CN106868565B - Oxidation treatment method for 7-series aluminum alloy - Google Patents
Oxidation treatment method for 7-series aluminum alloy Download PDFInfo
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- CN106868565B CN106868565B CN201611248658.XA CN201611248658A CN106868565B CN 106868565 B CN106868565 B CN 106868565B CN 201611248658 A CN201611248658 A CN 201611248658A CN 106868565 B CN106868565 B CN 106868565B
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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 an oxidation treatment method of 7 series aluminum alloy, wherein an oxidation solution contains 80 g/L-140 g/L concentrated sulfuric acid and 10 g/L-50 g/L oxalic acid, the proportion of the concentrated sulfuric acid and the oxalic acid is proper, in the process of forming an oxidation film by electrolysis under the conditions that the voltage is 15V-22V and the temperature is 14-22 ℃, oxalate ions and sulfate ions in the oxidation solution generate competitive adsorption, sulfate radicals are mainly adsorbed at the bottom of micropores of the oxidation film, oxalate radicals are mainly adsorbed at the wall of the micropores of the oxidation film, the dissolution of the oxalic acid on the oxidation film is weaker than that of sulfuric acid, the dissolution of the wall of the micropores is reduced, the formed oxidation film has small and compact pore diameter and uniform micropore distribution, so that the quality and the adhesive force of the oxidation films at different positions are uniformly distributed, the adhesive force of the oxidation films is stronger, and the oxidation films are not easy to fall off.
Description
Technical field
The present invention relates to oxidation technology fields, more particularly, to a kind of oxidation treatment method of 7 line aluminium alloys.
Background technique
In recent years, metal alloy in the electronics fields such as phone housing, computer casing and frame application increasingly
It is more.These alloy products generally will do it anodized such as aluminium alloy, magnesium alloy or titanium alloy, be formed on its surface resistance to
The preferable anode oxide film of mill property.
Compared with more commonly used 6 line aluminium alloy (main magnesium-doped with the aluminium alloy of silicon), (the main doping of 7 line aluminium alloys
The aluminium alloy of zinc) have higher hardness and strength.As the material of electronic product casing and center, 7 line aluminium alloys have weight
The advantages of measuring gently and be less susceptible to bending, deformation, is just favored by more and more electronic product manufacturers.
However, using traditional 6 line aluminium alloy technique (sulphuric acid anodizing) of anodic oxidation come when aoxidizing 7 line aluminium alloy,
Since 7 line aluminium alloys especially Al-Zn-Mg system alloying component is higher, the meeting that each constituent is difficult to avoid that in aluminium alloy is distributed
Unevenly, segregation, also referred to as gross segregation are generated.Aluminium is segregated in after sulphuric acid anodizing, aoxidizes the micropore size of film surface
Differ larger, coating mass and adhesive force the meeting different from of different location, portion oxidation film adhesive force is weaker, easily de-
It falls.
Summary of the invention
Based on this, it is necessary to provide a kind of oxidation treatment method of oxidation film 7 line aluminium alloys not easily to fall off.
A kind of oxidation treatment method of 7 line aluminium alloy, includes 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 are electrolysed the oxidation solution under conditions of being 14 DEG C~22 DEG C, to form oxidation film on 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 in the oxidation solution containing 100g/L~140g/L
Oxalic acid.
In one embodiment, the concentrated sulfuric acid is sulfuric acid of the concentration 98% or more.
In one embodiment, the concentrated sulfuric acid and 10g/L~50g/L in the oxidation solution containing 80g/L~140g/L
Oxalic acid and surplus water.
In one embodiment, before the operation 7 line aluminium alloys being immersed in the oxidation solution, further include by
7 line aluminium alloy impregnates handles 1h~2h in an acidic solution.
In one embodiment, described in voltage is 15V~22V, and temperature is electrolysed institute under conditions of being 14 DEG C~22 DEG C
It states in the operation of oxidation solution, the voltage control is constant voltage, and the temperature control is steady temperature.
