CN103695981A - Functional design method for aluminum alloy surface micro-arc oxidation film - Google Patents
Functional design method for aluminum alloy surface micro-arc oxidation film Download PDFInfo
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- CN103695981A CN103695981A CN201210375655.8A CN201210375655A CN103695981A CN 103695981 A CN103695981 A CN 103695981A CN 201210375655 A CN201210375655 A CN 201210375655A CN 103695981 A CN103695981 A CN 103695981A
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Abstract
Belonging to the technical field of aluminum alloy surface treatment, the invention discloses a functional design method for an aluminum alloy surface micro-arc oxidation film. The method is realized by applying square-wave pulse voltage and high frequency carrier wave simultaneously in an aluminum alloy micro-arc oxidation process. A supporting electrolyte solution is mainly composed of a basic composition, an auxiliary additive and a densification additive. Through mutual cooperation of specific external electrical parameters and the related supporting optimized electrolyte solution, the aluminum alloy micro-arc oxidation film realizes super-strong corrosion resistance, excellent wear resistance, good heat insulation, ultra-thinness, ultra-thickness, super-hardness and good smoothness directed at practical application situations.
Description
Technical field
The invention belongs to aluminum alloy surface processing technology field, be specifically related to a kind of method of aluminum alloy surface micro-arc oxidation films functionalized design.
Background technology
Differential arc oxidization technique, claims again micro-plasma oxidation, and anodic spark deposition or spark discharge anodic oxidation are a kind of new process for treating surface growing up on the basis of common anode oxidation.Aluminium alloy in electrolytic solution by electrion effect, its Surface Creation one deck be take the aluminum oxide that metallurgical mode is combined with matrix be main ceramic layer, and the high rigidity of pottery, high resistance and high stability meet the anti-sea-water corrosion of aluminium alloy, high temperature heat etching and improve the performance requriementss such as wear-resisting.This oxide film bonding force is good, and hardness, wear resistance and intensity are higher.Yet, considering the Application Areas diversity of following aluminum alloy differential arc oxidation film, certainly will have higher requirement to the functionalized design of aluminum alloy differential arc oxidation film properties.
At present, realize aluminum alloy differential arc oxidation film functionalized design and mainly contain two large influence factors: the 1) control of external electrical parameters; 2) optimization of supporting differential arc oxidation electrolytic solution.This patent based on above-mentioned two large factors by external electrical parameters master mode, and in conjunction with the electrolyte prescription of supporting optimization, thereby realize aluminum alloy differential arc oxidation film functionalized design.
Summary of the invention
The object of the invention is to provide a kind of method of aluminum alloy surface micro-arc oxidation films functionalized design, adopt described micro-arc oxidation process, realize the superpower solidity to corrosion of aluminum alloy differential arc oxidation film, excellent wear resistance, good thermal insulation, ultra-thin property, super thick property, superhard property and good smooth finish.
Technical scheme of the present invention is:
A kind of method of aluminum alloy differential arc oxidation film functionalized design, first Al alloy parts is placed in to electrolytic solution, pending workpiece surface in electrolytic solution as working electrode, stainless steel conductor is as to electrode, and form electrolysis loop with described work surface, and to described electrolysis loop, applying square wave pulse voltage and high frequency carrier carries out oxide treatment to Al alloy parts simultaneously, current density is controlled at 0.2-20A/dm simultaneously
2between, the treatment time is 30～200min, treatment temp is not higher than 50 ℃.
Its solvent of described electrolytic solution is water, solute by basis form, supplementary additive and densification additive form, the total concn of solute is 1-20g/L, the pH value of controlling electrolytic solution is 5 ~ 8 (utilize the NaOH of dilution, or dilute nitric acid solution adjusting); Described base set becomes one or more in sodium hydroxide, silicate, borate and phosphoric acid salt; Supplementary additive is one or more in vanadate, molybdate, dodecylbenzene sulfonate, caprate, benzotriazole, malate; Densification additive is one or more in Yttrium trinitrate, cerous nitrate, lanthanum nitrate.
