CN102586827A - Method for preparing tin-nickel alloy coating on surface of magnesium alloy - Google Patents
Method for preparing tin-nickel alloy coating on surface of magnesium alloy Download PDFInfo
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- CN102586827A CN102586827A CN201110006778XA CN201110006778A CN102586827A CN 102586827 A CN102586827 A CN 102586827A CN 201110006778X A CN201110006778X A CN 201110006778XA CN 201110006778 A CN201110006778 A CN 201110006778A CN 102586827 A CN102586827 A CN 102586827A
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Abstract
The invention provides a method for preparing a tin-nickel alloy coating on the surface of magnesium alloy in the field of processing of the surface of the magnesium alloy. The method comprises the steps of grinding and polishing, ultrasonic oil removal, alkali washing, acid washing, activation, zinc galvanizing, and washing between the steps. The method further comprises a step of carrying out zinc electro-deposition and tin-nickel alloy electro-deposition on the magnesium alloy processed by the steps. The invention solves the problems that the magnesium alloy has poor corrosion resistance, is easy to oxidize in the air and the electro-deposition is difficult to directly carry out on the surface of the magnesium alloy. The method has the characteristics that plating solution has high stability; the obtained coating has good electrochemical property, good weldability, high corrosion resistance and strong decorativeness. Not only is the cost obviously reduced and the application field of the magnesium alloy is widened, but also the process flow is simple, the steps are easy to control, the production efficiency is improved and the obtained coating is suitable for industrial production. The product prepared by the method has excellent performance, low cost, high benefit and a wide application prospect and is suitable to popularization.
Description
Technical field:The present invention relates to the method that a kind of Mg alloy surface prepares alloy layer, the method for the protecting decorative coating of specifically strong and good decorative property in Mg alloy surface deposition solidity to corrosion.
Background technology:Magnesiumalloy is as a kind of alloy in lightweight material; Compare with current main flow material that magnesiumalloy has that density is little, specific tenacity is high, castibility is strong, capability of electromagnetic shielding is good and good characteristics such as recyclable, be widely used in industries such as aerospace, the vehicles, opticinstrument, telecommunications, computingmachine at present.Though the Application of Magnesium prospect is comparatively extensive, the shortcoming of its solidity to corrosion difference is seriously restricting Application of Magnesium and popularization.Therefore will enlarge the Application of Magnesium scope, the solidity to corrosion that improves magnesiumalloy becomes the problem of a key.From domestic and international research, the application surface treatment technology is to improve its solidity to corrosion effective means the most.Surface treatment method is divided into surface-treated and top coat treatment technology; Mainly comprise metallic coating, anodic oxidation, chemical conversion, vapour deposition, laser modified etc.; A part of method is applied in industry, but most methods also is in exploration and improvement stage.Magnesium alloy surface protective property coating respectively has its relative merits.The chemical conversion film less investment, but the ununiformity of Mg alloy surface is that formation is even, the greatest difficulty of the conversion rete of atresia, and the corrosion resistance nature and the crocking resistance that transform rete in addition are all not enough so that its use separately under mal-condition.Anodic oxidation is the surface treatment method that is widely used in magnesiumalloy, but the corrosion resisting property of gained rete is still waiting raising, and surface film is very crisp, non-conductive, so be not suitable for the application scenario that load maybe need be conducted electricity.Vapour deposition, laser modified method compare environmental protection, but its facility investment is bigger, and the rete preparation cost is high.Though the electroless plating cost is lower, plating bath is stable inadequately and harmful to toxic elements in human body, also need carry out strict sealing treatment.
Summary of the invention:The object of the present invention is to provide a kind of method for preparing tin-nickel alloy coating at Mg alloy surface.Mainly be to overcome the deficiency that prior art exists; A kind of simple and effective surface treatment method of Mg alloy is provided, Mg alloy surface form the surface even, corrosion-resistant strong, have satisfactory electrical conductivity, weldability and have graceful outward appearance and good, the low-cost coating of bath stability.
