CN108166037A - A kind of anodized technique for controlling aluminium material surface oxidation film dusting - Google Patents

A kind of anodized technique for controlling aluminium material surface oxidation film dusting Download PDF

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Publication number
CN108166037A
CN108166037A CN201810021951.5A CN201810021951A CN108166037A CN 108166037 A CN108166037 A CN 108166037A CN 201810021951 A CN201810021951 A CN 201810021951A CN 108166037 A CN108166037 A CN 108166037A
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aluminium
anodized
material surface
solution
temperature
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Inventor
郭振武
高崇
方小明
江钟宇
黄瑞银
赵丕植
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China Aluminum Material Applied Research Institute Co Ltd
Chinalco Ruimin Co Ltd
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China Aluminum Material Applied Research Institute Co Ltd
Chinalco Ruimin Co Ltd
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Priority to CN201810021951.5A priority Critical patent/CN108166037A/en
Publication of CN108166037A publication Critical patent/CN108166037A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08Alloys based on aluminium with magnesium as the next major constituent with silicon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Printing Plates And Materials Therefor (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Manufacture Of Electron Tubes, Discharge Lamp Vessels, Lead-In Wires, And The Like (AREA)

Abstract

The invention discloses a kind of anodized techniques for controlling aluminium material surface oxidation film dusting, belong to technical field of alloy.Before anodized, then aluminium is carrying out anodized, using current constant control, current density is controlled in 1.0 ~ 2.5A/dm by alkali cleaning, pickling and chemical polishing processing by electrolyte of certain density sulfuric acid2, anodizing temperature is 18 ~ 20 DEG C, and anodizing time is 20 40min, and the film thickness after anodized is 3 ~ 20 μm, and thickness distribution is uniform(1.0 μm of standard deviation <).To the oxidation film colour and sealing pores, aluminium material surface is without powder phenomenon-tion.

