CN106757267A - A kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films - Google Patents

A kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films Download PDF

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Publication number
CN106757267A
CN106757267A CN201710039546.1A CN201710039546A CN106757267A CN 106757267 A CN106757267 A CN 106757267A CN 201710039546 A CN201710039546 A CN 201710039546A CN 106757267 A CN106757267 A CN 106757267A
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aluminum base
cast aluminum
workpiece
base composite
arc oxidation
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CN201710039546.1A
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张海荣
原增民
赵云成
师艳丽
郝亚楠
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Shanxi Pingyang Industry Machinery Co Ltd
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Shanxi Pingyang Industry Machinery Co Ltd
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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
    • C25D11/024Anodisation under pulsed or modulated current or potential
    • 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
    • C25D11/026Anodisation with spark discharge
    • 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
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • 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
    • C25D11/14Producing integrally coloured layers
    • 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
    • C25D11/16Pretreatment, e.g. desmutting

Abstract

The present invention is specially a kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films, solves the problems, such as that existing cast aluminum base composite material surface green film preparation has camouflage effectiveness difference and corrosion resistance, hardness, roughness are poor.A, workpiece surface is polished after clean;B, in deionized water addition NaOH 2 4g/L, NiSO4 2 4g/L, Na2SiO38 15g/L,(NaPO3)610 15g/L, Na2WO4The g/L of 5 10g/L, EDTA 38, stirring to fully dissolving;C, put the workpiece in solution, open mao power source, power parameter is set;Power supply is closed after d, 20 30min of oxidation;E, workpiece is cleaned up and dried.The present invention further increases the compactness of oxide-film, while film hardness is up to HV1500 2200.

