CN104005071B - Aluminum alloy surface process in sealing treatment method and the confining liquid of employing - Google Patents

Aluminum alloy surface process in sealing treatment method and the confining liquid of employing Download PDF

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Publication number
CN104005071B
CN104005071B CN201410220061.9A CN201410220061A CN104005071B CN 104005071 B CN104005071 B CN 104005071B CN 201410220061 A CN201410220061 A CN 201410220061A CN 104005071 B CN104005071 B CN 104005071B
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sealing treatment
confining liquid
aluminum alloy
treatment method
alloy surface
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CN104005071A (en
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马迪
齐轩
李树白
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Jiangsu University of Technology
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Jiangsu University of Technology
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Priority to CN201610594307.8A priority patent/CN106191961B/en
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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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment

Abstract

The invention discloses the confining liquid of a kind of sealing treatment method during aluminum alloy surface processes and employing thereof, the aluminium alloy after surface treated is placed in confining liquid and soaks, wash after taking-up, dries by sealing treatment method.Described confining liquid is made up of the component of following concentration: four cerium sulfate hydrate 5～25g/L, lanthanum nitrate hexahydrate 1～5g/L, Ammonium persulfate. 0.5～2.5g/L.The time soaked is 50～70min, and confining liquid temperature is 40～60 DEG C.The confining liquid of the present invention is not only friendly to environment and human body, and can be greatly improved the decay resistance of the oxide-film after sealing treatment.

