CN102560516A - Magnesium alloy surface homogenization pretreatment process - Google Patents

Magnesium alloy surface homogenization pretreatment process Download PDF

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Publication number
CN102560516A
CN102560516A CN2012100318320A CN201210031832A CN102560516A CN 102560516 A CN102560516 A CN 102560516A CN 2012100318320 A CN2012100318320 A CN 2012100318320A CN 201210031832 A CN201210031832 A CN 201210031832A CN 102560516 A CN102560516 A CN 102560516A
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alloy surface
magnesiumalloy
alkaline
magnesium alloy
liquid
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CN102560516B (en
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杨海燕
郭兴伍
吴国华
丁文江
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Shanghai Jiaotong University
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    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/22—Light metals
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/12—Light metals

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention discloses a magnesium alloy surface homogenization pretreatment process, comprising the steps of: a, polishing: polishing grease, oxide coatings, corrosion products and corners on the surface of a magnesium alloy so that the surface of the magnesium alloy is clean and fresh; b, alkaline degreasing treatment: preparing an alkaline degreasing solution, putting the polished magnesium alloy into the alkaline degreasing solution, and moderately stirring at a temperature of 65-80 DEG C for 5-10min; c, acidic activation treatment: preparing an acidic activation solution, putting the magnesium alloy after the alkaline degreasing treatment into the acidic activation solution, and moderately stirring at room temperature for 30-60s; and d, alkaline adjustment: preparing an alkaline adjustment solution, putting the magnesium alloy after the acidic activation treatment into the alkaline adjustment solution, and moderately stirring at a temperature of 65-80 DEG C for 5-30min, wherein the magnesium alloy is cleaned through running water for 3min between each two steps. Through the process disclosed by the invention, the problem of unevenness of surface chemical compositions and electrochemistry of the magnesium alloy is solved, the obtained surface films are more even and compact, and the protective performance of the film is greatly improved.