Described square wave pulse voltage frequency is 1000～400Hz, and forward amplitude is 250-400V, and pulsewidth is 0.6ms, and negative voltage amplitude is 450-700V, and pulsewidth is 0.4ms.The break make ratio of described square wave pulse voltage can be following four kinds of situations: 1) forward dutycycle 0%, negative sense dutycycle 0%; 2) forward dutycycle 10%, negative sense dutycycle 10%; 3) forward dutycycle 10%, negative sense dutycycle 20%; 4) forward dutycycle 10%, negative sense dutycycle 30%.Described high frequency carrier voltage magnitude is 50-300V, and high frequent carrier frequency is 2000-3000Hz.
Described aluminium alloy is LY11, LY12, LC4,2A70, ZL205, LY16,2024,5083,6063 or fine aluminium.
The present invention cooperatively interacts by specific external electrical parameters and relevant supporting optimization electrolytic solution, for the practical situation of applying, has realized aluminum alloy differential arc oxidation film functionalized design.The micro-arc oxidation films salient features of preparing in aluminum alloy surface is as follows: thickness 3～200 μ m, and more than neutral salt spray time 2000h, hardness Hv1000, dry friction coefficient f≤0.1, surface roughness Ra≤0.02 μ m, bonding force is greater than 30MPa.
Advantage of the present invention and beneficial effect are as follows:
The amplitude of the anodic pulse voltage 1, applying will be significantly less than the arc discharge of conventional differential arc oxidation process formation microplasma and require critical sparking voltage, but the voltage being oxidized higher than common anode belongs to anodic oxidation farad voltage belt.Be conducive to like this in general anodised faraday's current potential district, form microplasma and produce α-Al
2o
3phase transformation, promotes film microstructure chemical stability and has feasibility, thereby realizes wear resistance and the superhard property of the superpower solidity to corrosion of aluminum alloy differential arc oxidation film, excellence.
2, the pulsed voltage that the cathode pulse voltage applying will apply far above conventional micro-arc oxidation process, can realize minimum, step negative electrode rush current, and discharge frequency is very high.Like this, because having n-P Joint Properties, aluminium/oxide film/solution interface has rectifying action, when Faradaic current from oxidation become reduction current, when contacting of utmost point metal is ohmic contact, to make cathodic reduction electric current be easy to can occur reduce attenuate and reduce membrane resistance because the cathodic current effect going round and beginning again make the blocking layer of fenestra bottom by, aluminium surface film oxide.From macroscopic perspective, negative electrode carrier wave shock action can reduce microplasma generation discharge breakdown anode voltage, can make oxidation current reduce, as long as it is proper that negative electrode carrier wave electrical parameter is selected, just can effectively reduce the Jiao Erre producing because of film resistance and make interface heat due to the rapid diffusion of separating out of a large amount of hydrogen, thereby reduce disruptive strength and the chemical dissolution speed of the microplasma of aluminium porous surface oxide film, reduce the porosity of film.Make spontaneously uniformity of the electric discharge duct that forms, avoid causing due to distribution of current inequality generation or the development of local microcell macropore, make the densification of discharge channel different zones, homogenizing, make the electric discharge of anodizing process of different microcells meticulous controlled, realize the superpower solidity to corrosion of aluminum alloy differential arc oxidation film, excellent wear resistance and and thermal insulation.
3, apply high frequency sinusoidal carrier, can control the conversion of differential of the arc eruption strength and sintering strength, suppress the arc light eruption phenomenon when impacting oxidation of microplasma, energy is applied rationally and effectively for Al
2o
3inversion of phases, optimizes two kinds of crystalline state conversion process of jointly growing.Utilize α-Al
2o
3adjust the chemical stability of microstructure, γ-Al
2o
3adjust the structural performance of microstructure, control its growth distribution state, the state of adjusting seed size size, crystal lattice orientation, different crystalline phases, can effectively regulate and control the interaction between densification ordered structure and inversion of phases like this, obtain the phase structure with compactness, homogeneity and stability simultaneously, at abundant sintering with when completing and change to stable phase, realize the thickness of aluminum alloy differential arc oxidation film and stablize controlled.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 aluminum alloy surface micro-arc oxidation films micrograph.
