CN101161866B - Method for preparing magnesium and magnesium alloy surface coating - Google Patents
Method for preparing magnesium and magnesium alloy surface coating Download PDFInfo
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- CN101161866B CN101161866B CN2007100316502A CN200710031650A CN101161866B CN 101161866 B CN101161866 B CN 101161866B CN 2007100316502 A CN2007100316502 A CN 2007100316502A CN 200710031650 A CN200710031650 A CN 200710031650A CN 101161866 B CN101161866 B CN 101161866B
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- arc oxidation
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Abstract
The present invention discloses a magnesium and magnesium alloy surface cladding preparation method which comprises the following procedures: a) the surface is cleaned up; b) electrolyte for micro-arc oxidation is a water-based solution, wherein, the concentration of sodium fluoride is between 1 g/L and 40 g/L; the concentration of sodium phosphate is between 1 g/L and 100 g/L; the sodium fluoride and the sodium phosphate can be used separately or in a combined way, or sodium hydroxide with the concentration between 0.05 g / L and 10 g / L is further added to use; c) the surface is treated by chemical plating and/or d) electroplating; water cleaning is only required among the procedures. The invention based on the knowledge of the related mechanism of plating technology and micro-arc oxidation technology makes the best of the advantages in particular that the micro-arc oxidation ceramic film has the characteristics of corrosion resistance and porosity, and combines the surface ceramic technology and the surface alloy technology organically and solves the problems of complex working procedures, high cost, large pollution, imperfect effect, etc., in the prior plating art. With the method provided by the invention, a cladding with uniformity, smoothness, a compact structure and excellent performance can be achieved.
Description
Technical field
The invention belongs to light alloy process for modifying surface field, relate in particular to the technology of preparing of a kind of magnesium and magnesium alloy surface coating.
Background technology
As everyone knows, in recent years, magnesium has the good reputation of " 21 century green engineering material " because of the extremely each side's favor of its resource, price and structure properties advantage.Especially be significant or the field of special technical requirement is arranged in " lightweight ", " environmental protectionization " in various fields; as industrial sectors such as aerospace, automobile, electronics, communication, military affairs, five metals; magnesium alloy has obtained the unprecedented application of scale as structured material; and its application space is also in continuous expansion; consumption increases rapidly, as magnesium alloy consumption annual growth in the global range up to 20%.However, up to now, the large-scale industrial application that magnesium alloy advantage peculiar with it matches still is unrealized, and traces it to its cause, and main bottleneck problem is a solidity to corrosion.On the other hand, the expansion of magnesium alloy Application Areas is to its military service demands for higher performance based on solidity to corrosion.Therefore, magnesium and magnesium alloy are carried out intensive treatment, strengthen its surface generalization barrier propterty, be the primary critical technical problems that magnesium alloy more must solve in the large-scale application process based on solidity to corrosion, significant.
As the important channel that solves the protection of magnesium and magnesium alloy and the problem of decoration, have many advantages based on electroless plating and the coating technology of electroplating.Around the plating problem of magnesium and magnesium alloy, relevant R﹠D work promptly began as far back as the 1950's.Through accumulation for many years, now obtained great successes/result.But because all many-sides such as cost, stability, environmental protection, these achievement/results still have a segment distance from industrial applications.As being soaked zinc method and Dow direct chemical nickel plating method by ASTM B480-68 of American Society for testing and materials and the standardized Dow of ASTM B480-88:Standard guide for preparation of magnesium and magnesium alloys forelectroplating (magnesium and magnesium alloy plating standard guide), though be the milestone on the magnesium coating technology development history, but no matter be Dow method or other improved technology, the ubiquity operation is numerous and diverse, it is big to pollute, effect outstanding problem such as ideal not to the utmost.Is example to soak the zinc method than Dow because of the Dow direct chemical nickel plating method that operation is simplified, pollution reduces extremely high praise, remove strict water wash procedures between conventional polishing, polishing and each operation, plating pre-treatment (general designations of pre-all processing of plating piece before entering the plating bath plating) still comprises alkali cleaning, pickling, chemical erosion and activation step, operation is very numerous and diverse, is unfavorable for industrial applications.In addition, because CrO
3, prussiate, hydrofluoric acid etc. use, environmental protection and health problem become another major obstacle of above-mentioned process application.