Description

A kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films
Technical field
The present invention relates to cast aluminum base composite material process for treating surface, specially a kind of cast aluminum base composite material surface The preparation method of green black colour micro-arc oxidation films.
Background technology
Shell body belonging to underawater ordnance product, material is cast aluminum base composite material, to improve disguised, raising of fighting The combination properties such as corrosion resistance, insulating properties, the wearability of cast aluminum base composite material surface of shell, design requirement surface carries out military green Color differential arc oxidation, while proposing high requirement to performances such as film hardness, corrosion resistance, insulating properties, bond strengths.
Differential arc oxidation(MAO, Micro-arc oxidation), also known as " micro-plasma oxidation ", " anode spark sinks Shallow lake ", " spark discharge anodic oxidation ".Can be directly in valve metal(Mg、Al、Ti、Zr、Nb)Surface in situ grows ceramic film, reaches Increased substantially to workpiece surface reinforcing, hardness, the mesh that wear-resisting, anti-corrosion, insulation and the performance such as high temperature resistance thermal shock are improved 's.
Differential arc oxidation is grown up on the basis of traditional anodic oxidation, and its essence is exactly a ceramic membrane moment The process for puncturing.From initial " electron avalanche " model, ceramic layer breakdown voltage " microbridge electric discharge " model finally, it may be said that The theoretical research of differential arc oxidation is carried out mainly around electrical breakdown theory, during electrical breakdown, has been usually associated with spark Electric discharge phenomena are produced and morphology, the change of structure, are that physics electric discharge, electrochemical oxidation and heat chemistry, heat treatment etc. are assisted The result of same-action.The forming process of ceramic coating is extremely complex, so the more conventional oxidation of research difficulty is difficult, to being at present Only, there is no a kind of theoretical model can quantify, satisfactorily explains all of differential arc oxidation experimental phenomena and describe the formation of film layer Process.
At present, there is following weak point in the preparation research about green film:1st, Film color is close to white or tends to black Green, and irregular colour is even, influences camouflage effectiveness;2nd, the corrosion resistance of film layer, hardness, roughness can not meet cast aluminum base and be combined The combination property of material weapons.
The content of the invention
To there is camouflage effectiveness poor and anti-corrosion in order to solve the green film preparation of existing cast aluminum base composite material surface for the present invention A kind of poor problem of property, hardness, roughness, there is provided preparation of cast aluminum base composite material surface green black colour micro-arc oxidation films Method.
The present invention adopts the following technical scheme that realization:A kind of cast aluminum base composite material surface green black colour differential arc oxidation The preparation method of film, using following steps:A, cast aluminum base composite material workpiece surface is polished using waterproof abrasive paper after put Enter rinsing bowl to be cleaned;B, by following mass volume ratio sequentially add NaOH 2-4g/L, NiSO in deionized water4 2- 4g/L, Na2SiO38-15g/L,(NaPO3)610-15g/L, Na2WO45-10g/L, EDTA 3-8 g/L, the PH of obtained solution It is 8-11 to be worth, stirring to fully dissolving;C, cast aluminum base composite material workpiece is put into solution, workpiece is connected with anode, molten After the stainless steel plate connection negative electrode of liquid bath body, mao power source is opened, power parameter is set:Dutycycle 5-10%, power supply is frequently Rate 800-1000Hz, positive negative pulse stuffing compares 5:1, oxidation voltage 500-600V, current density 10-15A/dm2, operating temperature 35-45 DEG C, and to electrically for ladder gives electricity, 3-5 grades of ladder series;Power supply is closed after d, oxidation 20-30min, just can be in casting Make aluminum matrix composite workpiece surface and prepare green black colour micro-arc oxidation films;E, cast aluminum base composite material workpiece is put into washing Cleaned up in groove and dried.
Na in solution formula2SiO3With NaOH as system solution, work as Na2SiO3When too low with NaOH concentration, electrolyte is led Electric rate reduction, influences arcing voltage, in some instances it may even be possible to lead to not the starting the arc;Work as Na2SiO3When too high with NaOH concentration, electrolyte electricity Conductance is raised, and electric current becomes big, causes film layer coarse, in some instances it may even be possible to cause matrix ablation.
NiSO in solution formula4It is coloring salt, its concentration directly affects oxide-film color, tests prove that, NiSO4Concentration During less than 2 g/L, not substantially, oxide-film color is close white for coloring;Work as NiSO4When concentration is higher than 4 g/L, coloring is obvious, face Color tends to blackish green.
In solution formula(NaPO36It is suppression arc agent, the effect for suppressing arc light effect can be played, the power of arc light effect is straight The size of influence film layer hole is connect, appropriate arc light intensity is conducive to improving the compactness of film layer, reduces the formation of micro-crack.Examination Issue after examination and approval and show, when(NaPO36When concentration is less than 10g/L, the change of surface of test piece acnode is not obvious;As addition 10-15g/L(NaPO36 When, from big, dispersion is changed into small and uniform to surface of test piece acnode.
EDTA is complexing agent in solution formula, plays stabilization tank liquor composition, the effect of uniform ion distribution, when EDTA concentration When too low, there is the phenomenon of irregular colour in film layer.
Na in solution formula2WO4Used as additive, aluminium ion reacts reinforcement with oxonium ion in can making tank liquor, in workpiece Rejected region is adsorbed, and fills up hole, dense layer thickness is improved, so as to improve the corrosion resistance of film layer, hardness, roughness.
Differential arc oxidation essence is high electrical breakdown oxide-film, spark discharge is produced, so as to form the ceramic membrane of melting, voltage It is very crucial factor, when voltage is less than 300V, micro-arc oxidation process can not be normally carried out;And voltage be less than 500V when, Although forming differential arc oxidation film layer, because undertension is to puncture established oxide-film, cause oxide thickness thin;Work as electricity When pressure is higher than 600V, due to overtension, electric current also can be raised accordingly, and acutely, tank liquor temperature is raised spark discharge process, oxidation Film is coarse, so as to influence the performance of oxide-film, or even ablation phenomen occurs.
When differential arc oxidation starts, workpiece surface can be initially formed hardening oxidation film layer, by a liter high voltage, puncture oxide-film, Form new melting micro-arc oxidation films.Workpiece is for a long time in the solution in low current density, it may appear that galvano-cautery, damages work Part.In micro-arc oxidation process, such as current density is too low, and oxide-film generating rate is slow;As current density is too high, spark discharge process Acutely, film layer pore diameter becomes big, influences the thickness of compacted zone, and so as to cause film hardness, corrosion resistance reduction, film layer is coarse.