In one embodiment, described in voltage is 15V~22V, and temperature is electrolysed institute under conditions of being 14 DEG C~22 DEG C
It states in the operation of oxidation solution, the voltage is 18V, and the temperature is 15 DEG C.
In one embodiment, described in voltage is 15V~22V, and temperature is electrolysed institute under conditions of being 14 DEG C~22 DEG C
It states in the operation of oxidation solution, electrolysis time is 40min~80min.
In one embodiment, described in voltage is 15V~22V, and temperature is electrolysed institute under conditions of being 14 DEG C~22 DEG C
It states in the operation of oxidation solution, cathode is stereotype, stainless steel plate, titanium plate or graphite plate.
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, the condition that temperature is 14 DEG C~22 DEG C in voltage
During lower electrolysis forms oxidation film, oxalate denominationby and sulfate ion in oxidation solution generate competitive Adsorption, sulfate radical
Primary attachment is in the bottom hole of oxide-film micropore, and oxalate primary attachment, in the hole wall of oxide-film micropore, oxalic acid is to oxidation film
Dissolution is weaker than sulfuric acid, reduces the dissolution of micropore hole wall, and the aperture of the oxidation film of formation is small, fine and close, and micropore is evenly distributed,
So that the coating mass and adhesive force of different location are evenly distributed, oxidation film adhesive force is stronger, not easily to fall off.
Detailed description of the invention
Fig. 1 is the flow chart of the oxidation treatment method of 7 line aluminium alloys of an embodiment；
Fig. 2 handles 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 handles 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
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Referring to Fig. 1, the oxidation treatment method of 7 line aluminium alloys of an embodiment includes the following steps S110~S120.
S110, offer oxidation solution, the grass of the concentrated sulfuric acid containing 80g/L~140g/L and 10g/L~50g/L in oxidation solution
Acid.
Specifically, the mass ratio of the concentrated sulfuric acid and oxalic acid is 80~140:10~50 in oxidation solution.Inventor passes through optimization oxygen
Change the abundant of liquid, has been surprisingly found that the oxidation solution of the concentrated sulfuric acid containing 80g/L~140g/L and the oxalic acid of 10g/L~50g/L is special
It is suitable for 7 line aluminium alloy oxidation processes, the oxidation film of formation is not easily to fall off.
In one embodiment, the grass of the concentrated sulfuric acid in oxidation solution containing 100g/L~140g/L and 10g/L~25g/L
Acid.
Specifically, the concentrated sulfuric acid is sulfuric acid of the concentration 98% or more.Such as concentration be 98% sulfuric acid, concentration be 99%
Sulfuric acid etc..
In one embodiment, the grass of the concentrated sulfuric acid in oxidation solution containing 80g/L~140g/L and 10g/L~50g/L
The water of acid and surplus.With water as solvent, the concentrated sulfuric acid can be uniformly mixed with oxalic acid, and the electric conductivity of water is good.Into
One step, water can be deionized water.
Specifically, oxidation solution is ready-to-use.The oxidation solution of one embodiment is configured by following preparation method: by concentration
It is slowly flowed into a certain amount of deionized water for 98% sulfuric acid, it is stirring while adding, the first solution is obtained after mixing.Then
Oxalic acid is added in one solution, deionized water is added after mixing and is settled to preset volume, obtains oxidation solution.Wherein, every 1L oxidation
The concentrated sulfuric acid of 80g~140g need to be added in liquid, and the oxalic acid of 10g~50g need to be added in every 1L oxidation solution.
S120,7 line aluminium alloys are immersed in oxidation solution obtained in S110, using 7 line aluminium alloys as anode, in voltage
For 15V~22V, temperature is electrolytic oxidation liquid under conditions of 14 DEG C~22 DEG C, to form oxidation 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 7 line aluminium alloys being immersed in the operation in oxidation solution, further include by 7 be aluminium close
Gold impregnates handles 1h~2h in an acidic solution.Specifically, acid solution can be 20g/L~40g/L phosphoric acid solution.It is acid molten
Liquid can etch the surface of 7 line aluminium alloys, to keep the surface of 7 line aluminium alloys more smooth, the oxidation film formed after oxidation is attached
Put forth effort relatively strong.
