CN106757260A - A kind of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film its application - Google Patents
A kind of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film its application Download PDFInfo
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- CN106757260A CN106757260A CN201611036356.6A CN201611036356A CN106757260A CN 106757260 A CN106757260 A CN 106757260A CN 201611036356 A CN201611036356 A CN 201611036356A CN 106757260 A CN106757260 A CN 106757260A
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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
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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
- C25D11/024—Anodisation under pulsed or modulated current or potential
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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
- C25D11/026—Anodisation with spark discharge
Abstract
The invention discloses a kind of its application of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film, belong to technical field of aluminum alloy surface treatment.The composite Nano electrolyte is made up of initial treatment electrolyte and after-treatment composite electrolyte two parts；Initial treatment electrolyte is formed by NaOH and sodium metasilicate are soluble in water；The nano combined electrolyte of after-treatment is made up of basic electrolyte, auxiliary additive and nano combined additive.The present invention by adding composite nanometer additive in the electrolytic solution, and combine high frequency complex carrier control technology, differential arc oxidation aluminium microstructure crystal grain can be suppressed to grow up, reduce micro-arc oxidation films phase transition temperature, and then reduce residual stress in oxide ceramic membrane, reduce microstructure defect and improve densification degree, realize the combination properties such as the superpower corrosion resistance of aluminum alloy differential arc oxidation film, superhard and good finish.
Description
Technical field
The present invention relates to technical field of aluminum alloy surface treatment, and in particular to one kind is for preparing aluminum alloy surface differential of the arc oxygen
Change film composite Nano electrolyte its application.
Background technology
Differential arc oxidization technique, also known as micro-plasma oxidation, anodic spark deposition or spark discharge anodic oxidation are general
A kind of new process for treating surface grown up on the basis of logical anodic oxidation.Aluminium alloy passes through electrion in the electrolytic solution
Act on, the ceramic layer based on one layer of aluminum oxide metallurgically combined with matrix of its Surface Creation, the high rigidity of pottery, height
Impedance and high stability meet the anti-seawater corrosion of aluminium alloy, high temperature heat etching and improve the performance requirement such as wear-resisting.The oxide-film is combined
Power is excellent, and hardness, wearability and intensity are higher.But defect is easily produced in the heterogeneous microstructure of the oxide-film and is split
Line, is greatly reduced residual stress in oxide-film, so as to influence its practical application.Influence aluminum alloy differential arc oxidation film combination property has
Two big factors：1) control of external electrical parameters；2) optimization of supporting micro-arc oxidation electrolyte.The present invention is from these two aspects to preparing
Technique is optimized, and the combination property purpose of MAO is improved so as to reach.
The content of the invention
Present invention aim at provide a kind of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film its
Using by researching and developing a kind of new type compound nanometer additive, in adding it to basic electrolyte, and combining external electrical parameters
Control model, the defect and crackle that can effectively suppress in MAO heterogeneous microstructure is produced, and is significantly dropped
Residual stress in suboxides film, reaches the combination property purpose for improving MAO.
To achieve the above object, the technical solution adopted in the present invention is as follows：
A kind of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film, the composite Nano electrolyte be by
Initial treatment electrolyte and after-treatment composite electrolyte two parts are constituted；The initial treatment electrolyte is by NaOH and silicon
Sour sodium formation soluble in water；The nano combined electrolyte of after-treatment is answered by basic electrolyte, auxiliary additive and nanometer
Additive composition is closed, wherein：The basic electrolyte is by least one of silicate, borate and phosphate and NaOH
Be dissolved in the water the solution to be formed, and the auxiliary additive is the one kind or several in molybdate, BTA and malate
Kind, the nano combined additive is made up of nano magnesia and nano yttrium oxide.
Each component content is as follows in the initial treatment electrolyte：
4.5~5g/L of NaOH；
3.5~4g/L of silicate；
Water surplus.