Description

A kind of anodized technique for controlling aluminium material surface oxidation film dusting
Technical field
The invention belongs to technical field of alloy, and in particular at a kind of anodic oxidation for controlling aluminium material surface oxidation film dusting Science and engineering skill.
Background technology
Aluminium alloy passes through anodized, and multiple color can be presented in appearance, in automotive interior part, curtain wall decoration Material and consumption electronic product constructional appearance part application prospect are huge.But after anodized, aluminium material surface generation pollen Claim " dusting ", wipe rear reproducible pollen away with wet cloth, influence aluminium material surface aesthetics, seriously constrain anodization aluminium high-end The extensive use of industrial circle.Therefore, there is an urgent need for a kind of anodized techniques for controlling aluminium material surface oxidation film dusting.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of sun for controlling aluminium material surface oxidation film dusting Pole oxidation processing technique.The present invention keeps away surface by anodized process control aluminium material surface coating mass Exempt to generate powder phenomenon-tion, aluminium appearance uniformity is excellent, and this method is generally applicable in anodization aluminium, industrial easily real It is existing.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of anodized technique for controlling aluminium material surface oxidation film dusting, specifically comprises the following steps:
(1)Alkali cleaning is handled:Aluminium is immersed into NaOH solution, removes the oxidation film of the aluminium matrix surface self-assembling formation;
(2)Pickling processes:It will be through step(1)Alkali cleaning treated aluminium immerses HNO3Solution removes the aluminium alkali cleaning surface Residue;
(3)Chemical polishing is handled:It will be through step(2)Aluminium after pickling processes immerses mixed acid solution, makes aluminium material surface smooth, The composition of the mixed acid solution is:Phosphoric acid and sulfuric acid are 4 by volume:1 mixing;
(4)Pickling processes again:It will be through step(3)The aluminium of chemical polishing processing immerses HNO3Solution removes the aluminium Optical polishing handles surface residue;
(5)Anodized:It will be through step(4)The aluminium of pickling processes, which is placed in electrolyte, carries out anodized, work Skill state modulator is:Anodizing temperature is 18 ~ 20 DEG C, anodizing time 20-40min, current constant control current density model Enclose 1.0 ~ 2.5A/dm2, associated voltage 8 ~ 15V of range, the film thickness after anodized is 3 ~ 20 μm;
(6)Dyeing is handled:By step(5)Aluminium after anodized immerses staining solution, and dyeing temperature is 20 DEG C, is impregnated Time is 1-3min;
(7)Sealing of hole and drying and processing:By step(6)Aluminium after dyeing, which is immersed in the solution containing high temperature hole sealing agent, carries out sealing of hole Processing, the pH value of solution is 5 ~ 6, then carries out drying and processing, and drying temperature is 90 DEG C, and drying time is more than 1min.
The aluminium includes following component by mass percentage:Mg:2.3wt.%~4.8wt.%;Cu:≤ 0.05wt.%;Mn:0.01 wt.%~ 0.05wt.%;Cr:≤0.05wt.%;Si:≤0.08 wt.%;Fe:≤0.10 wt.%; Surplus is Al.
The step(1)Alkali cleaning processing technological parameter be:Alkali cleaning temperature is 65 DEG C, soaking time 10-20s, A concentration of 70-90g/L of NaOH solution.
The step(2)And step(4)The technological parameters of pickling processes be:Pickling temperature is 25 DEG C, and soaking time is 10-20s, HNO3A concentration of 180-220g/L of solution.
The step(3)Chemical polishing processing technological parameter be:The temperature that aluminium impregnates in mixed acid is 100 DEG C, soaking time 40-60s.
The step(5)Anodized used in electrolyte be 150-220g/L sulfuric acid solution.
Aluminium material surface powder phenomenon-tion Producing reason after anodized and anodic process be closely related and aluminium sheet Body characteristic influences little.Using under high current density condition, the coating mass of preparation is excessively poor, using Fischer FMP30 eddy current thickness meters test the thickness of oxidation film, find the inhomogeneities of thickness and its distribution(Standard deviation)It dramatically increases, table Face powder phenomenon-tion is serious;It is seen by Hitachi S4700 types field emission scanning electron microscope, finds high current densities Lower obtained oxidation film, on microcosmic easily layering come off, fragmentation, macroscopically showing as pollen phenomenon.Dusting(Pollen)Phenomenon It is mainly anodization temperature overheating to generate, and current density is excessively high, oxide growth degradation caused by anode overlong time, thick Degree, which is unevenly distributed, to be dramatically increased.It can be with by regulating and controlling the parameters such as the temperature in anodizing process, current density and anode time Control powder phenomenon-tion.
The beneficial effects of the present invention are:
1st, the oxidation layer surface that the present invention can be such that aluminium is formed after anodized does not generate powder phenomenon-tion, aluminium appearance Excellent in uniform;