The method for preparing tin-nickel alloy coating at Mg alloy surface of the present invention: promptly be that a kind of magnesiumalloy prepares the electrodepositing zinc transition layer under the electrodepositing zinc plating bath, under tin-nickel electrolytic plating liquid, prepare the method for galvanic deposit tin-nickel alloy coating then.It comprises: sanding and polishing, ultrasonic oil removing, alkali cleaning, pickling, activation, soak the washing between zinc step and each step, comprise that also the magnesiumalloy after above-mentioned steps handled carries out the step of electrodepositing zinc and galvanic deposit tin-nickel alloy.
The present invention compared with prior art has the following advantages and positively effect:
1, the present invention combines traditional electroplating technology with modern technologies; Develop a kind of at the omnidistance nontoxic electrodeposition technology of Mg alloy surface; Solved the problem of environmental pollution that brings in plating bath, coating performance instability and the production; Demonstrate fully the chemical research theory of new generation of environmental protection, compared with prior art had outstanding substantive distinguishing features and obvious improvement.
2, the present invention is being through soaking on the zinc-base plinth that electrodepositing zinc prepares transition layer and with this alternative cyaniding coating, effectively overcome directly the difficulty in the Mg alloy surface galvanic deposit.And can cover the defective on magnesium matrix surface, this transition layer can make magnesium matrix and follow-up coating combine closely, and creates good conditions for obtaining ideal coating.
3, the present invention has taked the technical scheme at the Mg alloy surface galvanic deposit tin-nickel alloy that forms the zinc transition layer; The solidity to corrosion and the wear resistance of magnesiumalloy are significantly improved; Its decorate properties also is fully reflected, and it is deficient to have solved the nickel resources that the long-term widespread use to this traditional decoration property material of nickel brings, thereby makes expensive that the price of nickel rises steadily and cause; It with tin-nickel alloy coating as being applied to material protection for nickel coatings; Obviously reduce cost, increased income, more improved graceful ornamental of weldability and the outward appearance of product; Simultaneously also widen the Application of Magnesium field, had more outstanding substantive distinguishing features and obvious improvement.
4, technical process of the present invention is simple, and step is easy to control, enhances productivity, and is fit to suitability for industrialized production.Excellent product performance, chemical property by the present invention's preparation is good, the cost poor benefit high,
Have a extensive future, suit to promote.
Description of drawings:
Fig. 1 is the surface topography map at Mg alloy surface dc electrodeposition zinc transition layer;
Fig. 2 is the surface topography map at Mg alloy surface pulse electrodeposition zinc transition layer;
Fig. 3 is the surface topography map behind Mg alloy surface galvanic deposit tin-nickel alloy:
Fig. 4 is magnesiumalloy pulse zinc and galvanic deposit tin-nickel alloy layer electrochemical tests figure.
Embodiment:Of the present inventionly prepare the method for tin-nickel alloy coating, form by sanding and polishing (1), ultrasonic oil removing (2), alkali cleaning (3), pickling (4) activation (5), the washing process step of soaking between zinc (6), electrodepositing zinc (7), galvanic deposit tin-nickel alloy (8) and each step at Mg alloy surface.
Sanding and polishing (1): be with 600
#, 1500
#Waterproof abrasive paper is polished to magnesium alloy workpiece successively, makes it smooth smooth, tentatively removes surface film oxide.
Ultrasonic oil removing (2): adopt acetone at room temperature to clean 10 min.If whole substrate surface hydrophilic, the no globule or nonwettable place, then oil removing is qualified.
Alkali cleaning (3): further oil removing under alkaline condition after the preliminary oil removing of acetone, transformation has taken place in the surface film oxide of magnesium, and magnesium oxide films changes the Marinco H film into and makes magnesiumalloy be in passivation region, has stoped the corrosion of magnesiumalloy in the oil removing operation.This alkaline cleaning formulation and parameter are: sodium hydroxide 50g/L, sodium phosphate 10g/L, 70 ℃-80 ℃ of temperature, alkali cleaning time are 10 min.
Pickling (4): the wetting flat surface of pickling ability, oil removing, degreasing, removal oxide on surface expose magnesium alloy substrate, form the oxide compound that is easy to remove and form hot spot, strengthen mechanical interlock to improve bonding force.Said pickle solution prescription and processing parameter are: oxalic acid 10g/L, pickling 1min under the room temperature.