In the nano combined electrolyte of after-treatment, the total concentration of solute is 8~23.2g/ in the basic electrolyte
L, the total concentration of the auxiliary additive is 1.7~2.3g/L, and the total concentration of the nano combined additive is 0.9~2.5g/
L.The species and composition of the after-treatment composite Nano electrolyte are preferably as follows：
It is used to prepare micro-arc oxidation of aluminum alloy surface film using above-mentioned composite Nano electrolyte, preparation process uses two step oxygen
Change method, it is specific as follows：
(1) being placed in Al alloy parts carries out oxidation processes in the initial treatment electrolyte, current density control 3~
5A/dm2Between, taken out after oxidation 10min；
(2) Al alloy parts after step (1) is aoxidized are put into the after-treatment composite electrolyte, then to described
Electrolysis loop applies high frequency complex carrier carries out oxidation processes to workpiece surface, and current density is controlled in 8~20A/dm2Between,
Time per treatment is 15min, number of processes 3~8 times.
In step (2), the high frequency complex carrier is made up of impulse wave and high frequency carrier；The parameter of the impulse wave is：
Pulse repetition frequency is 100~400Hz, and forward voltage amplitude is 250~400V, and positive pulsewidth is 0.6ms, negative voltage amplitude
It is 450~700V, negative sense pulsewidth is 0.4ms；The parameter of the high frequency carrier is：Voltage magnitude is 50~300V, high frequency carrier
Frequency is 2000~3000Hz.
The dutycycle of the impulse wave is one of following four situation：1) positive dutycycle 0%, negative sense dutycycle 0%；2)
Positive dutycycle 10%, negative sense dutycycle 10%；3) positive dutycycle 10%, negative sense dutycycle 20%；4) positive dutycycle
10%, negative sense dutycycle 30%.
The aluminium alloy is LY11, LY12, LC4,2A70, ZL205, LY16,2024,5083,6063 or fine aluminium.
Advantages of the present invention and have the beneficial effect that：
1st, compared with prior art, the additive package that the present invention is constituted using nano magnesia and nano yttrium oxide, will
It is added in basic electrolyte, and is acted synergistically with auxiliary additive, can generate the ceramic film of high-quality, significantly improves film layer
The combination property such as hardness, wearability, corrosion resistance, oxide ceramic membrane surfacing, porosity and micro-crack be significantly less, microcosmic
Institutional framework is evenly distributed.
2nd, nano magnesia can effectively suppress α-Al in oxide-film2O3Phase crystal grain is grown up, it is ensured that differential arc oxidation aluminium ceramics shape
Into microstructure, nano yttrium oxide can reduce sintering temperature, widen sintering range, and crystal boundary combines functional.Therefore, exist
Composite nanometer additive is introduced in micro-arc oxidation electrolyte can be reduced, α-Al2O3Phase transition temperature, crystal grain thinning, so as to reduce
The formation of crackle and defect in ceramic coating formed by micro-arc oxidation, makes the residual stress of ceramic coating formed by micro-arc oxidation small and is evenly distributed.
3rd, applying high frequency complex carrier can control the conversion of differential of the arc eruption strength and sintering strength, suppress microplasma
Impact oxidation when arc light erupt phenomenon, make energy apply rationally and effectively be used for Al2O3Inversion of phases, optimizes two kinds of crystalline state
Syntrophism conversion process, obtains the microstructure with compactness, uniformity and stability.
4th, employed in this technique high frequency complex carrier and nanometer additive can realize simultaneously suppress differential of the arc eruption strength and
Phase transition temperature is reduced, while ensureing to obtain excellent oxidation ceramic membrane combination property, oxide growth is greatly reduced
When energy ezpenditure, reduce production cost, with good economic benefit.
Brief description of the drawings
Fig. 1 is the microcosmic SEM photograph of micro-arc oxidation of aluminum alloy surface film of the embodiment of the present invention 1；Wherein：A () is using implementation
Aluminum alloy differential arc oxidation environmental microbes figure after the treatment of example 1；B () is that aluminum alloy differential arc oxidation film cuts after being processed using embodiment 1
Face shape appearance figure.
Fig. 2 is the microcosmic SEM photograph of micro-arc oxidation of aluminum alloy surface film of the embodiment of the present invention 2；Wherein：A () is using implementation
Aluminum alloy differential arc oxidation environmental microbes figure after the treatment of example 2；B () is that aluminum alloy differential arc oxidation film cuts after being processed using embodiment 2
Face shape appearance figure.
Fig. 3 is the microcosmic SEM photograph of micro-arc oxidation of aluminum alloy surface film of the embodiment of the present invention 3；Wherein：A () is using implementation
Aluminum alloy differential arc oxidation environmental microbes figure after the treatment of example 2；B () is that aluminum alloy differential arc oxidation film cuts after being processed using embodiment 3
Face shape appearance figure.
