluminium have very big affinity, quickly formed in aluminum alloy material surface
Alundum (Al2O3) oxide-film;In conjunction with the electrolyte solution used for sulfuric acid solution, sulfuric acid solution is to metallic aluminium and three oxidations two
Aluminum oxidation film is respectively provided with the effect of dissolving, and then during whole electrochemicial oxidation, there is following chemical reaction:
2Al+3H2SO4→Al2(SO4)3+3H2↑
Al2O3+3H2SO4→Al2(SO4)3+3H2O
It can be seen that in whole electrolytic process, there is two processes of electrochemical reaction and chemical reaction.It is anti-by electrochemistry
The generating process of oxide-film and the course of dissolution of the oxide-film in chemical reaction in answering so that in aluminium alloy conductive shield
Preparation process in, it is to be ensured that the speed of growth is more than dissolution velocity, and such conductive shield can just generate in aluminum alloy surface;And
And there are insulating properties when the conductive shield of aluminum alloy surface reaches more than 0.02 micron, and then cause oxidation treatment time
And treatment conditions and raw material are selected in order to which the factor of key, its reason are:In chemical reaction, for
The environment that concentration, raw material between each raw material are in is different, and the time of processing is different, and it is in electrochemical oxidation reactions process
In, it is different to form the speed of alundum (Al2O3) oxide-film and the thickness of generation in aluminum alloy surface;Meanwhile in aluminium
The oxidation film layer thickness that alloy surface is formed is relatively low, it will causes the corrosion resistance of aluminium alloy weaker, shortens aluminum alloy materials
The service life of equipment, based on this, this researcher in electrochemical reaction by generating alundum (Al2O3) oxidation film layer and sulfuric acid
The reaction of alundum (Al2O3) oxidation film layer is dissolved, by controlling oxidization time, the condition of electrochemical reaction and the selection of raw material
The forward and backward processing step with electrochemistry so that form thickness in aluminum alloy material surface as 0.005~0.008 micron so that aluminium closes
Gold surface oxidation film layer forms porous state, and comparatively dense oxide film protection layer is formed in aluminum alloy surface;And then make
The dyeing processing obtained subsequently can be adsorbed by aperture, by Dye Adsorption in aperture, and then obtain required aluminium alloy material
The color of material.So that in the uniform color of aluminum alloy material surface, the electric conductivity of aluminum alloy surface is improved, it is therefore prevented that oxidation
Film layer forms caused insulating properties so that the contact resistance of aluminum alloy surface is 22m Ω;In addition, it can be with root
According to the different demands of color, and then the product of different colours is produced, improve the color diversification after aluminium alloy conductive protection.
Embodiment
Limited with reference to specific embodiment technical scheme is further, but claimed
Scope is not only limited to made description.
Embodiment 1
A kind of preparation method of aluminium alloy golden yellow conductive oxide film, it is using gasoline that the greasy dirt of aluminum alloy material surface is clear
After wash clean, then aluminum alloy materials are placed in sodium hydroxide solution, the temperature for controlling sodium hydroxide solution is 60 DEG C, at immersion
After managing 0.5min, then the clear water of flowing is used to clean up;After being used salpeter solution immersion 0.5min again, using stream
Dynamic clear water cleans up;Electrolytic oxidation process is carried out again, i.e., the anode tap that aluminum alloy materials are placed in electrolytic cell is carried out
Electrolysis is handled, and the electrolyte in electrolytic process is sulfuric acid, and its concentration is 180g/l, and temperature is 13 DEG C, and current density is
0.5A/dm2, voltage 13V, processing time 4min;After the completion of processing, then the clear water of flowing is used to clean up;Again
Used dyeing liquor in temperature for 55 DEG C of immersion 1min, then used the clear water of flowing to clean up, and used pressure
Contracting air blow drying is packed behind surface, you can obtains product.The speed that compressed air is produced by boasting is 1.5-3.7m3/h。
After described dyeing liquor is the mass mixings such as the alizarin red that alizarin yellow and the concentration that concentration is 0.25g/l are 0.1g/l
Mixed liquor.
The surface contacted resistance of the product is detected, it is 21.7m Ω, and the thickness of oxidation film layer is 0.005 micron.