Activation (5): after handling, avoid that magnesiumalloy can generate sull or passivation film rapidly again in the extremely short time, therefore need carry out activation treatment through former procedures.Making Mg alloy surface produce one deck Sellaite protective membrane stops magnesium matrix to avoid the further corrosion of treatment solution.This activation treatment prescription and parameter are: phosphoric acid (85%) 20%, hydrogen fluoride ammonia 100g/L handles 1min under the room temperature.
Soak zinc (6): good zinc-impregnating layer can with magnesium matrix and follow-up coating good combination, and can cover the magnesium matrix surface imperfection, help to obtain ideal coating.The prescription and the processing parameter that soak the zinc process are: zinc sulfate 50g/L, trisodium phosphate 120g/L, Sodium Fluoride 5g/L, yellow soda ash 5g/L, 70 ℃-80 ℃ of temperature, time 10min, pH value 10.2-10.4.
Electrodepositing zinc (7): be to immerse in the electrodepositing zinc plating bath and handle with soaking magnesiumalloy behind the zinc.It promptly is that dc electrodeposition or pulse electrodeposition can be chosen one of which wantonly that dual mode is arranged.When utilizing dc electrodeposition, bath pH value is 7-9, and temperature is controlled at 40-50 ℃, and the treatment time is 15-20min, current density 4-6A/dm
2When adopting pulse electrodeposition, remove pulse-repetition 500Hz, pulse duty factor 20% outer other processing condition are identical with said dc electrodeposition condition.Said electrodepositing zinc plating bath is made up of sodium hydroxide 90-110g/L, zinc oxide 8-15g/L, trolamine 15-30g/L, DEP-III 4-6 ml/L.Specific embodiment sees following table 1 for details.
Table 1 electrodepositing zinc plating bath proportioning and electrodeposition condition
Said galvanic deposit tin-nickel alloy (8): be the magnesium alloy workpiece behind electrodepositing zinc (7) to be put into tin-nickel alloy solution carry out electrodeposition process.The pH value is 7-9 in the treating processes, and temperature is controlled at 40-50 ℃, and the time decides according to thickness of coating, is generally 15-20min.Current density: 1.0-2.0 A/dm
2
Said galvanic deposit tin-nickel alloy solution is made up of potassium pyrophosphate 250-300g/L, single nickel salt 35-50g/L, tin protochloride 30-45g/L, additive 1-4g/L.Particular case sees following table 2 for details.
Table 2 galvanic deposit tin-nickel alloy solution ratio and electrodeposition condition
Washing between said each step is to adopt deionized water rinsing.
In order to show the prepared performance of products of the present invention, we utilize S-570 type sem (SEM) to observe the surface topography of coating.Surface topography map by Fig. 1 magnesiumalloy dc electrodeposition zinc transition layer (this coating is table 1 the 2nd coating that assembly side obtains); Fig. 2 is that the surface topography map of magnesiumalloy pulse electrodeposition zinc transition layer (this coating is table 1 the 2nd coating that assembly side obtains) can find out that the surface topography of pulse coating compares with direct current coating, and hole obviously reduces, the obvious refinement of the crystal grain of coating.Adopting pulse electrodeposition zinc to be more suitable for doing transition layer than dc electrodeposition zinc is applied in the magnesiumalloy electrodeposition process tin-nickel alloy.And Fig. 3 does the transition layer surface topography map of galvanic deposit tin-nickel alloy (the 3rd coating that assembly side is obtained in the table 2) again with pulse electrodeposition zinc; Can find out smooth, the even compact of coating surface; Can obviously improve the solidity to corrosion of magnesiumalloy, and further confirmed (seeing the Tafel curve of Fig. 4 coating in 3.5% sodium chloride solution) through the corrosion resisting property of matrix and two kinds of coating electrokinetic potential polarization curve evaluation coating.All electro-chemical tests all adopt Dutch Autolab electrochemical workstation among Fig. 4, in the neutral etchant solution of 3.5wt.% sodium-chlor, under room temperature (25 ℃), carry out.Polarization curve is a working electrode with the sample, and platinum electrode is a counter electrode, and SCE is a reference electrode; The polarization curve sweep velocity is 1mV/s, under open circuit voltage, soaks 10min before the test, and is stable to guarantee test process.Test result sees the following form 3.