Fig. 2 is the XRD spectra of the embodiment of the present invention 1 aluminum alloy surface micro-arc oxidation films.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Material for test: LY12, size 100 * 100mm, Al alloy parts surface is placed in electrolytic solution as anode, and stainless steel is as negative electrode.Electrolyte ratio: sodium hydroxide 4～5g/L, water glass 3 ~ 5g/L, Sodium Tetraborate 6～7g/L, vanadic acid sodium 2.5～3g/L, sodium malate 0.7 ~ 1g/L, Yttrium trinitrate is 0.2～0.8g/L, cerous nitrate 0.8～1.2g/l, electrolyte ph is 5 ~ 8.Adopting Dole to examine the square wave pulse voltage frequency that special IV type great power pulse power source applies to electrolysis loop is 260～270Hz, and forward voltage amplitude is 360～390V, and pulsewidth is 0.6ms, and negative voltage amplitude is 520 ~ 550V, and pulsewidth is 0.4ms; Dutycycle is: forward dutycycle 0%, negative sense dutycycle 0%.The high frequency carrier voltage magnitude that applies is 80～100V, high frequent carrier frequency 2000Hz; Current density 1.5 ~ 16A/dm
2, oxidization time 140 ~ 150min, treatment temp is not higher than 40 ℃.
As shown in Figure 1, the XRD spectra of phase structure as shown in Figure 2 for its microscopic appearance of micro-arc oxidation films SEM of preparation.From Fig. 1 and Fig. 2, can find out the Al preparing with aforesaid method
2o
3ceramic membrane hole distribution is even, thicknesses of layers 30 ~ 50 μ m, Al
2o
3be mainly α phase.
The salient features of this aluminum alloy differential arc oxidation film is as follows: superpower solidity to corrosion (more than neutral salt spray 2000h), bonding force is greater than 30MPa.This functional membrane is not destroyed the fatigue property of matrix, and can increase substantially Corrosion Fatigue Properties.
Embodiment 2
Material for test: 5083, size 100 * 100mm, Al alloy parts surface is placed in electrolytic solution as anode, and stainless steel is as negative electrode.Electrolyte ratio: sodium hydroxide 4.5 ~ 5g/L, water glass 3.5～4g/L, Sodium Tetraborate 5.6 ~ 6.2g/L, Sodium orthomolybdate 0.2～0.3g/L, Sodium decanoic acid 0.8～1.1g/L, sodium malate 0.7～0.9g/L, cerous nitrate 0.8 ~ 1.1g/l, electrolyte ph is 5 ~ 8.Adopting Dole to examine the square wave pulse voltage frequency that special IV type great power pulse power source applies to electrolysis loop is 260～270Hz, and forward voltage amplitude is 330～350V, and pulsewidth is 0.6ms, and negative voltage amplitude is 580～600V, and pulsewidth is 0.4ms; Dutycycle is: forward dutycycle 10%, negative sense dutycycle 10%.The high frequency carrier voltage magnitude that applies is 70 ~ 90V, high frequent carrier frequency 2600Hz; Current density 4～10A/dm
2, oxidization time 180～200min, treatment temp is not higher than 40 ℃.
This aluminum alloy differential arc oxidation film there is good solidity to corrosion and excellent tribology performance, concrete performance index are as follows: thickness is 30 ~ 80 μ m, more than the neutral salt spray time reaches 2500h; Hardness is Hv1000; Dry friction coefficient f≤0.1), surface roughness Ra 0.02 μ m, bonding force is greater than 30MPa.