2nd, the present invention be by anodized process control aluminium material surface coating mass, and then make surface avoid generate powder Change phenomenon, this method is generally applicable in anodization aluminium, industrial easy to implement.
Description of the drawings
Fig. 1 is photo after aluminium material surface photo after 1 Anodic Oxidation of embodiment and its dyeing sealing pores;
Fig. 2 is aluminium material surface high magnification scanning electron microscopic picture after 1 Anodic Oxidation of embodiment;
Fig. 3 is photo after aluminium material surface photo after 2 Anodic Oxidation of embodiment and its dyeing sealing pores;
Fig. 4 is photo after aluminium material surface photo after 1 Anodic Oxidation of comparative example and its dyeing sealing pores;
Fig. 5 is photo after aluminium material surface photo after 2 Anodic Oxidation of comparative example and its dyeing sealing pores;
Fig. 6 is aluminium material surface high magnification scanning electron microscopic picture after 2 Anodic Oxidation of comparative example;
Fig. 7 is photo after aluminium dyeing sealing pores after 3 Anodic Oxidation of comparative example.
Specific embodiment
Hereinafter, the present invention is described in further detail by way of embodiment and comparative example.It should be noted that with Lower embodiment only illustrates several embodiments of the present invention, and the present invention is not limited to following embodiments.
Embodiment 1
(1)Alkali cleaning is handled:Aluminium is immersed to the NaOH solution of 70g/L, removes the oxidation of the aluminium matrix surface self-assembling formation Film, alkali cleaning temperature are 65 DEG C, soaking time 15s;
(2)Pickling processes:Aluminium is immersed to the HNO of 180g/L3Solution removes the aluminium alkali cleaning surface residue, pickling temperature It is 25 DEG C to spend, soaking time 10s;
(3)Chemical polishing is handled:Aluminium is immersed into mixed acid(Phosphoric acid:Sulfuric acid=4:1(Volume ratio))Solution puts down aluminium material surface Whole, temperature is 100 DEG C, soaking time 50s;
(4)Pickling processes again:Aluminium is immersed to the HNO of 200g/L3Solution removes the aluminiumization and throws processing remained on surface Object, pickling temperature are 25 DEG C, soaking time 10s;
(5)Anodized:Aluminium is placed in electrolyte and carries out anodized, electrolyte is that the sulfuric acid of 200g/L is molten Liquid, anodizing temperature are 20 DEG C, anodizing time 30min, current constant control current density 1.2A/dm2, associated voltage 8V;
(6)Dyeing is handled:Aluminium after anodic oxidation is immersed into staining solution, temperature is 20 DEG C, soaking time 1min;
(7)Sealing of hole and drying and processing:Aluminium immersion after dyeing is had to the solution of high temperature hole sealing agent, solution ph 6, drying temperature 90 DEG C of degree, drying time are more than 1min.
Aluminium material surface oxide thickness obtained by the anodic process is 3 μm, and standard deviation is 0.51 μm, and surface is without powder phenomenon-tion It generates.The surface of the embodiment is illustrated in Fig. 1, and the scanning electron microscope of the embodiment is illustrated in Fig. 2.
Embodiment 2
(1)Alkali cleaning is handled:Aluminium is immersed to the NaOH solution of 70g/L, removes the oxidation of the aluminium matrix surface self-assembling formation Film, alkali cleaning temperature are 65 DEG C, soaking time 15s;
(2)Pickling processes:Aluminium is immersed to the HNO of 180g/L3Solution removes the aluminium alkali cleaning surface residue, pickling temperature It is 25 DEG C to spend, soaking time 10s;
(3)Chemical polishing is handled:Aluminium is immersed into mixed acid(Phosphoric acid:Sulfuric acid=4:1(Volume ratio))Solution puts down aluminium material surface Whole, temperature is 100 DEG C, soaking time 50s;
(4)Pickling processes again:Aluminium is immersed to the HNO of 200g/L3Solution removes the aluminiumization and throws processing remained on surface Object, pickling temperature are 25 DEG C, soaking time 10s;
(5)Anodized:Aluminium is placed in electrolyte and carries out anodized, electrolyte is that the sulfuric acid of 220g/L is molten Liquid, anodizing temperature are 18 DEG C, anodizing time 30min, current constant control current density 1.9A/dm2, associated voltage 10V;
(6)Dyeing is handled:Aluminium after anodic oxidation is immersed into staining solution, temperature is 20 DEG C, soaking time 3min;
(7)Sealing of hole and drying and processing:Aluminium immersion after dyeing is had to the solution of high temperature hole sealing agent, solution ph 6, drying temperature 90 DEG C of degree, drying time are more than 1min.
Aluminium material surface oxide thickness obtained by the anodic process is 10 μm, and standard deviation is 0.44 μm, and surface shows without dusting As generating.The surface of the embodiment is illustrated in Fig. 3.
Comparative example 1
(1)Alkali cleaning is handled:Aluminium is immersed to the NaOH solution of 70g/L, removes the oxidation of the aluminium matrix surface self-assembling formation Film, alkali cleaning temperature are 65 DEG C, soaking time 15s;
(2)Pickling processes:Aluminium is immersed to the HNO of 180g/L3Solution removes the aluminium alkali cleaning surface residue, pickling temperature It is 25 DEG C to spend, soaking time 10s;
(3)Chemical polishing is handled:Aluminium is immersed into mixed acid(Phosphoric acid:Sulfuric acid=4:1(Volume ratio))Solution puts down aluminium material surface Whole, temperature is 100 DEG C, soaking time 50s;