Description

Mg alloy surface homogenizing pre-treating technology
Technical field
The present invention relates to metallic surface and handle particularly a kind of Mg alloy surface homogenizing pre-treating technology.
Background technology
Magnesiumalloy is because to have density low, and casting that specific tenacity, specific rigidity are high and good and machinability etc. have a wide range of applications in fields such as aerospace, telecommunications, automobile making, defence and militaries.But erosion resistance and wear resisting property difference have restricted the widespread use of magnesiumalloy.It is a kind of economy, quick and easy its corrosion resistance nature of raising and the method for wear resisting property that magnesiumalloy is carried out surface treatment.
Science and technology is looked into new and patent search result shows, magnesiumalloy is carried out surface treatment, and at present most widely used is anodic oxidation, chemical conversion, electroless plating and electroplating technology.The key of magnesium alloy surface treatment is the magnesiumalloy pre-treating technology.If pre-treating technology is suitable, in case after Mg alloy surface has successfully formed bottom, just can form rete at Mg alloy surface with property, to be suitable for various Service Environment.Yet magnesiumalloy is polyphase structure often, and this makes that magnesiumalloy all is uneven on chemical ingredients and electrochemistry; Matrix and the very big potential difference of the second alternate existence, when magnesiumalloy places treatment solution, different meeting shows different electrochemical behaviors; Two alternately also galvanic corrosion can take place; The rete that causes forming is each alternate there are differences, and the protection rete of Mg alloy surface is generally the cathodic rete, in case partial failure is arranged; This will speed up the corrosion of magnesium alloy substrate, and this is also poorer than there not being protective layer.For example, AZ91D is a typical duplex structure magnesiumalloy, the matrix phase α-Mg and the second β phase (Mg mutually 17Al 12) between have potential difference, when AZ91D being soaked Zn and handle, often be difficult to obtain satisfied effect, second obtain on mutually loose often, bonding force is poor, discontinuous Zn layer; On the AZ91D magnesiumalloy during chemical plating Mi-P alloy; Ni-P preferentially goes up forming core at the second phase β mutually, but after the Ni-P alloy mainly grow in that α-Mg is last, defectives such as pin hole mainly accumulate in the second phase β phase; In a single day corrosion takes place from here on, will speed up the corrosion of magnesium alloy substrate.Equally, anode oxide film, the formation of chemical conversion film also receives the influence of matrix second phase.
Therefore; People have carried out big quantity research to the magnesiumalloy pre-treatment; At present be: polishing → alkaline degreasing → chromic acid pickling → hydrofluoric acid activation to the most frequently used pre-treating process of magnesiumalloy; Purpose is to remove the Mg alloy surface grease, in the time of oxide compound and oxyhydroxide, forms the fine and close MgF of one deck at Mg alloy surface 2Film both can provide protective effect to magnesiumalloy in subsequent disposal liquid, make the current potential of Mg alloy surface more even simultaneously.But chromic acid, hydrofluoric acid are very big to environmental hazard, and MgF 2The influence that film can not avoid the second phase intermetallic compound that subsequent film is formed fully.
Summary of the invention
The object of the invention is exactly in order to provide a kind of Mg alloy surface homogenizing pre-treating technology, to remove the Mg alloy surface second phase intermetallic compound, for magnesiumalloy provides a chemical ingredients and the uniform preplating of electrochemistry surface.
To achieve these goals, the present invention has adopted following technical scheme: a kind of Mg alloy surface homogenizing pre-treating technology, and said magnesiumalloy is the Mg-Al alloy; May further comprise the steps:
A, polishing are polished to grease, oxide debris and corrosion product, the corner of Mg alloy surface, obtain clean fresh Mg alloy surface;
B, alkaline degreasing are handled, and preparation alkaline degreasing liquid places alkaline degreasing liquid with the clean magnesiumalloy of polishing, handle 5-10min, moderate agitation down at 65-80 ℃;