Description

Aluminum alloy surface process in sealing treatment method and the confining liquid of employing
Technical field
The invention belongs to technical field of aluminum alloy surface treatment, be specifically related to the confining liquid of a kind of sealing treatment method during aluminum alloy surface processes and employing thereof.
Background technology
The surface treatment of aluminium alloy mainly includes anodic oxidation and chemical oxidation, wherein needs to carry out pre-treatment before the oxidation, then needs to carry out sealing treatment after oxidation, and sealing treatment is mainly for improving the decay resistance of oxide-film.
Difference according to confining liquid, conventional sealing treatment method specifically includes that method closed by nickel fluorine system method, potassium dichromate method, rare chromic acid and rare earth closes method.
Wherein nickel fluorine system method, potassium dichromate method and rare chromic acid close method be advantageous in that sealing treatment after oxide-film there is good decay resistance, shortcoming is then that environment and human influence is relatively big, such as Ni2+And F-Human body and environment are caused high risks by capital, and Cr6+It is listed in one of chemical substance that harm is maximum especially, is internationally recognized carcinogen.
Rare earth is closed the advantage of method and is then in that environmental protection, environment and human body is friendly, the oxide-film decay resistance that shortcoming is then after sealing treatment is not good, and rare earth is closed the confining liquid of method employing and is mainly rare earth carbonate (Chinese patent literature CN1746341A, CN103173833A etc.) or rare earth nitrate (Chinese patent literature CN102560489A, CN103305892A, CN103614757A etc.).
Chinese patent literature CN102650068A discloses a kind of aluminum and aluminum alloy anodic oxide film sealant and preparation method thereof, and the sealer that the method adopts is made up of rare earth nitrate, oxidant, stabilizer and deionized water；Wherein rare earth nitrate is selected from cerous nitrate, Yttrium trinitrate or neodymium nitrate；Oxidant is selected from potassium permanganate, hydrogen peroxide, sodium perchlorate or potassium chlorate；Stabilizer is selected from potassium pyrophosphate or sodium pyrophosphate.The deficiency of the document is in that: the oxide-film decay resistance after being processed by this sealer is still undesirable.
Summary of the invention
An object of the present invention is in that to solve the problems referred to above, it is proposed to one is both friendly to environment and human body, ensure that again the oxide-film after closing has the sealing treatment method in the aluminum alloy surface process of the decay resistance of excellence.
Another object of the present invention is to the confining liquid providing above-mentioned sealing treatment method to adopt.
The technical scheme realizing one of the object of the invention is: the sealing treatment method in the process of a kind of aluminum alloy surface, is placed in by the aluminium alloy after surface treated in confining liquid and soaks, and washes, dries after taking-up；Described confining liquid is made up of the component of following concentration: four cerium sulfate hydrate 5～25g/L, lanthanum nitrate hexahydrate 1～5g/L, Ammonium persulfate. 0.5～2.5g/L.
Described confining liquid is preferably made up of the component of following concentration: four cerium sulfate hydrate 15g/L, lanthanum nitrate hexahydrate 3g/L, Ammonium persulfate. 1.5g/L.
The time of described immersion is 50～70min, and confining liquid temperature is 40～60 DEG C.
Described surface treatment is anodic oxidation or chemical oxidation.
The technical scheme realizing another object of the present invention is: the confining liquid that the sealing treatment method in the process of a kind of aluminum alloy surface adopts, and is made up of the component of following concentration: four cerium sulfate hydrate 5～25g/L, lanthanum nitrate hexahydrate 1～5g/L, Ammonium persulfate. 0.5～2.5g/L.
Preferably it is made up of the component of following concentration: four cerium sulfate hydrate 15g/L, lanthanum nitrate hexahydrate 3g/L, Ammonium persulfate. 1.5g/L.
The present invention has positive effect: (1) one aspect of the present invention adopts cerous sulfate to substitute cerous nitrate and Lanthanum (III) nitrate composition rare-earth salts, Ammonium persulfate. is adopted to substitute the rare earth confining liquid of the oxidants such as potassium permanganate and rare-earth salts composition on the other hand, this rare earth confining liquid is not only friendly to environment and human body, and can be greatly improved the decay resistance of the oxide-film after sealing treatment.(2) the oxide-film surface after the confining liquid of the present invention processes uniformly, without iris, compact structure, atresia.
Accompanying drawing explanation
Fig. 1 is the metallurgical microscope photo of 7075 aluminum alloy surface after embodiment 1 sealing treatment.
Fig. 2 is the metallurgical microscope photo of 6063 aluminum alloy surface after embodiment 6 sealing treatment.
Fig. 3 is the metallurgical microscope photo of 1060 aluminum alloy surface after embodiment 11 sealing treatment.
Detailed description of the invention
(embodiment 1)
The present embodiment is that 7075 aluminium alloys after anodic oxidation are carried out sealing treatment, and concrete grammar is as follows:
First 7075 aluminium alloys containing anode oxide film through anodic oxidation rear surface are mounted.
Then immersion 60min in the confining liquid of 50 DEG C is hung on；Consisting of of confining liquid: four cerium sulfate hydrate 5g/L, lanthanum nitrate hexahydrate 1g/L and Ammonium persulfate. 0.5g/L.
Finally 7075 aluminium alloys are taken out, wash, dry.
Fig. 1 is shown in by the metallurgical microscope photo of 7075 aluminum alloy surface after the present embodiment sealing treatment.
As seen from Figure 1: 7075 aluminum alloy surface after the present embodiment sealing treatment uniformly, without iris, compact structure, atresia.
7075 positive pole oxidation film on aluminum alloy surfaces after the present embodiment sealing treatment are carried out salt spray corrosion test and dropping corrosion test, and result is in Table 1.
Wherein salt spray corrosion test is neutral salt spray test, and condition is as follows: laboratory temperature 35 ± 1 DEG C, saturated air barrel temperature 47 ± 1 DEG C, 1 ± 0.01 normal atmosphere of air pressure, spray amount 1.0～2.0mL/80cm2/ h, sodium chloride concentration is 5wt%.
The potassium dichromate that volumetric solution is 0.6g that dropping corrosion test adopts is dissolved in the concentrated hydrochloric acid that 25mL concentration is 4mol/L.
(embodiment 2～embodiment 5)
Each embodiment is substantially the same manner as Example 1, and difference is in Table 1.
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Aluminium alloy 7075 aluminium alloys 7075 aluminium alloys 7075 aluminium alloys 7075 aluminium alloys 7075 aluminium alloys
Cerous sulfate 15g/L 5g/L 25g/L 15g/L 15g/L
Lanthanum (III) nitrate 3g/L 1g/L 5g/L 3g/L 3g/L
Ammonium persulfate. 1.5g/L 0.5g/L 2.5g/L 1.5g/L 1.5g/L
Confining liquid temperature 50℃ 50℃ 50℃ 40℃ 60℃
Soak time 60min 60min 60min 70min 50min
Salt-fog resistant time 153h 149h 151h 152h 153h
The resistance to drop time 12.56s 12.49s 12.52s 12.51s 12.53s
(embodiment 6)
The present embodiment is that 6063 aluminium alloys after anodic oxidation are carried out sealing treatment, and concrete grammar is with embodiment 1.
Fig. 2 is shown in by the metallurgical microscope photo of 6063 aluminum alloy surface after the present embodiment sealing treatment.
As seen from Figure 2: 6063 aluminum alloy surface after the present embodiment sealing treatment uniformly, without iris, compact structure, atresia.
6063 positive pole oxidation film on aluminum alloy surfaces after the present embodiment sealing treatment are carried out salt spray corrosion test and dropping corrosion test, and result is in Table 2.
(embodiment 7～embodiment 10)
Each embodiment is substantially the same manner as Example 6, and difference is in Table 2.
Table 2
Embodiment 6 Embodiment 7 Embodiment 8 Embodiment 9 Embodiment 10
Aluminium alloy 6063 aluminium alloys 6063 aluminium alloys 6063 aluminium alloys 6063 aluminium alloys 6063 aluminium alloys
Cerous sulfate 15g/L 5g/L 25g/L 15g/L 15g/L
Lanthanum (III) nitrate 3g/L 1g/L 5g/L 3g/L 3g/L
Ammonium persulfate. 1.5g/L 0.5g/L 2.5g/L 1.5g/L 1.5g/L
Confining liquid temperature 50℃ 50℃ 50℃ 40℃ 60℃
Soak time 60min 60min 60min 70min 50min
Salt-fog resistant time 150h 147h 149h 149h 150h
The resistance to drop time 12.23s 12.15s 12.19s 12.20s 12.21s
(embodiment 11)
The present embodiment is that 1060 aluminium alloys after anodic oxidation are carried out sealing treatment, and concrete grammar is with embodiment 1.
Fig. 3 is shown in by the metallurgical microscope photo of 1060 aluminum alloy surface after the present embodiment sealing treatment.
As seen from Figure 3: 1060 aluminum alloy surface after the present embodiment sealing treatment uniformly, without iris, compact structure, atresia.
1060 positive pole oxidation film on aluminum alloy surfaces after the present embodiment sealing treatment are carried out salt spray corrosion test and dropping corrosion test, and result is in Table 3.
(embodiment 12～embodiment 15)
Each embodiment is substantially the same manner as Example 11, and difference is in Table 3.
Table 3
Embodiment 11 Embodiment 12 Embodiment 13 Embodiment 14 Embodiment 15
Aluminium alloy 1060 aluminium alloys 1060 aluminium alloys 1060 aluminium alloys 1060 aluminium alloys 1060 aluminium alloys
Cerous sulfate 15g/L 5g/L 25g/L 15g/L 15g/L
Lanthanum (III) nitrate 3g/L 1g/L 5g/L 3g/L 3g/L
Ammonium persulfate. 1.5g/L 0.5g/L 2.5g/L 1.5g/L 1.5g/L
Confining liquid temperature 50℃ 50℃ 50℃ 40℃ 60℃
Soak time 60min 60min 60min 70min 50min
Salt-fog resistant time 151h 148h 149h 150h 151h
The resistance to drop time 12.35s 12.27s 12.29s 12.30s 12.32s
(comparative example 1～comparative example 5)
Each comparative example is substantially the same manner as Example 6, is different in that the composition of confining liquid, is specifically shown in table 4.
6063 positive pole oxidation film on aluminum alloy surfaces after each comparative example sealing treatment are carried out salt spray corrosion test and dropping corrosion test, and result is still in Table 4.
Table 4
Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5
Aluminium alloy 6063 aluminium alloys 6063 aluminium alloys 6063 aluminium alloys 6063 aluminium alloys 6063 aluminium alloys
Cerous nitrate - 15g/L - 15g/L 17g/L
Cerous sulfate 15g/L - 15g/L - -
Lanthanum (III) nitrate - 3g/L 3g/L 3g/L -
Ammonium persulfate. 1.5g/L 1.5g/L - - -
Potassium permanganate - - 1.5g/L 1.5g/L 0.6g/L
Potassium pyrophosphate - - - - 0.27g/L
Salt-fog resistant time 137h 140h 132h 120h 116h
The resistance to drop time 11.12s 11.21s 11.08s 10.85s 10.59s
Wherein comparative example 5 is the confining liquid of Chinese patent literature CN102650068A embodiment 1.
As can be seen from Table 4: the decay resistance of 6063 positive pole oxidation film on aluminum alloy surfaces after each comparative example sealing treatment is all undesirable, especially comparative example 4 and comparative example 5.

