CN102321906A - A kind of preparation method of Mg alloy surface composite film and solution formula thereof - Google Patents
A kind of preparation method of Mg alloy surface composite film and solution formula thereof Download PDFInfo
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Abstract
A kind of preparation method of Mg alloy surface composite film and solution formula thereof; The step of its method is: (1) the cleaned magnesium alloy workpiece of will polishing places and contains desire and infiltrate the electrolytic solution of element and carry out the plasma electrolysis osmotic treated earlier, forms to contain on its surface and infiltrates the surface reforming layer that element distributes; (2) again processed workpiece is cleaned after, be placed on and carry out plasma electrolytic oxidation in the alkaline electrolyte and handle, obtain at workpiece surface finally that hardness is high, anti-corrosion, wear-resistant, the composite film of the excellent combination property of antifriction.The prescription of its solution is that the electrolytic solution when carrying out the plasma electrolytic oxidation processing consists of and contains the compd A that desire is infiltrated Elements C, N, B, S: 10-140g/L, sodium hydroxide: 2-30g/L; Compd A is the combination of one or more materials in methane amide, urea, thanomin, borax, the thiocarbamide.
Description
Technical field
The present invention relates to the surface modifying method of magnesiumalloy.
Background technology
The main method of present nonferrous alloy material surface modifying both domestic and external has: thermospray, electroless plating, plating, organism coating, thermodiffusion, vapour deposition, high energy beam surface-treated, chemical conversion, anodic oxidation, plasma electrolytic oxidation etc.Surface Engineering new technology-plasma electrolysis deposition technique can be divided into plasma electrolysis infiltration technology and two branches of plasma electrolytic oxidation technology; Wherein plasma electrolytic oxidation is a kind of advanced person's of on anodised basis, growing up a process for treating surface; Be mainly used on the nonferrous alloy such as aluminium, magnesium, titanium; Can be directly at its surface in situ growth one deck pottery sull, with similar compared with techniques, the performance of handling the gained workpiece surface improves a lot.And the plasma electrolysis infiltration is to realize the ion implantation of elements such as nitrogen, carbon and metal at workpiece surface, thereby carries out the new technology of surface-treated, but is mainly used in the surface-treated field of ferrous metal.It is ion implantation with high energy beam, the thermo-chemical treatment plasma injects permeating method and compares, have efficient height, cost low, can the processed complex workpiece etc. advantage.Be that plasma electrolysis sedimentary two big branch technique are all used respectively at present, these two kinds of technology be not applied to simultaneously the public reported of ferrous metal or nonferrous alloy in the document.
In order further to improve the protective capacities of metal material surface, investigators begin various combination through above surface modifying method at the excellent composite film of metal material surface processability.With the plasma electrolytic oxidation technology that the present invention relates to is example; Existing complex method is through in electrolytic solution, adding functional particles; Under the effect of plasma electrolytic oxidation; The codeposition of ceramic phase in realization and the rete; Perhaps make composite package through the pottery sull being carried out processing such as follow-up thermospray, physical vapor deposition, electroless plating, plating, but these complex methods exist that technology is loaded down with trivial details, cost is high, restive, can not the complicated problems such as workpiece of machining shape, be difficult for realizing industrial applications.Also have the weak shortcoming of membranous layer binding force simultaneously, this is self to have the problem that the native defect of mechanical bond, molecular linkage combination is brought by these follow-up process for treating surface more.
Summary of the invention
The object of the present invention is to provide a kind of method and solution formula thereof for preparing the better composite package of over-all properties at Mg alloy surface.
The present invention is a kind of preparation method and solution formula thereof of Mg alloy surface composite film, and the step of its method is:
(1) the cleaned magnesium alloy workpiece of will polishing places and contains desire and infiltrate the electrolytic solution of element and carry out the plasma electrolysis osmotic treated earlier, forms to contain on its surface and infiltrates the surface reforming layer that element distributes;
(2) again processed workpiece is cleaned after, be placed on and carry out plasma electrolytic oxidation in the alkaline electrolyte and handle, obtain at workpiece surface finally that hardness is high, anti-corrosion, wear-resistant, the composite film of the excellent combination property of antifriction.
The solution formula that is used for the above preparing method's step (1), the electrolytic solution when carrying out the plasma electrolytic oxidation processing consist of and contain the compd A that desire is infiltrated Elements C, N, B, S: 10-140g/L, sodium hydroxide: 2-30g/L; Compd A is the combination of one or more materials in methane amide, urea, thanomin, borax, the thiocarbamide.