Acid activation solution is prepared in c, acidic activated processing, and the magnesiumalloy that will pass through the alkaline degreasing processing places acidic activated liquid, at room temperature handles 30-60s, moderate agitation;
D, alkalescence adjustment are handled, the preparation alkaline adjustment liquid, and the magnesiumalloy that will pass through acidic activated processing places alkaline adjustment liquid, handles 5-30min, moderate agitation down at 65-80 ℃;
Adopt flowing water to wash 3min in magnesiumalloy between above-mentioned each step.
Alkaline degreasing liquid described in the step b is by the formulated aqueous solution of sodium hydroxide, sodium phosphate, yellow soda ash and tensio-active agent; Wherein concentration sodium hydroxide is 30-60g/L; The concentration of sodium phosphate is 5-15g/L; The concentration of yellow soda ash is 1-5g/L, and surfactant concentrations is 10-80mg/L.
Described tensio-active agent is selected from one or both in sodium laurylsulfonate, the perfluoro octyl sulfonic acid tetraethyl-amine.
Acidic activated liquid described in the step c is by one or more the formulated aqueous solution in phosphoric acid, SODIUMNITRATE or the Hydrocerol A, and wherein concentration of phosphoric acid is 5-200mL/L, and the concentration of SODIUMNITRATE is 5-10g/L, and the concentration of Hydrocerol A is 50-100g/L.
Alkaline adjustment liquid described in the steps d is the aqueous solution of sodium hydroxide, and concentration sodium hydroxide is 50-200g/L.
The present invention is directed to the present situation of present magnesiumalloy pre-treating technology and the problem of existence; Adopt environmental protection; Cost is low, and pre-treating technology easy and simple to handle is removed Mg alloy surface second phase constitution; For the preplating magnesiumalloy obtains a chemical ingredients and the uniform condition of surface of electrochemistry, and have following advantage and characteristics:
1, environmental protection, cost is low, and is easy to operate;
2, remove Mg alloy surface second phase constitution fully, obtain chemical ingredients and the uniform preplating of electrochemistry surface, remove the disadvantageous effect that the second relative subsequent film forms at Mg alloy surface;
3, suitability is wide, can combine existing sophisticated surface treatment method, and the rete that obtains is more even, densification, and barrier propterty improves greatly.
Description of drawings
Fig. 1, Fig. 2 are AZ91D Mg alloy surface back scattering SEM figure: wherein, Fig. 1 is for before handling, and Fig. 2 is for after handling;
Fig. 3, Fig. 4 are AM-lite Mg alloy surface back scattering SEM figure: wherein, Fig. 3 is for before handling, and Fig. 4 is for after handling;
Fig. 5 is that the AZ91D magnesium alloy surface chemical after handling through pre-treating technology of the present invention soaks the Zn layer;
Fig. 6 is the AZ91D magnesium alloy surface chemical plating Ni-P layer after handling through pre-treating technology of the present invention.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
Embodiment one:
A kind of AZ91D Mg alloy surface homogenizing pre-treating technology, the AZ91D Mg alloy surface back scattering SEM figure before handling is as shown in Figure 1.Comprise following steps:
1, magnesiumalloy is polished to 1200#;
2, alkaline degreasing is handled: preparation alkaline degreasing liquid, comprise sodium hydroxide 60g/L in this liquid, and sodium phosphate 10g/L, yellow soda ash 5g/L, tensio-active agent 30mg/L, surplus is a water.Wherein tensio-active agent is a sodium laurylsulfonate.Water is zero(ppm) water or deionized water; Alkaline degreasing liquid is heated to 65 ℃, the magnesiumalloy of polishing is put into alkaline degreasing wash 8min, moderate agitation;
3, acid activation solution is prepared in acidic activated processing, comprises Hydrocerol A 100g/L in this liquid, and surplus is a water, and water is zero(ppm) water or deionized water, and the magnesiumalloy that will pass through alkaline degreasing is put into acidic activated liquid and washed 30s, and treatment temp is a room temperature, moderate agitation;
4, alkalescence adjustment is handled, and the preparation alkaline adjustment liquid comprises sodium hydroxide 200g/L in this liquid, and surplus is a water, and alkaline adjustment liquid is heated to 65 ℃, will pass through magnesiumalloy after acid-wash activation is handled and put into alkaline adjustment liquid and wash 5min, moderate agitation;