Specific embodiment
The present invention is described further with reference to embodiment.
Embodiment 1
Material for test：LY12,100 × 100mm of size, Al alloy parts surface is placed in as anode in electrolyte, stainless
Steel is used as negative electrode.It is that 4.5g/L, sodium silicate silicate are 3.7g/L and molten that first Al alloy parts are placed in containing naoh concentration
Agent is in the initial treatment electrolyte of water, current density is controlled in 4.5A/dm2Between, taken out after oxidation 10min.Cleaned with water
Afterwards, Al alloy parts are put into the nano combined electrolyte of after-treatment, electrolyte composition is：Naoh concentration is 4.6g/
L, sodium silicate silicate is 3.5g/L, and molybdic acid na concn is 0.2g/L, and natrium malicum concentration is 0.75/L, and nano oxidized magnesium density is
0.8g/L, nano yttrium oxide concentration is 0.5g/L, and water is surplus.Then high frequency complex carrier is applied to work to the electrolysis loop
Part surface carries out oxidation processes, and current density is controlled in 12A/dm2Between, impulse wave electric voltage frequency is 260~290Hz, positive
Amplitude is 330~350V, and pulsewidth is 0.6ms, and negative voltage amplitude is 500~520V, and pulsewidth is 0.4ms, positive dutycycle
10%, negative sense dutycycle 10%；High frequency carrier voltage magnitude is 120~130V, and high frequent carrier frequency is 2100Hz.It is per treatment
Time is 15min, number of processes 3 times.The microscopic appearance SEM of prepared micro-arc oxidation films is as shown in figure 1, aluminum alloy differential arc oxygen
Change 25~28 μm of ceramic film thickness, uniform texture, by residual stress experimental test, the ceramic coating formed by micro-arc oxidation it is residual
Residue stress is 33.53 ± 8.50MPa, and residual stress is smaller and is evenly distributed.The resistance to neutral salt spray examination of the aluminum alloy differential arc oxidation film
The time is tested up to more than 3000h, up to more than Hv1500, roughness Ra is between 0.01~0.03 μm for microhardness.
Embodiment 2
Material for test：5083,100 × 100mm of size, Al alloy parts surface is placed in as anode in electrolyte, stainless
Steel is used as negative electrode.It is that 4.7g/L, sodium silicate silicate are 3.8g/L and molten that first Al alloy parts are placed in containing naoh concentration
Agent is in the initial treatment electrolyte of water, current density is controlled in 3.6A/dm2Between, taken out after oxidation 10min.Cleaned with water
Afterwards, Al alloy parts are put into the nano combined electrolyte of after-treatment, electrolyte composition is：Naoh concentration is 5g/L,
Boratex 5.8g/L, phosphoric acid na concn is 5.5g/L, and BTA concentration is 0.96g/L, and natrium malicum concentration is 0.78g/
L, nano oxidized magnesium density is 1.2g/L, and nano yttrium oxide concentration is 0.6g/L, and water is surplus.Then applied to the electrolysis loop
Increasing frequency complex carrier carries out oxidation processes to workpiece surface, and current density is controlled in 9A/dm2Between, impulse wave electric voltage frequency
It is 180~190Hz, positive amplitude is 360~370V, pulsewidth is 0.6ms, and negative voltage amplitude is 620~630V, and pulsewidth is
0.4ms, positive dutycycle 10%, negative sense dutycycle 20%；High frequency carrier voltage magnitude is 150~160V, high frequent carrier frequency
It is 2200Hz.Time per treatment is 15min, number of processes 5 times.Microscopic appearance SEM such as Fig. 2 of prepared micro-arc oxidation films
Shown, aluminum alloy differential arc oxidation ceramic membrane hole is evenly distributed, 26~30 μm of thicknesses of layers, uniform texture, by ginseng
With stress test test, the residual stress of the ceramic coating formed by micro-arc oxidation is 26.68 ± 5.12MPa, and residual stress is smaller and is distributed
Uniformly.The aluminum alloy differential arc oxidation film resistance to neutral salt spray test time up to more than 3500h, microhardness up to Hv1800, slightly
Rugosity Ra is between 0.03~0.05 μm.