Embodiment 2
A kind of preparation method of aluminium alloy golden yellow conductive oxide film, using gasoline by aluminum alloy materials 1m2The oil on surface
After dirt cleans up, then aluminum alloy materials are placed in sodium hydroxide solution, the temperature for controlling sodium hydroxide solution is 70 DEG C, leaching
After bubble processing 1min, then the clear water of flowing is used to clean up;After being used salpeter solution immersion 1min again, using stream
Dynamic clear water cleans up;Electrolytic oxidation process is carried out again, i.e., the anode tap that aluminum alloy materials are placed in electrolytic cell is carried out
Electrolysis is handled, and the electrolyte in electrolytic process is sulfuric acid, and its concentration is 200g/l, and temperature is 15 DEG C, and current density is
0.8A/dm2, voltage 15V, processing time 6min;After the completion of processing, then the clear water of flowing is used to clean up;Again
Used dyeing liquor in temperature for 60 DEG C of immersion 2min, then used the clear water of flowing to clean up, and used pressure
Contracting air blow drying is packed behind surface, you can obtains product.The speed that compressed air is produced by boasting is 1.5-3.7m3/h。
Above-mentioned sodium hydroxide solution, its concentration are 60g/l;The mass percent of above-mentioned salpeter solution is 50%.
After described dyeing liquor is the mass mixings such as the alizarin red that alizarin yellow and the concentration that concentration is 0.3g/l are 0.15g/l
Mixed liquor.
The surface contacted resistance of the product is detected, it is 22m Ω, and the thickness of oxidation film layer is 0.008 micron.Electricity
Mirror figure is observed, the uniform color on its surface, in golden yellow.
Embodiment 3
A kind of preparation method of aluminium alloy golden yellow conductive oxide film, using gasoline by aluminum alloy materials 5m2The oil on surface
After dirt cleans up, then aluminum alloy materials are placed in sodium hydroxide solution, the temperature for controlling sodium hydroxide solution is 65 DEG C, leaching
After bubble processing 0.8min, then clear water is used to clean up;After being used salpeter solution immersion 0.7min again, using clear water
Clean up;Being carried out electrolytic oxidation process again, i.e., the anode tap that aluminum alloy materials are placed in electrolytic cell carries out electrolysis processing,
Electrolyte in electrolytic process is sulfuric acid, and its concentration is 190g/l, and temperature is 14 DEG C, current density 0.7A/dm2, electricity
Press as 14V, processing time 5min;After the completion of processing, then clear water is used to clean up;Dyeing liquor is used again in temperature
Spend and soak 1.5min for 58 DEG C, then used clear water to clean up, and packed after being used compressed air drying surface, i.e.,
Product can be obtained.
Described dyeing liquor is the mass mixings such as the alizarin red that the alizarin yellow that concentration is 0.28g/l is 0.13g/l with concentration
Mixed liquor afterwards.
Above-mentioned gasoline is using 120# gasoline.
Above-mentioned sodium hydroxide solution, its concentration are 65g/l;The mass percent of above-mentioned salpeter solution is 50%.
The surface contacted resistance of the product is detected, it is 22.1m Ω, and the thickness of oxidation film layer is 0.007 micron.
Observed using electron microscope, its surface color is consistent, in golden yellow.
Embodiment 4
A kind of preparation method of aluminium alloy golden yellow conductive oxide film, using gasoline by aluminum alloy materials 10m2The oil on surface
After dirt cleans up, then aluminum alloy materials are placed in sodium hydroxide solution, the temperature for controlling sodium hydroxide solution is 60 DEG C, leaching
After bubble processing 1min, then the clear water of flowing is used to clean up;After being used salpeter solution immersion 0.5min again, use
The clear water of flowing cleans up;Electrolytic oxidation process is carried out again, i.e., the anode tap that aluminum alloy materials are placed in electrolytic cell enters
Row electrolysis is handled, and the electrolyte in electrolytic process is sulfuric acid, and its concentration is 180g/l, and temperature is 15 DEG C, and current density is
0.5A/dm2, voltage 15V, processing time 4min;After the completion of processing, then the clear water of flowing is used to clean up;Again
Used dyeing liquor in temperature for 55 DEG C of immersion 2min, then used the clear water of flowing to clean up, and used sky
Air-blowing is packed after doing surface, you can obtains product.
Described dyeing liquor is the mass mixings such as the alizarin red that the alizarin yellow that concentration is 0.25g/l is 0.13g/l with concentration
Mixed liquor afterwards.
Above-mentioned gasoline is using 120# gasoline.
Above-mentioned sodium hydroxide solution, its concentration are 63g/l;The mass percent of above-mentioned salpeter solution is 50%.
The surface contacted resistance of the product is detected, it is 22.1m Ω, and the thickness of oxidation film layer is 0.006 micron.
Observed using electron microscope, its surface color is consistent, in golden yellow.