The solution formula that is used for the above preparing method's step (2) consists of sodium hydroxide carrying out the electrolytic solution of plasma electrolytic oxidation when handling, perhaps Pottasium Hydroxide: 2～40g/L, Potassium monofluoride: 5～30g/L, compd B: 10～50g/L; Compd B is the combination of one or more materials in silicate, borate, carbonate, aluminate, zirconates, titanate, molybdate, tungstate, vannadate, the manganate.
Plasma electrolysis sedimentary two big branch technique are all used respectively at present; Wherein the plasma electrolysis infiltration technology is mainly used in the surface-treated field of ferrous metal; And the plasma electrolytic oxidation technology is mainly used in the surface treatment aspect of nonferrous alloy such as aluminium, magnesium, titanium, these two kinds of technology is not applied to simultaneously the public reported of ferrous metal or nonferrous alloy in the document.The present invention is used for magnesiumalloy simultaneously with these two kinds of technology; And carry out the plasma electrolysis osmotic treated earlier; Form the surface reforming layer that contains the distribution of infiltration element earlier at material surface; And then carry out plasma electrolytic oxidation and handle, further generate the oxidation film layer of excellent performance, and the element that infiltrated in handling of the first step also to be participated in the chemical reaction of this moment and generate the high-quality thing and is present in the composite film mutually at material surface.Finally obtain at workpiece surface that hardness is high, wear-resistant, antifriction, high-quality composite film that solidity to corrosion is good.Therefore, advantage of the present invention is:
The advantage of binding plasma electrolysis infiltration of the present invention and two kinds of treatment process of plasma electrolytic oxidation has obtained the better composite film of over-all properties at magnesium alloy work-piece surface.Handle and to obtain the oxide compound and salt thereof of magnesium except containing plasma electrolytic oxidation in this composite film, have the high-quality thing phase of wear-resisting, anti-corrosion, high firmness, self-lubricating property in addition, like Si
3N
4, TiN, V
2N, AlN, SiC, B
4C, TiC, WC, V
2C, Mo
2C, SiB
4, TiB
2, MnB
2, MoS
2, WS
2Deng, therefore greatly improved the over-all properties of workpiece surface.Elements such as C, N, B, S infiltrate the regional existence of infiltration layer that forms during simultaneously owing to the first step plasma electrolysis osmotic treated, have both reduced the chemically reactive of film basal plane, have improved its solidity to corrosion, have also improved the supporting capacity of magnesium alloy work-piece surface.And the growth in situ characteristic when ion implantation characteristic during owing to the plasma electrolysis infiltration and plasma electrolytic oxidation also is greatly improved the bonding strength between film basal plane and the rete.
The content of high-quality thing phase and kind can be controlled through processing parameter and solution formula in the composite film.
The workpiece polishing is cleaned the back and just can be handled, and does not have such loaded down with trivial details pre-treating technology such as plating, electroless plating.
It is on same power unit, to accomplish that two steps of workpiece handle, and all is in liquid phase environment, to carry out.This technology is simple, efficient is high, does not also receive the restriction of workpiece shape, can process complex contour and have the workpiece of inner chamber, and solutions employed is pollution-free, cost is low.
Description of drawings
Fig. 1 is the XRD spectra of the pottery composite film that obtains of AZ91D magnesiumalloy.
Embodiment
The present invention is a kind of preparation method and solution formula thereof of Mg alloy surface composite film, and its method steps is:
(1) the cleaned magnesium alloy workpiece of will polishing places and contains desire and infiltrate the electrolytic solution of element and carry out the plasma electrolysis osmotic treated earlier, forms to contain on its surface and infiltrates the surface reforming layer that element distributes;
(2) again processed workpiece is cleaned after, be placed on and carry out plasma electrolytic oxidation in the alkaline electrolyte and handle, obtain at workpiece surface finally that hardness is high, anti-corrosion, wear-resistant, the composite film of the excellent combination property of antifriction.
According to above-described preparation method; When carrying out the plasma electrolysis osmotic treated, magnesium alloy workpiece is connected on the electrode of power supply, treating processes voltage is 150～400V, and frequency is 500～800HZ; Dutycycle is 20～90%, and the treatment time is 10～90min.