In one embodiment, voltage control is constant voltage, and temperature control is steady temperature.Constant voltage and perseverance
Fixed temperature is conducive to oxidation balance progress, enhances the adhesive force of oxidation film.
In one embodiment, voltage 18V, temperature are 15 DEG C.Voltage is appropriate with temperature, is suitable for 7 line aluminium alloys
The oxidation film of oxidation processes, formation is not easily to fall 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 for, and adhesive force is by force not
It is easy to fall off.
In one embodiment, cathode is stereotype, stainless steel plate, titanium plate or graphite plate.Specifically, 7 line aluminium alloys are made
For anode, stereotype, stainless steel plate, titanium plate or graphite plate are immersed in as cathode, anode and cathode containing 80g/L~140g/L's
In the electrolyte of the oxalic acid of the concentrated sulfuric acid and 10g/L~50g/L, after powering on, fine and close oxidation can be formed in anode surface
Film.
In one embodiment, 7 line aluminium alloys obtained after the oxidation treatment method of above-mentioned 7 line aluminium alloy, warp
It after the processing of the processes such as table tune, dyeing, sealing of hole, ash disposal, drying, then tears through 180 DEG C of high-temperature bakings and 3M gluing, counts its demoulding number
Amount.
7 line aluminium alloys are the aluminium alloy of main doping zinc, and 7 line aluminium alloys have higher hardness and strength, however due to 7
Line aluminium alloy especially Al-Zn-Mg system alloying component is higher, and the meeting that each constituent is difficult to avoid that in aluminium alloy is unevenly distributed
Even, general method is easy to produce 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 and 10g/L~50g/L in liquid containing 80g/L~140g/L, the concentrated sulfuric acid and oxalic acid is appropriate, mixes
Conjunction acid formula is simple, and raw material is cheap and easy to get.It is 15V~22V in voltage, temperature is electrolysed under conditions of being 14 DEG C~22 DEG C and is formed
During oxidation film, oxalate denominationby and sulfate ion in oxidation solution generate competitive Adsorption, 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 oxidation film
Sulfuric acid is weak, reduces the dissolution of micropore hole wall, and the aperture of the oxidation film of formation is small, fine and close, and micropore is evenly distributed, so that not
Coating mass and adhesive force with position are evenly distributed, and oxidation film adhesive force is stronger, not easily to fall off.
The oxidation treatment method of above-mentioned 7 line aluminium alloy, oxidation operation is easy, and technological parameter is easy to control, can be widely applied
In the surface treatment of the electronic products such as mobile phone, the computer of 7 line aluminium alloy materials.
The following are specific embodiments.
Following embodiment unless otherwise instructed, test method without specific conditions, usually according to normal condition.Implement
The concentrated sulfuric acid described in example 1~11 is the sulfuric acid that concentration is 98%.
Embodiment 1
7 line aluminium alloys are immersed in oxidation solution, the oxalic acid of the concentrated sulfuric acid and 15g/L in oxidation solution containing 120g/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, thus
7 line aluminium alloy surfaces form oxidation film.
Embodiment 2
7 line aluminium alloys are immersed in oxidation solution, the oxalic acid of the concentrated sulfuric acid and 10g/L in oxidation solution containing 80g/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, thus 7
Line aluminium alloy surface forms oxidation film.
Embodiment 3
7 line aluminium alloys are immersed in oxidation solution, the oxalic acid of the concentrated sulfuric acid and 50g/L in oxidation solution containing 140g/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, thus 7
Line aluminium alloy surface forms oxidation film.
Embodiment 4
7 line aluminium alloys are immersed in oxidation solution, the oxalic acid of the concentrated sulfuric acid and 15g/L in oxidation solution containing 80g/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, thus 7
Line aluminium alloy surface forms oxidation film.