Embodiment 3
Material for test: LC4, size 100 * 100mm, Al alloy parts surface is placed in electrolytic solution as anode, and stainless steel is as negative electrode.Electrolyte ratio: sodium hydroxide 3 ~ 5g/L, water glass 4.5 ~ 5g/L, vanadic acid sodium 3.5～4.2g/L, Sodium orthomolybdate 0.2 ~ 0.4g/L, benzotriazole 0.5～0.7g/L, sodium malate 0.7～0.8g/L, cerous nitrate 0.8～1.1g/L, electrolyte ph is 5 ~ 8.Adopting Dole to examine the square wave pulse voltage frequency that special IV type great power pulse power source applies to electrolysis loop is 150 ~ 170Hz, and forward voltage amplitude is 250～270V, and pulsewidth is 0.6ms, and negative voltage amplitude is 590～610V, and pulsewidth is 0.4ms; Dutycycle is: forward dutycycle 10%, negative sense dutycycle 20%.The high frequency carrier voltage magnitude that applies is 120～130V, high frequent carrier frequency 2500Hz; Current density is controlled at 5.5 ~ 8.5A/dm
2, oxidization time 180～210min, treatment temp is not higher than 40 ℃.
This aluminum alloy differential arc oxidation film realize ultra-thin performance, there is good thermal insulation, solidity to corrosion and smooth finish simultaneously.Concrete performance index are as follows: thickness is 5 ~ 15 μ m, and low heat insulation (≤5%), the neutral salt spray time reaches 1800～2000h; The accelerated corrosion of sea water resistance copper is more than 2 years; Surface roughness Ra 0.01 μ m, bonding force is greater than 30MPa.
Embodiment 4
Material for test: 2A70, size 100 * 100mm, Al alloy parts surface is placed in electrolytic solution as anode, and stainless steel is as negative electrode.Electrolyte ratio: sodium hydroxide 3 ~ 5g/L, water glass 3.5～4.5g/L, Sodium Tetraborate 6.5 ~ 8g/L, vanadic acid sodium 3.5～4.5g/L, Sodium dodecylbenzene sulfonate 0.1～0.3g/L, Sodium decanoic acid 0.8～1.2g/L, sodium malate 0.7～0.9g/L, cerous nitrate 0.8～1.2g/L, Yttrium trinitrate 0.7 ~ 1.1g/L, electrolyte ph is 5 ~ 8.Adopting Dole to examine the square wave pulse voltage frequency that special IV type great power pulse power source applies to electrolysis loop is 280～300Hz, and forward voltage amplitude is 320～360V, and pulsewidth is 0.6ms, and negative voltage amplitude is 590～630V, and pulsewidth is 0.4ms; Dutycycle is: forward dutycycle 10%, negative sense dutycycle 30%.The high frequency carrier voltage magnitude that applies is 150 ~ 180V, high frequent carrier frequency 2700Hz; Current density is controlled at 7.5 ~ 11.5A/dm
2, oxidization time 200～220min, treatment temp is not higher than 40 ℃.
This aluminum alloy differential arc oxidation film realize super thick performance and superpower wear resistance.Concrete index is as follows: thickness 100～120 μ m, hardness is 5 times of hard oxygen, 3 times of hard chromium).Bonding force is 50 ~ 70MPa.
Above-described embodiment is the present invention at aluminum alloy surface embodiment preferably; but embodiments of the present invention are not restricted to the described embodiments; other any changes of not doing under spirit of the present invention and principle, modification, substitute, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (6)
1. the method for an aluminum alloy surface micro-arc oxidation films functionalized design, it is characterized in that: first the method is placed in electrolytic solution by Al alloy parts, pending workpiece surface in electrolytic solution as working electrode, stainless steel conductor is as to electrode, and forms electrolysis loop with described workpiece surface; Then to described electrolysis loop, apply square wave pulse voltage and high frequency carrier carries out oxide treatment to workpiece surface, current density is controlled at 0.2-20A/dm simultaneously simultaneously
2between, the treatment time is 30～200min, treatment temp is not higher than 50 ℃.
2. the method for aluminum alloy surface micro-arc oxidation films functionalized design according to claim 1, is characterized in that: its solvent of described electrolytic solution is water, solute by basis form, supplementary additive and densification additive form; Described base set becomes one or more in sodium hydroxide, silicate, borate and phosphoric acid salt; Supplementary additive is one or more in vanadate, molybdate, dodecylbenzene sulfonate, caprate, benzotriazole, malate; Densification additive is one or more in Yttrium trinitrate, cerous nitrate, lanthanum nitrate.