Claims (7)

1. the sealing treatment method in aluminum alloy surface process, is placed in the aluminium alloy after surface treated in confining liquid and soaks, and washes, dries after taking-up；It is characterized in that: described confining liquid is made up of the component of following concentration: four cerium sulfate hydrate 5～25g/L, lanthanum nitrate hexahydrate 1～5g/L, Ammonium persulfate. 0.5～2.5g/L.
2. the sealing treatment method in aluminum alloy surface according to claim 1 process, it is characterised in that: described confining liquid is made up of the component of following concentration: four cerium sulfate hydrate 15g/L, lanthanum nitrate hexahydrate 3g/L, Ammonium persulfate. 1.5g/L.
3. the sealing treatment method in aluminum alloy surface according to claim 1 and 2 process, it is characterised in that: the time of described immersion is 50～70min, and confining liquid temperature is 40～60 DEG C.
4. the sealing treatment method in aluminum alloy surface according to claim 3 process, it is characterised in that: described surface treatment is anodic oxidation or chemical oxidation.
5. the sealing treatment method in aluminum alloy surface according to claim 1 and 2 process, it is characterised in that: described surface treatment is anodic oxidation or chemical oxidation.
6. the confining liquid that the sealing treatment method in an aluminum alloy surface process adopts, it is characterised in that be made up of the component of following concentration: four cerium sulfate hydrate 5～25g/L, lanthanum nitrate hexahydrate 1～5g/L, Ammonium persulfate. 0.5～2.5g/L.
7. the confining liquid that the sealing treatment method in aluminum alloy surface according to claim 6 process adopts, it is characterised in that be made up of the component of following concentration: four cerium sulfate hydrate 15g/L, lanthanum nitrate hexahydrate 3g/L, Ammonium persulfate. 1.5g/L.
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