Embodiment 5
A kind of preparation method of aluminium alloy golden yellow conductive oxide film, it is using gasoline that the greasy dirt of aluminum alloy material surface is clear
After wash clean, then aluminum alloy materials are placed in sodium hydroxide solution, the temperature for controlling sodium hydroxide solution is 70 DEG C, at immersion
After managing 0.5min, then the clear water of flowing is used to clean up;After being used salpeter solution immersion 1min again, using flowing
Clear water clean up;Electrolytic oxidation process is carried out again, i.e., the anode tap that aluminum alloy materials are placed in electrolytic cell carries out electricity
Solution is handled, and the electrolyte in electrolytic process is sulfuric acid, and its concentration is 200g/l, and temperature is 13 DEG C, current density 0.8A/
Dm2, voltage 13V, processing time 4-6min;After the completion of processing, then the clear water of flowing is used to clean up;Again by it
Use dyeing liquor in temperature for 55 DEG C of immersion 1min, then used the clear water of flowing to clean up, and used air to blow
Packed behind dry surface, you can obtain product.
After described dyeing liquor is the mass mixings such as the alizarin red that alizarin yellow and the concentration that concentration is 0.28g/l are 0.1g/l
Mixed liquor.
Above-mentioned gasoline is using 120# gasoline.
Above-mentioned sodium hydroxide solution, its concentration are 64g/l;The mass percent of above-mentioned salpeter solution is 50%.
The surface contacted resistance of the product is detected, it is 22.05m Ω, and the thickness of oxidation film layer is micro- for 0.0075
Rice.Observed using electron microscope, its surface color is uniform, in golden yellow.
In addition, above-mentioned dyeing liquor is also substituted for the raw material of other color and lusters by this researcher, and then draws and dye out
The color and luster of the aluminum alloy material surface come is homogeneous, is not in have a plurality of color ribbon, i.e., will not show rainbow color so that aluminium
The even dyeing of alloy material surface, quality are more excellent;Especially by electrochemical reaction and chemical reaction balance each other a little when
Between, the control of the concentration and voltage, electric current of temperature and electrolyte so that it is homogeneous to form some in aluminum alloy material surface
Space, by the absorption in space, reach the purpose of even dyeing, but also be aluminum alloy material surface formed one layer protection
Film, the diaphragm are alundum (Al2O3) oxidation film layer, and its thickness is between 0.005-0.008 microns so that is preventing aluminium alloy
During the corrosion of material, it is ensured that the electric conductivity of aluminum alloy materials, its surface contacted resistance are 21.7~22.1m Ω, electric conductivity
Can be good.
Claims (7)
1. a kind of preparation method of aluminium alloy golden yellow conductive oxide film, it is characterised in that go aluminum alloy materials by gasoline
After greasy dirt, clear water cleaning;After being placed on sodium hydroxide solution degreasing again, clear water cleaning;It is placed in salpeter solution and soaks again
After steeping 0.5-1min, clear water cleaning;It is placed in electrolytic tank electrolysis as anode again to aoxidize, the concentration of electrolyte in electrolytic cell is
180-200g/l sulfuric acid solution, its temperature are 13-15 DEG C, electrolytic processing time 4-6min, decomposition voltage 13-15V, electricity
Solution current density is 0.5-0.8A/dm2, after the completion of electrolysis, clear water cleaning;The dyeing liquor that temperature is 55-60 DEG C is placed on again
Middle immersion 1-2min, clear water cleaning;Drying, packaging;Golden yellow conductive oxide film is prepared, thickness is that 0.005-0.008 is micro-
Rice, surface contacted resistance is 21.7-22.1m Ω;Described sodium hydroxide solution degreasing, it is that aluminum alloy materials are placed in into hydrogen
Immersion treatment 0.5-1min in sodium hydroxide solution;
Described salpeter solution, its mass percent are 50%.
2. the preparation method of aluminium alloy golden yellow conductive oxide film as claimed in claim 1, it is characterised in that described gasoline
Degreasing is to carry out cleaning treatment to the surface of aluminum alloy materials using 120# gasoline.
3. the preparation method of aluminium alloy golden yellow conductive oxide film as claimed in claim 1, it is characterised in that described clear water
Cleaning, it is to carry out cleaning treatment using the clear water of flowing.
4. the preparation method of aluminium alloy golden yellow conductive oxide film as claimed in claim 1, it is characterised in that described hydrogen-oxygen
Change sodium solution, its concentration is 60-65g/l.
5. the preparation method of the aluminium alloy golden yellow conductive oxide film as described in claim 1 or 4, it is characterised in that described
Sodium hydroxide solution, its temperature are 60-70 DEG C.
6. the preparation method of aluminium alloy golden yellow conductive oxide film as claimed in claim 1, it is characterised in that described dyeing
Liquid, its composition of raw materials be alizarin yellow and the concentration that concentration is 0.25-0.3g/l be 0.1-0.15g/l alizarin red according to etc. quality
Than the mixed liquor of mixing.
7. the preparation method of aluminium alloy golden yellow conductive oxide film as claimed in claim 1, it is characterised in that described blows
Dry, it uses the surface of air blow drying aluminum alloy materials.
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