(4)Pickling processes again:Aluminium is immersed to the HNO of 200g/L3Solution removes the aluminiumization and throws processing remained on surface Object, pickling temperature are 25 DEG C, soaking time 10s;
(5)Anodized:Aluminium is placed in electrolyte and carries out anodized, electrolyte is that the sulfuric acid of 200g/L is molten Liquid, anodizing temperature are 18 DEG C, anodizing time 30min, current constant control current density 15A/dm2, associated voltage 15V;
(6)Dyeing is handled:Aluminium after anodic oxidation is immersed into staining solution, temperature is 20 DEG C, soaking time 3min;
(7)Sealing of hole and drying and processing:Aluminium immersion after dyeing is had to the solution of high temperature hole sealing agent, solution ph 6, drying temperature 90 DEG C of degree, drying time are more than 1min.
Aluminium material surface oxide thickness obtained by the anodic process is 31 μm, and standard deviation is 1.13 μm, and surface generates part Powder phenomenon-tion.The surface of the comparative example is illustrated in Fig. 4.
Comparative example 2
(1)Alkali cleaning is handled:Aluminium is immersed to the NaOH solution of 70g/L, removes the oxidation of the aluminium matrix surface self-assembling formation Film, alkali cleaning temperature are 65 DEG C, soaking time 15s;
(2)Pickling processes:Aluminium is immersed to the HNO of 180g/L3Solution removes the aluminium alkali cleaning surface residue, pickling temperature It is 25 DEG C to spend, soaking time 10s;
(3)Chemical polishing is handled:Aluminium is immersed into mixed acid(Phosphoric acid:Sulfuric acid=4:1(Volume ratio))Solution puts down aluminium material surface Whole, temperature is 100 DEG C, soaking time 50s;
(4)Pickling processes again:Aluminium is immersed to the HNO3 solution of 200g/L, the aluminiumization is removed and throws processing remained on surface Object, pickling temperature are 25 DEG C, soaking time 10s;
(5)Anodized:Aluminium is placed in electrolyte and carries out anodized, electrolyte is that the sulfuric acid of 200g/L is molten Liquid, anodizing temperature are 20 DEG C, anodizing time 30min, current constant control current density 40A/dm2, associated voltage 16V;
(6)Dyeing is handled:Aluminium after anodic oxidation is immersed into staining solution, temperature is 20 DEG C, soaking time 1min;
(7)Sealing of hole and drying and processing:Aluminium immersion after dyeing is had to the solution of high temperature hole sealing agent, solution ph 6, drying temperature 90 DEG C of degree, drying time are more than 2min.
Aluminium material surface oxide thickness obtained by the anodic process is 18 μm, and standard deviation is 2.33 μm, and surface generates whole face Powder phenomenon-tion.The surface of the comparative example is illustrated in Fig. 5, and the scanning electron microscope of the comparative example is illustrated in Fig. 6.
Comparative example 3
(1)Alkali cleaning is handled:Aluminium is immersed to the NaOH solution of 70g/L, removes the oxidation of the aluminium matrix surface self-assembling formation Film, alkali cleaning temperature are 65 DEG C, soaking time 15s;
(2)Pickling processes:Aluminium is immersed to the HNO of 180g/L3Solution removes the aluminium alkali cleaning surface residue, pickling temperature It is 25 DEG C to spend, soaking time 10s;
(3)Chemical polishing is handled:Aluminium is immersed into mixed acid(Phosphoric acid:Sulfuric acid=4:1(Volume ratio))Solution puts down aluminium material surface Whole, temperature is 100 DEG C, soaking time 50s;
(4)Pickling processes again:Aluminium is immersed to the HNO of 200g/L3Solution removes the aluminiumization and throws processing remained on surface Object, pickling temperature are 25 DEG C, soaking time 10s;
(5)Anodized:Aluminium is placed in electrolyte and carries out anodized, electrolyte is that the sulfuric acid of 220g/L is molten Liquid, anodizing temperature are 35 DEG C, anodizing time 30min, current constant control current density range 1.2A/dm2, associated voltage Range 8V;
(6)Dyeing is handled:Aluminium after anodic oxidation is immersed into staining solution, temperature is 20 DEG C, soaking time 1min;
(7)Sealing of hole and drying and processing:Aluminium immersion after dyeing is had to the solution of high temperature hole sealing agent, solution ph 6, drying temperature 90 DEG C of degree, drying time are more than 3min.
Aluminium material surface oxide thickness obtained by the anodic process is 11 μm, and standard deviation is 2.08 μm, and surface generates whole face Powder phenomenon-tion.The surface of the comparative example is illustrated in Fig. 7.
In conclusion the aluminium of 1 ~ 3 Anodic Oxidation process of comparative example, there is different degrees of dusting and shows in surface ;The aluminium of 1 ~ 2 Anodic Oxidation process of the embodiment of the present invention, surface does not generate powder phenomenon-tion.With prior art phase Than whether anode oxidation process provided by the invention, controllable aluminium material surface generates powder phenomenon-tion with dusting degree.
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the common skill of fields Art personnel, which should be appreciated that, can be modified or replaced equivalently the specific embodiment of the present invention with reference to above-described embodiment, These without departing from spirit and scope of the invention any modification or wait.

