CN106868565A - The oxidation treatment method of 7 line aluminium alloys - Google Patents
The oxidation treatment method of 7 line aluminium alloys Download PDFInfo
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- CN106868565A CN106868565A CN201611248658.XA CN201611248658A CN106868565A CN 106868565 A CN106868565 A CN 106868565A CN 201611248658 A CN201611248658 A CN 201611248658A CN 106868565 A CN106868565 A CN 106868565A
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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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
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Abstract
The invention discloses a kind of oxidation treatment method of 7 line aluminium alloy, the oxalic acid of the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L in oxidation solution, the ratio of the concentrated sulfuric acid and oxalic acid is appropriate, it is 15V~22V in voltage, during temperature is for electrolysis forms oxide-film under conditions of 14 DEG C~22 DEG C, oxalate denominationby in oxidation solution produces competitive Adsorption with sulfate ion, bottom hole of the sulfate radical primary attachment in oxide-film micropore, and oxalate primary attachment is in the hole wall of oxide-film micropore, oxalic acid is weaker than sulfuric acid to the dissolution of oxide-film, reduce the dissolving of micropore hole wall, the aperture of the oxide-film of formation is small, it is fine and close, micropore is evenly distributed, so that the coating mass and adhesive force of diverse location are evenly distributed, oxide-film adhesive force is stronger, it is difficult for drop-off.
Description
Technical field
The present invention relates to oxidation technology field, more particularly, to a kind of oxidation treatment method of 7 line aluminium alloy.
Background technology
In recent years, application of the metal alloy in the electronics fields such as phone housing, computer casing and frame be increasingly
It is many.These alloy products, such as aluminium alloy, magnesium alloy or titanium alloy, can typically carry out anodized, form resistance on its surface
Mill property preferably anode oxide film.
Compared with 6 line aluminium alloys (the main magnesium-doped aluminium alloy with silicon) for more often using, (the main doping of 7 line aluminium alloys
The aluminium alloy of zinc) possess hardness and intensity higher.Used as electronic product casing and the material of center, 7 line aluminium alloys have weight
Amount is light and is less susceptible to bending, the advantage of deformation, is just favored by increasing electronic product manufacturer.
However, aoxidized during 7 line aluminium alloy using traditional line aluminium alloy technique (sulphuric acid anodizing) of anodic oxidation 6,
Because 7 line aluminium alloys particularly Al-Zn-Mg systems alloying component is higher, the meeting distribution that each constituent is difficult to avoid that in aluminium alloy
It is uneven, produce segregation, also referred to as gross segregation.Aluminium is segregated in after sulphuric acid anodizing, the micropore size on oxide-film surface
Difference is larger, and the coating mass and adhesive force of diverse location can be otherwise varied, and portion oxide-film adhesive force is weaker, easily de-
Fall.
The content of the invention
Based on this, it is necessary to provide a kind of oxidation treatment method of oxide-film 7 line aluminium alloys difficult for drop-off.
A kind of oxidation treatment method of 7 line aluminium alloy, comprises the following steps：
The oxidation solution of offer, the grass of the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L in the oxidation solution
Acid；And
7 line aluminium alloys are immersed in the oxidation solution, using 7 line aluminium alloy as anode, voltage be 15V~
22V, temperature under conditions of 14 DEG C~22 DEG C to be electrolysed the oxidation solution, so as to form oxide-film on the 7 line aluminium alloy surface.
In one embodiment, 7 line aluminium alloy is aluminium-zinc-magnesium system alloy, the aluminium, the zinc and the magnesium
Mass ratio be 100：1~8：1~4.
In one embodiment, the concentrated sulfuric acid and 10g/L~25g/L containing 100g/L~140g/L in the oxidation solution
Oxalic acid.
In one embodiment, the concentrated sulfuric acid is sulfuric acid of the concentration more than 98%.
In one embodiment, the concentrated sulfuric acid and 10g/L~50g/L containing 80g/L~140g/L in the oxidation solution
Oxalic acid and surplus water.
In one embodiment, before the operation that 7 line aluminium alloys are immersed in the oxidation solution, also including inciting somebody to action
The 7 line aluminium alloy immersion processes 1h~2h in an acidic solution.
In one embodiment, described is 15V~22V in voltage, and temperature under conditions of 14 DEG C~22 DEG C to be electrolysed institute
State in the operation of oxidation solution, the voltage is controlled to constant voltage, the temperature control is steady temperature.