Adopt flowing water to wash 3min between each step.
Analyze through SEM and EDXS, through the AZ91D Mg alloy surface second phase Mg of above-mentioned processing 17Al 12Be removed, surface composition is even, and the AZ91D Mg alloy surface back scattering SEM figure after the processing is as shown in Figure 2.To soak Zn to the magnesiumalloy through above-mentioned processing and handle, the Zn layer that obtains is even, densification, and fraction of coverage is high, and is as shown in Figure 5.
Embodiment two:
A kind of AM-lite Mg alloy surface homogenizing pre-treating technology, the AM-lite Mg alloy surface back scattering SEM figure before handling is as shown in Figure 3.Comprise following steps:
1, magnesiumalloy is polished to 1200#;
2, alkaline degreasing is handled: preparation alkaline degreasing liquid, comprise sodium hydroxide 50g/L in this liquid, and sodium phosphate 8g/L, yellow soda ash 5g/L, tensio-active agent 10mg/L, surplus is a water.Wherein tensio-active agent is a perfluoro octyl sulfonic acid tetraethyl-amine.Water is zero(ppm) water or deionized water; Alkaline degreasing liquid is heated to 65 ℃, the magnesiumalloy of polishing is put into alkaline degreasing wash 5min, moderate agitation;
3, acid activation solution is prepared in acidic activated processing, comprises phosphoric acid 5ml/L in this liquid; SODIUMNITRATE 10g/L, surplus is a water, water is zero(ppm) water or deionized water; The magnesiumalloy that will pass through alkaline degreasing is put into pickle solution and is washed 60s, and treatment temp is a room temperature, moderate agitation;
4, the alkalescence adjustment is handled, and the preparation alkaline adjustment liquid comprises sodium hydroxide 50g/L in this liquid, and surplus is a water; Alkaline adjustment liquid is heated to 70 ℃, and the magnesiumalloy after will passing through acid-wash activation and handling is put into alkaline adjustment liquid and is washed 5min, moderate agitation;
Adopt flowing water to wash 3min between each step.
Analyze through SEM and EDXS, the AM-lite Mg alloy surface second of the above-mentioned processing of process is removed mutually, and surface composition is even, and the AM-lite Mg alloy surface back scattering SEM figure after the processing is as shown in Figure 4.To carry out chemical conversion to the magnesiumalloy through above-mentioned processing and handle, the chemical conversion rete that obtains is even, densification, and barrier propterty improves.
Embodiment three:
A kind of AZ91D Mg alloy surface homogenizing pre-treating technology comprises following steps:
1, magnesiumalloy is polished to 1200#;
2, alkaline degreasing is handled: preparation alkaline degreasing liquid, comprise sodium hydroxide 60g/L in this liquid, and sodium phosphate 10g/L, yellow soda ash 5g/L, tensio-active agent 10mg/L, surplus is a water.Wherein tensio-active agent is a perfluoro octyl sulfonic acid tetraethyl-amine, and water is zero(ppm) water or deionized water; Alkaline degreasing liquid is heated to 70 ℃, the magnesiumalloy of polishing is put into alkaline degreasing wash 8min, moderate agitation;
3, acid activation solution is prepared in acidic activated processing, comprises Hydrocerol A 100g/L in this liquid, and surplus is a water, and water is zero(ppm) water or deionized water, and the magnesiumalloy that will pass through alkaline degreasing is put into pickle solution and washed 45s, and treatment temp is a room temperature, moderate agitation;
4, the alkalescence adjustment is handled, and the preparation alkaline adjustment liquid comprises sodium hydroxide 100g/L in this liquid, and surplus is a water; Alkaline adjustment liquid is heated to 70 ℃, and the magnesiumalloy after will passing through acid-wash activation and handling is put into alkaline adjustment liquid and is washed 30min, moderate agitation;
Adopt flowing water to wash 3min between each step.
Analyze through SEM and EDXS, through the AZ91D Mg alloy surface second phase Mg of above-mentioned processing 17Al 12Be removed, surface composition is even.To carry out chemical Ni-P plating to the magnesiumalloy through above-mentioned processing and handle, the Ni-P layer that obtains is even, densification, and barrier propterty is high, and is as shown in Figure 6.