According to above-described preparation method; When carrying out the plasma electrolytic oxidation processing; The magnesium alloy workpiece that passes through the plasma electrolysis osmotic treated is connected on the anode of power supply, and treating processes voltage is 200～450V, and frequency is 600～900HZ; Dutycycle is 10～50%, and the treatment time is 10～60min.
The solution formula that is used for the above preparing method's step (1), the electrolytic solution when carrying out the plasma electrolytic oxidation processing consist of and contain the compd A that desire is infiltrated Elements C, N, B, S: 10-140g/L, sodium hydroxide: 2-30g/L; Compd A is the combination of one or more materials in methane amide, urea, thanomin, borax, the thiocarbamide.
The solution formula that is used for the above preparing method's step (2) consists of sodium hydroxide carrying out the electrolytic solution of plasma electrolytic oxidation when handling, perhaps Pottasium Hydroxide: 2～40g/L, Potassium monofluoride: 5～30g/L, compd B: 10～50g/L; Compd B is the combination of one or more materials in silicate, borate, carbonate, aluminate, zirconates, titanate, molybdate, tungstate, vannadate, the manganate.
Further launch the present invention below in conjunction with embodiment.
Embodiment 1
Handling sample is as cast condition AZ91D magnesiumalloy; Be cut into disk, specification is
The concrete operations step is:
1. sample pretreatment: sample successively through 400 orders, 800 orders, 1500 purpose sand paperings, is cleaned with zero(ppm) water.
2. sample carries out the plasma electrolysis osmotic treated earlier: sample is connected to power electrode, place to consist of methane amide 20ml/L, and in the solution of sodium hydroxide 2g/L, control voltage: 200V, frequency: 600HZ, dutycycle 50%, treatment time 30min.
3. sample carries out the plasma electrolytic oxidation processing: after the sample process plasma electrolysis osmotic treated, clean, be connected to power anode, place to consist of water glass 25g/L with zero(ppm) water, and sodium aluminate 7g/L, sodium hydroxide 2g/L is in the solution of Potassium monofluoride 20g/L.Control voltage: 350V, frequency: 700HZ, dutycycle 40%, treatment time 10min.Finally obtaining thickness at sample surfaces is the composite film of 20-25 μ m.
Embodiment 2
Handling sample is as cast condition AZ91D magnesiumalloy; Be cut into disk, specification is
The concrete operations step is:
1. sample pretreatment: sample successively through 400 orders, 800 orders, 1500 purpose sand paperings, is cleaned with zero(ppm) water.
2. sample carries out the plasma electrolysis osmotic treated earlier: sample is connected to power electrode, places to consist of methane amide 50ml/L, thiocarbamide 40g/L; In the solution of sodium hydroxide 5g/L, control voltage: 330V, frequency: 700HZ; Dutycycle 20%, treatment time 50min.
3. sample carries out the plasma electrolytic oxidation processing: after the sample process plasma electrolysis osmotic treated, clean with zero(ppm) water, be connected to power anode; Place to consist of water glass 15g/L Sodium orthomolybdate 5g/L, sodium wolframate 7g/L; Pottasium Hydroxide 6g/L is in the solution of Potassium monofluoride 13g/L.Control voltage: 400V, frequency: 700HZ, dutycycle 20%, treatment time 30min.As shown in Figure 1, finally obtaining thickness at sample surfaces is the composite film of 30-34 μ m.
Claims (5)
1. the preparation method of a Mg alloy surface composite film the steps include:
(1) the cleaned magnesium alloy workpiece of will polishing places and contains desire and infiltrate the electrolytic solution of element and carry out the plasma electrolysis osmotic treated earlier, forms to contain on its surface and infiltrates the surface reforming layer that element distributes;
(2) again processed workpiece is cleaned after, be placed on and carry out plasma electrolytic oxidation in the alkaline electrolyte and handle, obtain at workpiece surface finally that hardness is high, anti-corrosion, wear-resistant, the composite film of the excellent combination property of antifriction.
2. preparation method according to claim 1; It is characterized in that: when carrying out the plasma electrolysis osmotic treated, magnesium alloy workpiece is connected on the electrode of power supply; Treating processes voltage is 150～400V; Frequency is 500～800HZ, and dutycycle is 20～90%, and the treatment time is 10～90min.