At the defective that the plating technic that with the Dow method is mother matrix especially plates pretreatment procedure, numerous scholars have carried out improving research, have obtained gratifying effect.It is representative that wherein Zhenmin Liu, Lee build medium people's work.As people such as Zhenmin Liu at " Applied Surface Science " 2006 the 253rd phase 2988-2991 pages or leaves, deliver the article that is entitled as " A novel process of electroless Ni-P plating with plasmaelectrolytic oxidation pretreatment ", reported research situation, and compared with the traditional chemical plating based on the magnesium alloy chemical plating of differential arc oxidation plating pre-treatment.Result of study shows, not only technology environmental protection of new technology, and also the quality of coating that obtains (comprising outward appearance, bonding force, solidity to corrosion) is higher, shows as the electrochemical polarization test result, and corrosion electric current density reduces nearly 2 orders of magnitude.Lee builds medium people at " Rare Metals Materials and engineering " 2007 36 volumes the 3rd phase 528-532 page or leaf, deliver the paper that is entitled as " research of magnesium alloy differential arc oxidation-electroless plating ", having introduced with the differential arc oxidation is main plating pretreatment technology, with single nickel salt is environmental-friendly magnesium alloy " floride-free acid " the electroless plating novel process of main salt, has obtained the good coating of overall quality.
Compare with traditional coating technology, the preparation of feeling free to try undoubtedly to magnesium and magnesium alloy surface coating that Zhenmin Liu and Lee build medium people provides new thinking.But according to the technological line that they provide, pre-plating piece is still needed and is carried out SnCl after handling through differential arc oxidation
2Sensitization, PdCl
2Activation and NaH
2PO
2Reduction is handled, and just can enter the plating operation, still has problems such as operation is numerous, cost height.
Summary of the invention
The present invention is directed to that the operation that exists in the existing coating technology is numerous and diverse, cost is high, pollutions is big, plating effect problem such as ideal not to the utmost, provide a kind of and plate the magnesium of pre-treatment and the preparation method of magnesium alloy surface coating based on differential arc oxidation.
The present invention is achieved by the following technical programs: the preparation method of a kind of magnesium and magnesium alloy surface coating may further comprise the steps:
A) surface dressing to magnesium and magnesium alloy polish successively, polishing and skimming treatment;
B) differential arc oxidation immerses magnesium and magnesium alloy in the differential arc oxidation electrolytic solution for preparing, and energising is carried out surface ceramic deposition and handled;
C) electroless plating will immerse the chemical plating fluid for preparing through the magnesium and the magnesium alloy of step b) differential arc oxidation, and control bath pH value and temperature are carried out the electroless plating plating, and plating time requires to decide because of thickness of coating;
D) electroplate and will immerse the electroplate liquid for preparing through the magnesium and the magnesium alloy of step b) differential arc oxidation or step c) electroless plating, control cathode current density and bath pH value and temperature are electroplated plating, and plating time requires to decide because of thickness of coating.
Magnesium and magnesium alloy are through above-mentioned steps b) wash after the differential arc oxidation, directly carry out electroless plating or plating after the washing.
The used electrolytic solution of step b) differential arc oxidation of the present invention is group water solution, concentration of sodium fluoride 1-40g/L wherein, and sodium phosphate concentration 1-100g/L, both independent or composite uses, or further to add concentration be that the sodium hydroxide of 0.05-10g/L uses.
After each operation of step a) surface dressing of the present invention, and c) electroless plating or d) electroplate after, magnesium and magnesium alloy are washed.