Claims (5)

1. Mg alloy surface homogenizing pre-treating technology, said magnesiumalloy is the Mg-Al alloy; It is characterized in that, may further comprise the steps:
A, polishing are polished to grease, oxide debris and corrosion product, the corner of Mg alloy surface, obtain clean fresh Mg alloy surface;
B, alkaline degreasing are handled, and preparation alkaline degreasing liquid places alkaline degreasing liquid with the clean magnesiumalloy of polishing, handle 5-10min, moderate agitation down at 65-80 ℃;
Acid activation solution is prepared in c, acidic activated processing, and the magnesiumalloy that will pass through the alkaline degreasing processing places acidic activated liquid, at room temperature handles 30-60s, moderate agitation;
D, alkalescence adjustment are handled, the preparation alkaline adjustment liquid, and the magnesiumalloy that will pass through acidic activated processing places alkaline adjustment liquid, handles 5-30min, moderate agitation down at 65-80 ℃;
Adopt flowing water to wash 3min in magnesiumalloy between above-mentioned each step.
2. Mg alloy surface homogenizing pre-treating technology as claimed in claim 1; It is characterized in that: the alkaline degreasing liquid described in the step b is by the formulated aqueous solution of sodium hydroxide, sodium phosphate, yellow soda ash and tensio-active agent; Wherein concentration sodium hydroxide is 30-60g/L; The concentration of sodium phosphate is 5-15g/L, and the concentration of yellow soda ash is 1-5g/L, and surfactant concentrations is 10-80mg/L.
3. Mg alloy surface homogenizing pre-treating technology as claimed in claim 2 is characterized in that: described tensio-active agent is selected from one or both in sodium laurylsulfonate, the perfluoro octyl sulfonic acid tetraethyl-amine.
4. Mg alloy surface homogenizing pre-treating technology as claimed in claim 1; It is characterized in that: the acidic activated liquid described in the step c is by one or more the formulated aqueous solution in phosphoric acid, SODIUMNITRATE or the Hydrocerol A; Wherein concentration of phosphoric acid is 5-200mL/L; The concentration of SODIUMNITRATE is 5-10g/L, and the concentration of Hydrocerol A is 50-100g/L.
5. Mg alloy surface homogenizing pre-treating technology as claimed in claim 1 is characterized in that: the alkaline adjustment liquid described in the steps d is the aqueous solution of sodium hydroxide, and concentration sodium hydroxide is 50-200g/L.
CN201210031832.0A 2012-02-13 2012-02-13 Magnesium alloy surface homogenization pretreatment process Active CN102560516B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103757614A (en) * 2014-01-02 2014-04-30 上海交通大学 Magnesium and magnesium alloy coating and preparation method thereof
CN108456884A (en) * 2017-02-21 2018-08-28 中国科学院金属研究所 A kind of pre-treating method of magnesium alloy chromium-free conversion film homogenization
CN113564611A (en) * 2020-04-28 2021-10-29 南京海创表面处理技术有限公司 Oil removing agent for surface of magnesium-aluminum alloy workpiece and oil removing method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1434149A (en) * 2002-01-23 2003-08-06 中国科学院金属研究所 Method for preparing corrosion-resisting wearing-resisting coat used for magnesium and alloy thereof
CN1477229A (en) * 2003-07-10 2004-02-25 上海交通大学 Zinc-impregnating layer anodic oxidation method colouring process and its treatment solution formula
CN101451239A (en) * 2007-11-29 2009-06-10 比亚迪股份有限公司 Chemical conversion treatment fluid and treatment method of magnesium alloy surface
US20110114497A1 (en) * 2009-11-18 2011-05-19 Kc Chemical Co., Ltd. Method for surface treatment of magnesium or magnesium alloy by anodization

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1434149A (en) * 2002-01-23 2003-08-06 中国科学院金属研究所 Method for preparing corrosion-resisting wearing-resisting coat used for magnesium and alloy thereof
CN1477229A (en) * 2003-07-10 2004-02-25 上海交通大学 Zinc-impregnating layer anodic oxidation method colouring process and its treatment solution formula
CN101451239A (en) * 2007-11-29 2009-06-10 比亚迪股份有限公司 Chemical conversion treatment fluid and treatment method of magnesium alloy surface
US20110114497A1 (en) * 2009-11-18 2011-05-19 Kc Chemical Co., Ltd. Method for surface treatment of magnesium or magnesium alloy by anodization

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103757614A (en) * 2014-01-02 2014-04-30 上海交通大学 Magnesium and magnesium alloy coating and preparation method thereof
CN108456884A (en) * 2017-02-21 2018-08-28 中国科学院金属研究所 A kind of pre-treating method of magnesium alloy chromium-free conversion film homogenization
CN108456884B (en) * 2017-02-21 2019-10-22 中国科学院金属研究所 A kind of pre-treating method of magnesium alloy chromium-free conversion film homogenization
CN113564611A (en) * 2020-04-28 2021-10-29 南京海创表面处理技术有限公司 Oil removing agent for surface of magnesium-aluminum alloy workpiece and oil removing method thereof

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