In one embodiment, described is 15V~22V in voltage, and temperature under conditions of 14 DEG C~22 DEG C to be electrolysed institute
State in the operation of oxidation solution, the voltage is 18V, the temperature is 15 DEG C.
In one embodiment, described is 15V~22V in voltage, and temperature under conditions of 14 DEG C~22 DEG C to be electrolysed institute
State in the operation of oxidation solution, electrolysis time is 40min~80min.
In one embodiment, described is 15V~22V in voltage, and temperature under conditions of 14 DEG C~22 DEG C to be electrolysed institute
State in the operation of oxidation solution, negative electrode is stereotype, stainless steel plate, titanium plate or graphite cake.
The oxidation treatment method of above-mentioned 7 line aluminium alloy, the concentrated sulfuric acid and 10g/L containing 80g/L~140g/L in oxidation solution
The ratio of the oxalic acid of~50g/L, the concentrated sulfuric acid and oxalic acid is appropriate, is 15V~22V in voltage, and temperature is 14 DEG C~22 DEG C of condition
During lower electrolysis forms oxide-film, the oxalate denominationby in oxidation solution produces competitive Adsorption, sulfate radical with sulfate ion
, in the bottom hole of oxide-film micropore, and oxalate primary attachment, in the hole wall of oxide-film micropore, oxalic acid is to oxide-film for primary attachment
Dissolution is weaker than sulfuric acid, reduces the dissolving of micropore hole wall, and the aperture of the oxide-film of formation is small, densification, and micropore is evenly distributed,
So that the coating mass and adhesive force of diverse location are evenly distributed, oxide-film adhesive force is stronger, difficult for drop-off.
Brief description of the drawings
Fig. 1 is the flow chart of the oxidation treatment method of 7 line aluminium alloys of an implementation method；
Fig. 2 processes the statistics of the demoulding fraction defective after 7 multiple batches of line aluminium alloys for the method for embodiment 1 and embodiment 11
Result figure；
Fig. 3 processes the statistics of the demoulding fraction defective after 7 multiple batches of line aluminium alloys for the method for embodiment 1 and embodiment 12
Result figure.
Specific embodiment
To enable the above objects, features and advantages of the present invention more obvious understandable, below in conjunction with the accompanying drawings to the present invention
Specific embodiment be described in detail.Elaborate many details in order to fully understand this hair in the following description
It is bright.But the present invention can be implemented with being much different from other manner described here, and those skilled in the art can be not
Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited by following public specific implementation.
Fig. 1 is referred to, the oxidation treatment method of 7 line aluminium alloys of an implementation method comprises the following steps S110~S120.
S110, the oxidation solution for providing, the grass of the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L in oxidation solution
Acid.
Specifically, the concentrated sulfuric acid and the mass ratio of oxalic acid are 80~140 in oxidation solution：10~50.Inventor is by optimizing oxygen
Change the abundant of liquid, have been surprisingly found that the oxidation solution of the oxalic acid of the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L is special
Suitably to 7 line aluminium alloy oxidation processes, the oxide-film of formation is difficult for drop-off.
In one embodiment, in oxidation solution the concentrated sulfuric acid containing 100g/L~140g/L and 10g/L~25g/L grass
Acid.
Specifically, the concentrated sulfuric acid is sulfuric acid of the concentration more than 98%.Such as concentration be 98% sulfuric acid, concentration be 99%
Sulfuric acid etc..
In one embodiment, in oxidation solution the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L grass
Acid and the water of surplus.With water as solvent, the concentrated sulfuric acid can be well mixed with oxalic acid, and the electric conductivity of water is good.Enter
One step, water can be deionized water.
Specifically, oxidation solution is now with the current.The oxidation solution of one implementation method is configured by following preparation method：By concentration
Sulfuric acid for 98% slowly flows into a certain amount of deionized water, stirring while adding, and the first solution is obtained after mixing.Then
Oxalic acid is added in one solution, adds deionized water to be settled to default volume after mixing, obtain oxidation solution.Wherein, aoxidized per 1L
Liquid need to add the concentrated sulfuric acid of 80g~140g, and the oxalic acid of 10g~50g need to be added per 1L oxidation solutions.