Pulse frequency influences the discharge energy of individual pulse.Pulse frequency is too low, and individual pulse discharge energy is bigger, spark Electric discharge is stronger, and film layer compactness can be reduced;Pulse frequency is too high, and film layer compactness is improved, film hardness, corrosion resistance, wear-resisting Property etc. performance improve, but film layer generating rate can be influenceed.
Dutycycle influences the individual pulse discharge period, and dutycycle is too low, and the individual pulse time is too short, and energy is not enough, Micro-arc discharge is insufficient;Dutycycle is too high, and individual pulse overlong time, energy is excessive, causes film layer pore diameter to become big, hardness And corrosion resistance reduction, rough surface.
Temperature is also extremely crucial in micro-arc oxidation process, and temperature is too high to make the enhancing of tank liquor ion activity, and electrical conductivity is carried Height, oxide-film generating rate is accelerated, and film layer roughness increases.
The present invention selects the constituent content and mao power source parameter of solution by a large amount of experiments repeatedly, overcomes Existing cast aluminum base composite material surface green film preparation there is camouflage effectiveness difference and corrosion resistance, hardness, roughness be poor Problem.
NaF is free of in preparation method of the present invention, is volatilized without HF in oxidizing process, operating process is safer;And The compactness of oxide-film is further increased, micro-crack is reduced, while film hardness is up to HV1500-2200, corrosion resistance is salt Mist tests the corrosion-free signs of 200h, uses range to be detected for the insulation resistance meter of 500M Ω, and insulaion resistance is+∞;Bond strength The MPa of > 30;And evidence of corrosion occur in prior art differential arc oxidation film layer 96h salt spray tests, insulaion resistance is 100M Ω.Have Technique simplifies, the advantage that camouflage effectiveness is good and hardness, corrosion resistance, wearability, insulating properties, bond strength are good, improves surface Roughness.
Specific embodiment
Embodiment 1
A kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films, using following steps:A, using water Sand paper is put into rinsing bowl and cleans after polishing cast aluminum base composite material workpiece surface;B, in deionized water by such as Lower mass volume ratio sequentially adds NaOH 2g/L, NiSO4 2g/L, Na2SiO38g/L,(NaPO3)610g/L, Na2WO4 5g/ The g/L of L, EDTA 3, the pH value of obtained solution is 8, stirring to fully dissolving;C, cast aluminum base composite material workpiece is put into it is molten In liquid, workpiece is connected with anode, after the stainless steel plate connection negative electrode of solution cell body, opens mao power source, sets power supply ginseng Number:Dutycycle 10%, supply frequency 1000Hz, positive negative pulse stuffing compares 5:1, oxidation voltage 500V, current density 15A/dm2, 35 DEG C of operating temperature, and to electrically for ladder gives electricity, 3 grades of ladder series;Power supply is closed after d, oxidation 20min, just can be in casting Make aluminum matrix composite workpiece surface and prepare green black colour micro-arc oxidation films;E, cast aluminum base composite material workpiece is put into washing Cleaned up in groove and dried.
Ladder is shown in Table 1 to ammeter.
The ladder time (min) Voltage(V) Electric current(A/dm2
2 300 15
3 400 15
15 500 15
Table 1
Obtained oxide-film color is shallow green black colour, and 23 μm of thickness, film hardness HV1680, salt spray test 200 hours is corrosion-free Sign, uses range to be detected for the insulation resistance meter of 500M Ω, and insulaion resistance is+∞;Bond strength > 30MPa.
Embodiment 2
A kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films, using following steps:A, using water Sand paper is put into rinsing bowl and cleans after polishing cast aluminum base composite material workpiece surface;B, in deionized water by such as Lower mass volume ratio sequentially adds NaOH 3.7g/L, NiSO4 2.3g/L, Na2SiO313g/L,(NaPO3)611g/L, Na2WO48g/L, EDTA 3.5g/L, the pH value of obtained solution is 9.8, stirring to fully dissolving;C, by cast aluminum base composite wood Material workpiece is put into solution, and workpiece is connected with anode, after the stainless steel plate connection negative electrode of solution cell body, opens differential arc oxidation electricity Source, sets power parameter:Dutycycle 5%, supply frequency 938Hz, positive negative pulse stuffing compares 5:1, oxidation voltage 600V, electric current is close Degree 10A/dm2, 39 DEG C of operating temperature, and to electrically for ladder gives electricity, 4 grades of ladder series;Electricity is closed after d, oxidation 27min Source, just can prepare green black colour micro-arc oxidation films in cast aluminum base composite material workpiece surface;E, by cast aluminum base composite material Workpiece is put into rinsing bowl and cleans up and dry.
Ladder is shown in Table 2 to ammeter.
The ladder time (min) Voltage(V) Electric current(A/dm2
2 300 10
3 400 10
4 500 10
11 600 10
Table 2
Obtained oxide-film color is green black colour, 24 μm of thickness, film hardness HV1910,200 hours corrosion-free marks of salt spray test As, use range to be detected for the insulation resistance meter of 500M Ω, insulaion resistance is+∞;Bond strength > 30MPa.
Embodiment 3
A kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films, using following steps:A, using water Sand paper is put into rinsing bowl and cleans after polishing cast aluminum base composite material workpiece surface;B, in deionized water by such as Lower mass volume ratio sequentially adds NaOH 4g/L, NiSO4 4g/L, Na2SiO315g/L,(NaPO3)615g/L, Na2WO4 The g/L of 10g/L, EDTA 8, the pH value of obtained solution is 11, stirring to fully dissolving;C, cast aluminum base composite material workpiece is put Enter in solution, workpiece is connected with anode, after the stainless steel plate connection negative electrode of solution cell body, open mao power source, electricity is set Source parameter:Dutycycle 8%, supply frequency 1000Hz, positive negative pulse stuffing compares 5:1, oxidation voltage 547V, current density 12A/ dm2, 45 DEG C of operating temperature, and to electrically for ladder gives electricity, 4 grades of ladder series;Power supply is closed after d, oxidation 30min, just may be used Green black colour micro-arc oxidation films are prepared in cast aluminum base composite material workpiece surface;E, cast aluminum base composite material workpiece is put into Cleaned up in rinsing bowl and dried.
Ladder is shown in Table 3 to ammeter.
The ladder time (min) Voltage(V) Electric current(A/dm2
2 300 12
3 400 12
4 500 12
21 600 12
Table 3
Obtained oxide-film color is deep green black colour, 32 μm of thickness, film hardness HV2100, and salt spray test 200 hours is corrosion-free Sign, uses range to be detected for the insulation resistance meter of 500M Ω, and insulaion resistance is+∞;Bond strength > 30MPa.
In specific implementation process, the size of cast aluminum base composite material workpiece is 100mm × 50mm × 5mm, material model It is YRZ-02;Using exchange dipulse differential arc oxidation production line, power supply is MAO300, power 300KW to equipment, as needed Constant voltage oxidizing process or constant current oxidizing process can be used.