Embodiment 3
Material for test：LC4,100 × 100mm of size, Al alloy parts surface is placed in electrolyte as anode, stainless steel
As negative electrode.It is 5g/L that first Al alloy parts are placed in containing naoh concentration, sodium silicate silicate is 4g/L and solvent is water
Initial treatment electrolyte in, current density control in 4.2A/dm2Between, taken out after oxidation 10min.After being cleaned with water, by aluminium
Alloy workpiece is put into the nano combined electrolyte of after-treatment, and electrolyte composition is：Naoh concentration is 5g/L, and sodium metasilicate is dense
It is 4g/L to spend, and phosphoric acid na concn is 7g/L, and molybdic acid na concn is 0.25g/L, and BTA concentration is 1g/L, nano magnesia
Concentration is 0.6g/L, and nano yttrium oxide concentration is 0.7g/L, and water is surplus.Then the compound load of high frequency is applied to the electrolysis loop
Ripple carries out oxidation processes to workpiece surface, and current density is controlled in 15A/dm2Between, impulse wave electric voltage frequency be 120~
130Hz, positive amplitude is 270~280V, and pulsewidth is 0.6ms, and negative voltage amplitude is 490~500V, and pulsewidth is 0.4ms, just
To dutycycle 10%, negative sense dutycycle 30%；High frequency carrier voltage magnitude is 90~100V, and high frequent carrier frequency is 2400Hz.
Time per treatment is 15min, number of processes 6 times.The microscopic appearance SEM of prepared micro-arc oxidation films is as shown in figure 3, aluminium is closed
Golden arc differential oxide ceramic film hole is evenly distributed, 25~27 μm of thicknesses of layers, uniform texture, by participating in stress test
Test, the residual stress of the ceramic coating formed by micro-arc oxidation is 21.38 ± 7.61MPa, and residual stress is smaller and is evenly distributed.The aluminium is closed
The golden micro-arc oxidation films resistance to neutral salt spray test time, up to Hv2000, roughness Ra was 0.02 for microhardness up to more than 3300h
Between~0.04 μm.
Claims (8)
1. a kind of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film, it is characterised in that：The composite Nano
Electrolyte is made up of initial treatment electrolyte and after-treatment composite electrolyte two parts；The initial treatment electrolyte is by hydrogen
Sodium oxide molybdena and sodium metasilicate formation soluble in water；The nano combined electrolyte of after-treatment is by basic electrolyte, auxiliary addition
Agent and nano combined additive are constituted, wherein：The basic electrolyte is by least one of silicate, borate and phosphate
Be dissolved in the water the solution to be formed with NaOH, and the auxiliary additive is in molybdate, BTA and malate
One or more, the nano combined additive is made up of nano magnesia and nano yttrium oxide.
2. the composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film according to claim 1, its feature
It is：Each component content is as follows in the initial treatment electrolyte：
4.5~5g/L of NaOH；
3.5~4g/L of silicate；
Water surplus.
3. the composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film according to claim 2, its feature
It is：In the nano combined electrolyte of after-treatment, the total concentration of solute is 8~23.2g/L, institute in the basic electrolyte
The total concentration of auxiliary additive is stated for 1.7~2.3g/L, the total concentration of the nano combined additive is 0.9~2.5g/L.
4. the composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film according to claim 3, its feature
It is：After-treatment composite Nano electrolyte composition is as follows：
5. according to any described composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film of claim 1-4
Using, it is characterised in that：The composite Nano electrolyte is used to prepare micro-arc oxidation of aluminum alloy surface film, and preparation process uses two steps
Oxidizing process, it is specific as follows：
(1) being placed in Al alloy parts carries out oxidation processes in the initial treatment electrolyte, current density is controlled in 3~5A/
dm2Between, taken out after oxidation 10min；
(2) Al alloy parts after step (1) is aoxidized are put into the after-treatment composite electrolyte, then to the electrolysis
Loop applies high frequency complex carrier carries out oxidation processes to workpiece surface, and current density is controlled in 8~20A/dm2Between, every time
Process time is 15min, number of processes 3~8 times.
6. the application for preparing the composite Nano electrolyte of micro-arc oxidation of aluminum alloy surface film according to claim 5,
It is characterized in that：In step (2), the high frequency complex carrier is made up of impulse wave and high frequency carrier；The parameter of the impulse wave
For：Pulse repetition frequency is 100~400Hz, and forward voltage amplitude is 250~400V, and positive pulsewidth is 0.6ms, negative voltage
Amplitude is 450~700V, and negative sense pulsewidth is 0.4ms；The parameter of the high frequency carrier is：Voltage magnitude is 50~300V, high frequency
Carrier frequency is 2000~3000Hz.