S120,7 line aluminium alloys are immersed in the oxidation solution obtained in S110, using 7 line aluminium alloys as anode, in voltage
It is 15V~22V, temperature is electrolytic oxidation liquid under conditions of 14 DEG C~22 DEG C, so as to form oxide-film on 7 line aluminium alloy surfaces.
In present embodiment, 7 line aluminium alloys are aluminium-zinc-magnesium system alloy, and the mass ratio of aluminium, zinc and magnesium is 100：1~8：1
~4.Further, the mass ratio of aluminium, zinc and magnesium is 100：7~8：1~2.
In one embodiment, before the operation 7 line aluminium alloys being immersed in oxidation solution, also including being that aluminium is closed by 7
Gold immersion processes 1h~2h in an acidic solution.Specifically, acid solution can be 20g/L~40g/L phosphoric acid solutions.It is acid molten
Liquid energy enough etches the surface of 7 line aluminium alloys, so that the surface of 7 line aluminium alloys is more smooth, the oxide-film formed after oxidation is attached
Put forth effort stronger.
In one embodiment, voltage is controlled to constant voltage, and temperature control is steady temperature.Constant voltage and perseverance
Fixed temperature is conducive to the oxidation balance to carry out, and strengthens the adhesive force of oxide-film.
In one embodiment, voltage is 18V, and temperature is 15 DEG C.Voltage is appropriate with temperature, suitably to 7 line aluminium alloys
Oxidation processes, the oxide-film of formation is difficult for drop-off.
In one embodiment, electrolysis time is 40min~80min.In the concentrated sulfuric acid containing 80g/L~140g/L and
40min~80min is electrolysed in the oxidation solution of the oxalic acid of 10g/L~50g/L, the oxide thickness of formation is suitable, adhesive force is by force not
It is easy to fall off.
In one embodiment, negative electrode is stereotype, stainless steel plate, titanium plate or graphite cake.Specifically, 7 line aluminium alloys are made
It is anode, used as negative electrode, anode is immersed in negative electrode and contains 80g/L~140g/L's for stereotype, stainless steel plate, titanium plate or graphite cake
In the electrolyte of the oxalic acid of the concentrated sulfuric acid and 10g/L~50g/L, after switching on power, the oxidation of densification can be formed in anode surface
Film.
In one embodiment, by 7 line aluminium alloys obtained after the oxidation treatment method of above-mentioned 7 line aluminium alloy, warp
After the treatment of the operations such as table tune, dyeing, sealing of hole, ash disposal, drying, then through 180 DEG C of high-temperature bakings and 3M is gluing tears, its demoulding number is counted
Amount.
7 line aluminium alloys are the aluminium alloy of mainly doping zinc, and 7 line aluminium alloys possess hardness and intensity higher, yet with 7
Line aluminium alloy particularly Al-Zn-Mg systems alloying component is higher, the meeting skewness that each constituent is difficult to avoid that in aluminium alloy
Even, general method easily produces segregation, also referred to as gross segregation when aoxidizing.The oxidation treatment method of above-mentioned 7 line aluminium alloy, oxidation
The ratio of the oxalic acid of the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L in liquid, the concentrated sulfuric acid and oxalic acid is appropriate, and it is mixed
Close acid formula simple, raw material is cheap and easy to get.It is 15V~22V in voltage, temperature is electrolysis formation under conditions of 14 DEG C~22 DEG C
During oxide-film, the oxalate denominationby in oxidation solution produces competitive Adsorption with sulfate ion, and sulfate radical primary attachment exists
The bottom hole of oxide-film micropore, and oxalate primary attachment is in the hole wall of oxide-film micropore, dissolution ratio of the oxalic acid to oxide-film
Sulfuric acid is weak, reduces the dissolving of micropore hole wall, and the aperture of the oxide-film of formation is small, densification, and micropore is evenly distributed, so that not
It is evenly distributed with the coating mass and adhesive force of position, oxide-film adhesive force is stronger, difficult for drop-off.
The oxidation treatment method of above-mentioned 7 line aluminium alloy, oxidation operation is easy, and technological parameter is easily controlled, can extensive use
The surface treatment of the electronic products such as mobile phone, computer in 7 line aluminium alloy materials.
It is below specific embodiment.
Following examples unless otherwise instructed, the experimental technique of unreceipted actual conditions, generally according to normal condition.Implement
The concentrated sulfuric acid described in example 1~11 is sulfuric acid that concentration is 98%.