Table 3
Further show through test result: the solidity to corrosion through magnesiumalloy after the electrodepositing zinc obviously improves, and coating only has 5 μ m, and coating is thin but to have solidity to corrosion preferably.Because magnesiumalloy belongs to difficult plating metal, tin-nickel alloy directly galvanic deposit to magnesium alloy substrate.Before the galvanic deposit tin-nickel alloy, electrodepositing zinc can make tin-nickel alloy be easy to galvanic deposit to magnesiumalloy and combine firmly to be integrally formed.Be improved once more through solidity to corrosion behind the galvanic deposit tin-nickel alloy, thickness of coating reaches 12 μ m, and visible process galvanic deposit tin-nickel alloy is significantly strengthened corrosion stability of magnesium alloy.And all embodiment all reach national 1 grade standard of film adhesive testing standard GB/T9286-1998.
Claims (3)
1. method for preparing tin-nickel alloy coating at Mg alloy surface; It comprises sanding and polishing (1), ultrasonic oil removing (2), alkali cleaning (3), pickling (4) activation (5), soaks the washing between zinc (6) step and each step, it is characterized in that: this method also comprises the step of the magnesiumalloy after the above-mentioned steps processing being carried out electrodepositing zinc (7) and galvanic deposit tin-nickel alloy (8).
2. the method for preparing tin-nickel alloy coating at Mg alloy surface according to claim 1; It is characterized in that: said electrodepositing zinc (7) is that the magnesiumalloy after soaking zinc (6) art breading is immersed by zinc oxide 8-15g/L; Sodium hydroxide 90-110g/L handles in the electrodepositing zinc plating bath that trolamine 15-30g/L, DEP-III 4-6 ml/L form.
3. according to claim 1ly prepare the method for tin-nickel alloy coating at Mg alloy surface, it is characterized in that: said galvanic deposit tin-nickel alloy (8) is that the magnesiumalloy after electrodepositing zinc (7) is handled immerses in the solution of being made up of potassium pyrophosphate 250-300g/L, single nickel salt 35-50g/L, tin protochloride 30-45g/L, Padil 1-4g/L again and handles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849912A (en) * | 2012-11-29 | 2014-06-11 | 沈阳工业大学 | Electroplating technology of shining tin zinc nickel alloy |
| CN108301026A (en) * | 2018-02-05 | 2018-07-20 | 上海应用技术大学 | A kind of plating solution and electroplating technology of Bright Sn-ni Alloys |
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| CN101148762A (en) * | 2007-11-12 | 2008-03-26 | 湖南大学 | One-step acid washing activating plating pre-processing technique for magnesium alloy surface |
| CN101748450A (en) * | 2010-01-14 | 2010-06-23 | 杭州顿力实业有限公司 | EDP environmental-friendly zinc plating solution and preparation method |
| CN101857965A (en) * | 2009-04-10 | 2010-10-13 | 吉林师范大学 | Method for depositing zinc and zinc-nickel alloy on surface of magnesium alloy without cyanogen or fluorine |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4282073A (en) * | 1979-08-22 | 1981-08-04 | Thomas Steel Strip Corporation | Electro-co-deposition of corrosion resistant nickel/zinc alloys onto steel substrates |
| CN1037178A (en) * | 1988-04-25 | 1989-11-15 | 东北工学院 | Electro-galvanizing is with making up brightening agent |
| CN1678428A (en) * | 2002-07-24 | 2005-10-05 | 克里斯铝轧制品有限公司 | Brazing product and method of manufacturing a brazing product |
| CN101148762A (en) * | 2007-11-12 | 2008-03-26 | 湖南大学 | One-step acid washing activating plating pre-processing technique for magnesium alloy surface |
| CN101857965A (en) * | 2009-04-10 | 2010-10-13 | 吉林师范大学 | Method for depositing zinc and zinc-nickel alloy on surface of magnesium alloy without cyanogen or fluorine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849912A (en) * | 2012-11-29 | 2014-06-11 | 沈阳工业大学 | Electroplating technology of shining tin zinc nickel alloy |
| CN108301026A (en) * | 2018-02-05 | 2018-07-20 | 上海应用技术大学 | A kind of plating solution and electroplating technology of Bright Sn-ni Alloys |
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Application publication date: 20120718 |