Embodiment 7
7 line aluminium alloys are immersed in oxidation solution, the oxalic acid of the concentrated sulfuric acid and 17g/L in oxidation solution containing 80g/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, thus 7
Line aluminium alloy surface forms oxidation film.
Embodiment 8
7 line aluminium alloys are immersed in oxidation solution, the grass of the concentrated sulfuric acid and 21.53g/L in oxidation solution containing 100.91g/L
The deionized water of acid and surplus.It is 18V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, from
And oxidation film is formed on 7 line aluminium alloy surfaces.
Embodiment 9
7 line aluminium alloys are immersed in oxidation solution, the grass of the concentrated sulfuric acid and 15.59g/L in oxidation solution containing 120.49g/L
The deionized water of acid and surplus.It is 18V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, from
And oxidation film is formed on 7 line aluminium alloy surfaces.
Embodiment 10
7 line aluminium alloys are immersed in oxidation solution, the grass of the concentrated sulfuric acid and 15.59g/L in oxidation solution containing 120.49g/L
The deionized water of acid and surplus.It is 15V in constant voltage, steady temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C, from
And oxidation film is formed 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 in sulfuric acid solution containing 120g/L.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 and surplus in oxidation solution containing 120g/L
Water.It is 14V~15V in voltage, temperature is electrolytic oxidation liquid 60min under conditions of 15 DEG C~16 DEG C, thus in 7 line aluminium alloy tables
Face forms oxidation film.
Test one
The method that Examples 1 to 10 is respectively adopted handles 20 piece of 7 line aluminium alloy, and treated, and 7 line aluminium alloys are placed in 180 DEG C
40min is toasted under high temperature, is then torn with 3M sticker, and 200 pieces of treated 7 line aluminium alloys are without stripping phenomenon.
Test two
Repeat contrast verification
The method that embodiment 11 and embodiment 1 is respectively adopted handles 7 multiple batches of line aluminium alloys, treated 7 be aluminium close
Gold is placed under 180 DEG C of high temperature and toasts 40min, is then torn with 3M sticker, if there is demoulding, for defective products, counts total fraction defective.
The results are shown in Table 1, and the data statistics figure of table 1 please refers to Fig. 2.
Table 1: the method for embodiment 11 and embodiment 1 handles 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 (being free of oxalic acid 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 handles 7 multiple batches of line aluminium alloys, treated 7 be aluminium close
Gold assembling hot melt test, if there is demoulding, for defective products, counts total fraction defective.The results are shown in Table 2, the data statistics of table 2
Figure please refers to Fig. 3.
Table 2: the method for embodiment 12 and embodiment 1 handles the test result after 7 multiple batches of line aluminium alloys
| Processing method | It puts into (block) | Defective products (block) | Fraction defective |
| Implement 12 | 83 | 2 | 2.40% |
| Embodiment 1 | 181 | 0 | 0 |
The side for (being free of oxalic acid in oxidation solution, voltage and temperature are not constant when electrolysis) from table 2 it can be seen that embodiment 12
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, no stripping phenomenon.
Test four
7 multiple batches of line aluminium alloys are handled using the method for embodiment 1, including part reprocessed products (after oxidation processes
7 line aluminium alloys of demoulding), reprocessed products first use 30g/L phosphoric acid solution to impregnate 1.5h, to clean the oxidation that oxidation is formed for the first time
Film.Processing, which is placed under 180 DEG C of high temperature, toasts 40min, is then torn with 3M sticker, if there is demoulding, for defective products, counts total
Fraction defective.The results are shown in Table 3,
Table 3: the method for embodiment 1 handles 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, no demoulding is existing
As.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those 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
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
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| CN101498021B (en) * | 2009-01-15 | 2011-01-26 | 浙江名琦机电制造有限公司 | Surface treating method for tap |
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| US3997412A (en) * | 1974-05-22 | 1976-12-14 | Riken Light Metal Industries Company, Ltd. | Method of forming oxide film on aluminum or aluminum alloy |
| CN101298690A (en) * | 2007-05-04 | 2008-11-05 | 特耐固国际有限公司 | Anodizing aluminium and alloys thereof |
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