Embodiment 1
7 line aluminium alloys are immersed in oxidation solution, in oxidation solution the oxalic acid of the concentrated sulfuric acid containing 120g/L and 15g/L and
The deionized water of surplus.It is 18V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, so that
7 line aluminium alloy surfaces form oxide-film.
Embodiment 2
7 line aluminium alloys are immersed in oxidation solution, in oxidation solution the oxalic acid of the concentrated sulfuric acid containing 80g/L and 10g/L and
The deionized water of surplus.It is 15V in constant voltage, steady temperature is electrolytic oxidation liquid 80min under conditions of 14 DEG C, so as to 7
Line aluminium alloy surface forms oxide-film.
Embodiment 3
7 line aluminium alloys are immersed in oxidation solution, in oxidation solution the oxalic acid of the concentrated sulfuric acid containing 140g/L and 50g/L and
The deionized water of surplus.It is 22V in constant voltage, steady temperature is electrolytic oxidation liquid 40min under conditions of 22 DEG C, so as to 7
Line aluminium alloy surface forms oxide-film.
Embodiment 4
7 line aluminium alloys are immersed in oxidation solution, in oxidation solution the oxalic acid of the concentrated sulfuric acid containing 80g/L and 15g/L and
The deionized water of surplus.It is 15V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, so as to 7
Line aluminium alloy surface forms oxide-film.
Embodiment 7
7 line aluminium alloys are immersed in oxidation solution, in oxidation solution the oxalic acid of the concentrated sulfuric acid containing 80g/L and 17g/L and
The deionized water of surplus.It is 15V in constant voltage, steady temperature is electrolytic oxidation liquid 65min under conditions of 15 DEG C, so as to 7
Line aluminium alloy surface forms oxide-film.
Embodiment 8
7 line aluminium alloys are immersed in oxidation solution, the grass of the concentrated sulfuric acid containing 100.91g/L and 21.53g/L in oxidation solution
Acid and the deionized water of surplus.It is 18V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, from
And form oxide-film on 7 line aluminium alloy surfaces.
Embodiment 9
7 line aluminium alloys are immersed in oxidation solution, the grass of the concentrated sulfuric acid containing 120.49g/L and 15.59g/L in oxidation solution
Acid and the deionized water of surplus.It is 18V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, from
And form oxide-film on 7 line aluminium alloy surfaces.
Embodiment 10
7 line aluminium alloys are immersed in oxidation solution, the grass of the concentrated sulfuric acid containing 120.49g/L and 15.59g/L in oxidation solution
Acid and the deionized water of surplus.It is 15V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, from
And form oxide-film on 7 line aluminium alloy surfaces.
Embodiment 11
7 line aluminium alloys are immersed in sulfuric acid solution, the water of the surplus of the concentrated sulfuric acid containing 120g/L in sulfuric acid solution.Its
Remaining electrolytic condition is same as Example 1.
Embodiment 12
7 line aluminium alloys are immersed in oxidation solution, the deionization of the concentrated sulfuric acid containing 120g/L and surplus in oxidation solution
Water.It is 14V~15V in voltage, temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C~16 DEG C, so as in 7 line aluminium alloy tables
Face forms oxide-film.
Test one
The method that embodiment 1~10 is respectively adopted processes 20 piece of 7 line aluminium alloy, and 7 line aluminium alloys after treatment are placed in 180 DEG C
40min is toasted under high temperature, is then torn with 3M stickers, 7 line aluminium alloys after 200 pieces for the treatment of are without stripping phenomenon.
Test two
Repeat contrast verification
The method that embodiment 11 and embodiment 1 is respectively adopted processes 7 multiple batches of line aluminium alloys, and after treatment 7 is that aluminium is closed
Gold toasts 40min under being placed in 180 DEG C of high temperature, is then torn with 3M stickers, is defective products if there is demoulding, counts total fraction defective.
As shown in table 1, the data statistics figure of table 1 refers to Fig. 2 to result.
Table 1：The method of embodiment 11 and embodiment 1 processes the test result after 7 multiple batches of line aluminium alloys
As it can be seen from table 17 line aluminium alloys after the method oxidation processes of embodiment 11 (oxalic acid is free of in oxidation solution) are not
Yield is 5.35%, and demoulding ratio is high.And 7 line aluminium alloy fraction defectives after the method oxidation processes of embodiment 1 are only 0.51%,
Demoulding ratio is low.