3. preparation method according to claim 1; It is characterized in that: when carrying out the plasma electrolytic oxidation processing; The magnesium alloy workpiece that passes through the plasma electrolysis osmotic treated is connected on the anode of power supply, and treating processes voltage is 200～450V, and frequency is 600～900HZ; Dutycycle is 10～50%, and the treatment time is 10～60min.
4. the solution formula that is used for the said preparing method's of claim 1 step (1); It is characterized in that: the electrolytic solution when carrying out the plasma electrolytic oxidation processing consists of and contains the compd A that desire is infiltrated Elements C, N, B, S: 10-140g/L, sodium hydroxide: 2～30g/L; Compd A is the combination of one or more materials in methane amide, urea, thanomin, borax, the thiocarbamide.
5. the solution formula that is used for the said preparing method's of claim 1 step (2); It is characterized in that: the electrolytic solution when carrying out the plasma electrolytic oxidation processing consists of sodium hydroxide; Perhaps Pottasium Hydroxide: 2～40g/L, Potassium monofluoride: 5～30g/L, compd B: 10～50g/L; Compd B is the combination of one or more materials in silicate, borate, carbonate, aluminate, zirconates, titanate, molybdate, tungstate, vannadate, the manganate.
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Cited By (7)
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| CN103320841A (en) * | 2013-05-10 | 2013-09-25 | 上海理工大学 | Formula and application method of magnesium alloy micro-arc oxidation solution |
| CN103938254A (en) * | 2014-04-02 | 2014-07-23 | 兰州空间技术物理研究所 | Preparation method of connecting corrosion-resisting micro-arc oxidation layer on surface of magnesium alloy |
| CN105839165A (en) * | 2016-04-20 | 2016-08-10 | 深圳八六三计划材料表面技术研发中心 | Austenitic stainless steel and treatment method for improving hardness and corrosion resistance |
| CN107937965A (en) * | 2017-12-18 | 2018-04-20 | 嘉兴学院 | A kind of magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN108048893A (en) * | 2017-12-18 | 2018-05-18 | 嘉兴学院 | A kind of environmental-protection type magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN110773215A (en) * | 2018-07-31 | 2020-02-11 | 哈尔滨工业大学 | Method for preparing transition metal carbonitride material ceramic film layer efficient OER catalyst by aqueous phase plasma vapor deposition method |
| CN114107881A (en) * | 2021-11-15 | 2022-03-01 | 湖南弘辉科技有限公司 | High-speed fan blade machining process |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320841A (en) * | 2013-05-10 | 2013-09-25 | 上海理工大学 | Formula and application method of magnesium alloy micro-arc oxidation solution |
| CN103320841B (en) * | 2013-05-10 | 2015-12-23 | 上海理工大学 | A kind of magnesium alloy differential arc oxidation solution formula and application method thereof |
| CN103938254A (en) * | 2014-04-02 | 2014-07-23 | 兰州空间技术物理研究所 | Preparation method of connecting corrosion-resisting micro-arc oxidation layer on surface of magnesium alloy |
| CN105839165A (en) * | 2016-04-20 | 2016-08-10 | 深圳八六三计划材料表面技术研发中心 | Austenitic stainless steel and treatment method for improving hardness and corrosion resistance |
| CN107937965A (en) * | 2017-12-18 | 2018-04-20 | 嘉兴学院 | A kind of magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN108048893A (en) * | 2017-12-18 | 2018-05-18 | 嘉兴学院 | A kind of environmental-protection type magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN108048893B (en) * | 2017-12-18 | 2019-07-16 | 嘉兴学院 | A kind of environmental-protection type magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN107937965B (en) * | 2017-12-18 | 2019-07-23 | 嘉兴学院 | A kind of magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN110773215A (en) * | 2018-07-31 | 2020-02-11 | 哈尔滨工业大学 | Method for preparing transition metal carbonitride material ceramic film layer efficient OER catalyst by aqueous phase plasma vapor deposition method |
| CN110773215B (en) * | 2018-07-31 | 2022-09-09 | 哈尔滨工业大学 | Method for preparing high-efficiency OER catalyst of transition metal carbonitride material ceramic film layer by plasma deposition method |
| CN114107881A (en) * | 2021-11-15 | 2022-03-01 | 湖南弘辉科技有限公司 | High-speed fan blade machining process |
| CN114107881B (en) * | 2021-11-15 | 2023-07-25 | 湖南弘辉科技有限公司 | High-speed fan blade processing technology |
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Application publication date: 20120118 |