3. the method for aluminum alloy surface micro-arc oxidation films functionalized design according to claim 2, is characterized in that: the total concn of described solute is 1-20g/L, and the pH value of controlling electrolytic solution is 5 ~ 8.
4. the method for aluminum alloy surface micro-arc oxidation films functionalized design according to claim 1, it is characterized in that: described square wave pulse voltage frequency is 100～400Hz, forward amplitude is 250-400V, and pulsewidth is 0.6ms, negative voltage amplitude is 450-700V, and pulsewidth is 0.4ms.Described high frequency carrier voltage magnitude is 50-300V, and high frequent carrier frequency is 2000-3000Hz.
5. the method for aluminum alloy surface micro-arc oxidation films functionalized design according to claim 4, is characterized in that: the dutycycle of described square wave pulse voltage is one of following four kinds of situations: 1) forward dutycycle 0%, negative sense dutycycle 0%; 2) forward dutycycle 10%, negative sense dutycycle 10%; 3) forward dutycycle 10%, negative sense dutycycle 20%; 4) forward dutycycle 10%, negative sense dutycycle 30%.
6. the method for aluminum alloy surface micro-arc oxidation films functionalized design according to claim 1, is characterized in that: described aluminium alloy is LY11, LY12, LC4,2A70, ZL205, LY16,2024,5083,6063 or fine aluminium.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106757260A (en) * | 2016-11-22 | 2017-05-31 | 中国科学院金属研究所 | A kind of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film its application |
| CN108431934A (en) * | 2015-12-22 | 2018-08-21 | 应用材料公司 | The corrosion-resistant coating of semiconductor processing equipment |
| 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 |
| CN112575358A (en) * | 2020-11-27 | 2021-03-30 | 广东电网有限责任公司佛山供电局 | Aluminum-plated steel surface corrosion-resistant micro-arc oxidation film layer and preparation method and application thereof |
| CN112853360A (en) * | 2020-12-31 | 2021-05-28 | 安徽百圣鑫金属科技有限公司 | Aluminum alloy surface treatment method |
| CN113106516A (en) * | 2021-03-15 | 2021-07-13 | 中国科学院金属研究所 | Method for improving compactness of aluminum alloy micro-arc oxidation film by regulating negative electric parameters |
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| CN101230475A (en) * | 2007-11-05 | 2008-07-30 | 南昌航空大学 | Aluminum alloy differential arc oxidation batch production technique |
| CN101270495A (en) * | 2008-04-21 | 2008-09-24 | 华南理工大学 | Method for preparing corrosion protection abrasion resistant ceramic coating with alloy surface differential arc oxidization |
| CN102553814A (en) * | 2010-12-31 | 2012-07-11 | 中国科学院金属研究所 | Wave-absorbing functional protecting coating on surface of aluminum alloy and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108431934A (en) * | 2015-12-22 | 2018-08-21 | 应用材料公司 | The corrosion-resistant coating of semiconductor processing equipment |
| CN106757260A (en) * | 2016-11-22 | 2017-05-31 | 中国科学院金属研究所 | A kind of composite Nano electrolyte for preparing micro-arc oxidation of aluminum alloy surface film its application |
| 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 |
| CN112575358A (en) * | 2020-11-27 | 2021-03-30 | 广东电网有限责任公司佛山供电局 | Aluminum-plated steel surface corrosion-resistant micro-arc oxidation film layer and preparation method and application thereof |
| CN112853360A (en) * | 2020-12-31 | 2021-05-28 | 安徽百圣鑫金属科技有限公司 | Aluminum alloy surface treatment method |
| CN113106516A (en) * | 2021-03-15 | 2021-07-13 | 中国科学院金属研究所 | Method for improving compactness of aluminum alloy micro-arc oxidation film by regulating negative electric parameters |
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