Test three
The method that embodiment 12 and embodiment 1 is respectively adopted processes 7 multiple batches of line aluminium alloys, and after treatment 7 is that aluminium is closed
Gold assembling hot melt test, is defective products if there is demoulding, counts total fraction defective.Result is as shown in table 2, the data statistics of table 2
Figure refers to Fig. 3.
Table 2：The method of embodiment 12 and embodiment 1 processes the test result after 7 multiple batches of line aluminium alloys
| Processing method | Input (block) | Defective products (block) | Fraction defective |
| Implement 12 | 83 | 2 | 2.40% |
| Embodiment 1 | 181 | 0 | 0 |
From table 2 it can be seen that the side of embodiment 12 (oxalic acid being free of in oxidation solution, voltage and temperature are not constant during electrolysis)
The fraction defective of 7 line aluminium alloys after method oxidation processes is 2.4%, and demoulding ratio is high.And after the method oxidation processes of embodiment 1
The fraction defective 0% of 7 line aluminium alloys, without stripping phenomenon.
Test four
7 multiple batches of line aluminium alloys are processed using the method for embodiment 1, including part reprocessed products (after oxidation processes
7 line aluminium alloys of demoulding), reprocessed products first soak 1.5h with 30g/L phosphoric acid solutions, to clean the oxidation that oxidation is formed for the first time
Film.It is placed in after treatment under 180 DEG C of high temperature and toasts 40min, then torn with 3M stickers, be defective products if there is demoulding, is counted total
Fraction defective.Result is as shown in table 3,
Table 3：The method of embodiment 1 processes the test result after 7 multiple batches of line aluminium alloys
From table 3 it can be seen that the fraction defective 0% of 7 line aluminium alloys after the method oxidation processes of embodiment 1, existing without demoulding
As.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of oxidation treatment method of 7 line aluminium alloy, it is characterised in that comprise the following steps：
The oxidation solution of offer, the oxalic acid of the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L in the oxidation solution；With
And
7 line aluminium alloys are immersed in the oxidation solution, are 15V~22V, temperature in voltage using 7 line aluminium alloy as anode
Spend to be electrolysed the oxidation solution under conditions of 14 DEG C~22 DEG C, so as to form oxide-film on the 7 line aluminium alloy surface.
2. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that 7 line aluminium alloy is
Aluminium-zinc-magnesium system alloy, the aluminium, the zinc are 100 with the mass ratio of the magnesium：1~8：1~4.
3. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that contain in the oxidation solution
The concentrated sulfuric acid of 100g/L~140g/L and the oxalic acid of 10g/L~25g/L.
4. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that the concentrated sulfuric acid is concentration
Sulfuric acid more than 98%.
5. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that contain in the oxidation solution
The water of the concentrated sulfuric acid of 80g/L~140g/L and the oxalic acid of 10g/L~50g/L and surplus.
6. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that described by the leaching of 7 line aluminium alloys
Before steeping the operation in the oxidation solution, also including 7 line aluminium alloy immersion is processed into 1h~2h in an acidic solution.
7. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that it is described voltage be 15V~
22V, temperature is to be electrolysed in the operation of the oxidation solution under conditions of 14 DEG C~22 DEG C, and the voltage is controlled to constant voltage, institute
Temperature control is stated for steady temperature.
8. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that it is described voltage be 15V~
22V, temperature is to be electrolysed in the operation of the oxidation solution under conditions of 14 DEG C~22 DEG C, and the voltage is 18V, and the temperature is 15
℃。
9. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that it is described voltage be 15V~
22V, temperature is to be electrolysed in the operation of the oxidation solution under conditions of 14 DEG C~22 DEG C, and electrolysis time is 40min~80min.
10. the oxidation treatment method of 7 line aluminium alloy according to claim 1, it is characterised in that described is 15V in voltage
~22V, temperature is to be electrolysed in the operation of the oxidation solution under conditions of 14 DEG C~22 DEG C, and negative electrode is stereotype, stainless steel plate, titanium plate
Or graphite cake.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129854A (en) * | 2018-02-08 | 2019-08-16 | 华为技术有限公司 | A kind of preparation method and terminal device of oxidation film |
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