7. the application for preparing the composite Nano electrolyte of micro-arc oxidation of aluminum alloy surface film according to claim 6,
It is characterized in that：The dutycycle of the impulse wave is one of following four situation：1) positive dutycycle 0%, negative sense dutycycle
0%；2) positive dutycycle 10%, negative sense dutycycle 10%；3) positive dutycycle 10%, negative sense dutycycle 20%；4) forward direction is accounted for
Sky compares 10%, negative sense dutycycle 30%.
8. the application for preparing the composite Nano electrolyte of micro-arc oxidation of aluminum alloy surface film according to claim 5,
It is characterized in that：The aluminium alloy is LY11, LY12, LC4,2A70, ZL205, LY16,2024,5083,6063 or fine aluminium.
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Cited By (8)
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| CN107604411A (en) * | 2017-11-08 | 2018-01-19 | 江门市江海区杰德化工有限公司 | A kind of aluminum alloy differential arc oxidation processing method |
| CN108707943A (en) * | 2018-05-27 | 2018-10-26 | 中南大学 | A kind of micro-arc oxidation electrolyte and its application on preparing high surface hardness aluminium alloy plate |
| CN108823626A (en) * | 2018-05-27 | 2018-11-16 | 中南大学 | A kind of Al2O3/ Al/Mg stratiform density gradient material and its preparation method and application |
| CN109023468A (en) * | 2018-07-27 | 2018-12-18 | 福建龙溪轴承(集团)股份有限公司 | The preparation method of 2XXX aluminium and aluminum alloy surface high-antiwear self-lubricating differential arc oxidation film layer |
| CN109183115A (en) * | 2018-10-19 | 2019-01-11 | 北京杜尔考特科技有限公司 | A kind of surface is covered with the preparation method of the aluminium alloy of superhard ceramic coating formed by micro-arc oxidation |
| CN109252200A (en) * | 2018-11-05 | 2019-01-22 | 佛山市南海镕信金属制品有限公司 | A kind of aluminum alloy die casting surface treatment method |
| WO2020190251A1 (en) * | 2019-03-20 | 2020-09-24 | Олександр Анатолийовыч САМОЙЛЕНКО | Antibacterial ceramic coating and method for coating titanium alloy implants |
| CN111910238A (en) * | 2020-08-14 | 2020-11-10 | 常州大学 | Electrolyte for realizing blackening of magnesium alloy surface and blackening process method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107604411A (en) * | 2017-11-08 | 2018-01-19 | 江门市江海区杰德化工有限公司 | A kind of aluminum alloy differential arc oxidation processing method |
| CN108707943A (en) * | 2018-05-27 | 2018-10-26 | 中南大学 | A kind of micro-arc oxidation electrolyte and its application on preparing high surface hardness aluminium alloy plate |
| CN108823626A (en) * | 2018-05-27 | 2018-11-16 | 中南大学 | A kind of Al2O3/ Al/Mg stratiform density gradient material and its preparation method and application |
| CN109023468A (en) * | 2018-07-27 | 2018-12-18 | 福建龙溪轴承(集团)股份有限公司 | The preparation method of 2XXX aluminium and aluminum alloy surface high-antiwear self-lubricating differential arc oxidation film layer |
| CN109183115A (en) * | 2018-10-19 | 2019-01-11 | 北京杜尔考特科技有限公司 | A kind of surface is covered with the preparation method of the aluminium alloy of superhard ceramic coating formed by micro-arc oxidation |
| CN109252200A (en) * | 2018-11-05 | 2019-01-22 | 佛山市南海镕信金属制品有限公司 | A kind of aluminum alloy die casting surface treatment method |
| WO2020190251A1 (en) * | 2019-03-20 | 2020-09-24 | Олександр Анатолийовыч САМОЙЛЕНКО | Antibacterial ceramic coating and method for coating titanium alloy implants |
| CN111910238A (en) * | 2020-08-14 | 2020-11-10 | 常州大学 | Electrolyte for realizing blackening of magnesium alloy surface and blackening process method |
| CN111910238B (en) * | 2020-08-14 | 2022-05-31 | 常州大学 | Electrolyte for realizing blackening of magnesium alloy surface and blackening process method |
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