Claims (1)

1. a kind of preparation method of cast aluminum base composite material surface green black colour micro-arc oxidation films, it is characterised in that:Using as follows Step:A, cast aluminum base composite material workpiece surface is polished using waterproof abrasive paper after be put into rinsing bowl and clean;B, In deionized water NaOH 2-4g/L, NiSO are sequentially added by following mass volume ratio42-4g/L, Na2SiO38-15g/L, (NaPO3)610-15g/L, Na2WO45-10g/L, EDTA 3-8 g/L, the pH value of obtained solution is 8-11, and stirring is to abundant Dissolving;C, cast aluminum base composite material workpiece is put into solution, workpiece is connected with anode, the stainless steel plate connection of solution cell body After negative electrode, mao power source is opened, power parameter is set:Dutycycle 5-10%, supply frequency 800-1000Hz, positive and negative arteries and veins Punching compares 5:1, oxidation voltage 500-600V, current density 10-15A/dm2, 35-45 DEG C of operating temperature, and to being electrically Ladder is to electricity, 3-5 grades of ladder series;Power supply is closed after d, oxidation 20-30min, just can be in cast aluminum base composite material workpiece table Prepare green black colour micro-arc oxidation films in face;E, cast aluminum base composite material workpiece is put into rinsing bowl cleans up and dry.
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CN109402699A (en) * 2018-11-01 2019-03-01 中国科学院兰州化学物理研究所 A kind of aluminum alloy surface acid resistance corrosion function ceramic membrane preparation process
CN111549366A (en) * 2020-06-08 2020-08-18 上海交通大学 Preparation method of in-situ growth green corrosion-resistant ceramic membrane on surface of aluminum-based composite material

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