Claims (7)

1. a kind of anodized technique for controlling aluminium material surface oxidation film dusting, it is characterised in that:Specifically include following step Suddenly:
(1)Alkali cleaning is handled:Aluminium is immersed into NaOH solution, removes the oxidation film of the aluminium matrix surface self-assembling formation;
(2)Pickling processes:It will be through step(1)Alkali cleaning treated aluminium immerses HNO3It is residual to remove the aluminium alkali cleaning surface for solution Stay object;
(3)Chemical polishing is handled:It will be through step(2)Aluminium after pickling processes immerses mixed acid solution, makes aluminium material surface smooth, The composition of the mixed acid solution is:Phosphoric acid and sulfuric acid are 4 by volume:1 mixing;
(4)Pickling processes again:It will be through step(3)The aluminium of chemical polishing processing immerses HNO3Solution removes the aluminium chemistry Polishing surface residue;
(5)Anodized:It will be through step(4)The aluminium of pickling processes, which is placed in electrolyte, carries out anodized, work Skill state modulator is:Anodizing temperature is 18 ~ 20 DEG C, anodizing time 20-40min, current constant control current density model Enclose 1.0 ~ 2.5A/dm2, associated voltage 8 ~ 15V of range, the film thickness after anodized is 3 ~ 20 μm;
(6)Dyeing is handled:By step(5)Aluminium after anodized immerses staining solution, and dyeing temperature is 20 DEG C, is impregnated Time is 1-3min;
(7)Sealing of hole and drying and processing:By step(6)Aluminium after dyeing, which is immersed in the solution containing high temperature hole sealing agent, carries out sealing of hole Processing, the pH value of solution is 5 ~ 6, then carries out drying and processing, and drying temperature is 90 DEG C, and drying time is more than 1min.
2. the anodized technique of control aluminium material surface oxidation film dusting according to claim 1, feature exist In:The aluminium includes following component by mass percentage:Mg:2.3wt.%~4.8wt.%;Cu:≤0.05wt.%;Mn: 0.01 wt.%~ 0.05wt.%;Cr:≤0.05wt.%;Si:≤0.08 wt.%;Fe:≤0.10 wt.%;Surplus is Al.
3. the anodized technique of control aluminium material surface oxidation film dusting according to claim 1, it is characterised in that: The step(1)Alkali cleaning processing technological parameter be:Alkali cleaning temperature is 65 DEG C, soaking time 10-20s, NaOH solution A concentration of 70-90g/L.
4. the anodized technique of control aluminium material surface oxidation film dusting according to claim 1, it is characterised in that: The step(2)And step(4)The technological parameters of pickling processes be:Pickling temperature is 25 DEG C, soaking time 10-20s, HNO3A concentration of 180-220g/L of solution.
5. the anodized technique of control aluminium material surface oxidation film dusting according to claim 1, it is characterised in that: The step(3)Chemical polishing processing technological parameter be:The temperature that aluminium impregnates in mixed acid is 100 DEG C, during immersion Between be 40-60s.
6. the anodized technique of control aluminium material surface oxidation film dusting according to claim 1, feature exist In:The step(5)Anodized used in electrolyte be 150-220g/L sulfuric acid solution.
7. the anodized technique of control aluminium material surface oxidation film dusting according to claim 1, feature exist In:The step(5)Anode oxide film thickness distribution it is uniform, 1.0 μm of standard deviation <.
CN201810021951.5A 2018-01-10 2018-01-10 A kind of anodized technique for controlling aluminium material surface oxidation film dusting Pending CN108166037A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110396695A (en) * 2019-08-15 2019-11-01 成都亚佳工程新技术开发有限公司 A kind of method of the aluminising of air-guide handrail, anodic oxidation and coloring

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101676439A (en) * 2008-09-18 2010-03-24 浙江帝龙新材料股份有限公司 Aluminum strip continuous anodic oxidation automatic production line
CN104762538A (en) * 2015-04-09 2015-07-08 广东欧珀移动通信有限公司 Aluminum alloy and anodic oxidation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101676439A (en) * 2008-09-18 2010-03-24 浙江帝龙新材料股份有限公司 Aluminum strip continuous anodic oxidation automatic production line
CN104762538A (en) * 2015-04-09 2015-07-08 广东欧珀移动通信有限公司 Aluminum alloy and anodic oxidation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110396695A (en) * 2019-08-15 2019-11-01 成都亚佳工程新技术开发有限公司 A kind of method of the aluminising of air-guide handrail, anodic oxidation and coloring

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