The purpose of step a) surface dressing of the present invention is to remove magnesium and magnesium alloy or its product surface at the burr of processing, transport, produce between the shelf lives, grease etc., obtains smooth, clean Surface.Surface dressing can be undertaken by any known or special close physics and/or chemical process in the prior art.For example: sand papering; The polishing cloth polishing; Organic solvent comprises direct or degreasing under the ultrasonic wave effect such as dehydrated alcohol, acetone or trieline, or the alkali cleaning degreasing.
Differential arc oxidation operational condition of the present invention such as voltage, current density, solution temperature and treatment time decide because of the requirement of ceramic membrane thickness, microtexture etc.
Electroless plating of the present invention or plating plating technology adopt in the prior art by known or specially close magnesium and magnesium alloy chemical plating electroplate liquid formulation and operational condition.Plating time requires to decide because of thickness of coating.
The purpose of washing of the present invention is to avoid the solution crossed contamination, and then influences treatment effect.Washing available tap water, distilled water or deionized water carries out.
Compared with prior art, advantage of the present invention is many-sided, and outstanding behaviours is aspect following two:
(1) integration advantage improves the quality and the present invention is based on understanding to coating technology and differential arc oxidization technique related mechanism, and the advantage of differential arc oxidation and coating technology is organic compound, for the surface strengthening of magnesium and magnesium alloy provides new approach.Utilize technology provided by the invention, can solve the plating problem of magnesium and magnesium alloy, for the plating process carry out smoothly and the preparation of high quality coating creates conditions.Particularly, adopt differential arc oxidization technique that pre-plating piece is plated pre-treatment, both utilized the solidity to corrosion of ceramic layer, especially the plating initial stage is not subjected to the plating bath excessive erosion in plating process subsequently for protection magnesium and magnesium alloy; Modes such as chemical constitution, thickness, porosity by the control ceramic layer again, assurance plating process is carried out smoothly, replacement(metathesis)reaction between the positively charged ion is carried out with controllable mode, for the initial formation of nickel nuclear with catalytic activity creates conditions, avoid the plating failure or because of plating the too fast quality of coating problem that causes of speed.Utilize method provided by the invention, can obtain the coating of uniform and smooth, compact structure, excellent property.Owing to have the existence of the arc differential oxide ceramic layer of insulation characterisitic in the middle of coating and the base metal, from the thermodynamics angle, greatly reduce the possibility that strong galvanic corrosion takes place under the service state when coating is destroyed, help further expanding magnesium and Application of Magnesium field.
(2) simplify working process to reduce cost and utilize technology provided by the invention, magnesium and magnesium alloy only need be washed after differential arc oxidation, directly carry out electroless plating after the washing or electroplate plating, intermediate process steps such as sensitization in the prior art, activation and reduction have been removed from, simplify operation greatly, reduced cost.On the other hand, owing to abandoning of high carcinogenic and high toxicity compound such as chromic anhydride and prussiate, severe corrosive and volatile compound such as hydrofluoric acid etc., plating technic greatly reduces the potential threat of ecotope, enterprise employee health and production unit.Moreover, because ceramic coating formed by micro-arc oxidation is relatively stable, utilize technology provided by the invention, stay the time can not do particular requirement to the sky between plating pre-treatment and the plating, therefore increased the handiness of plating production operation greatly.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The preparation method of magnesium of the present invention and magnesium alloy surface coating can have following three kinds of realization approach, that is: (1) surface dressing+differential arc oxidation+electroless plating; (2) surface dressing+differential arc oxidation+plating; (3) surface dressing+differential arc oxidation+electroless plating+plating.When preparation magnesium and magnesium alloy surface coating, can select suitable route according to concrete needs.
Below in conjunction with embodiment the present invention is described in further detail, presses table 1 prescription and Fig. 1 flow implementation.
Table 1: the plating technology that the embodiment of the invention is used
| Numbering | Electroplate liquid formulation and plating condition | The technology source |
| 01 | Basic nickel carbonate 10g/L | ASTM?B480-88 |
| Hydrofluoric acid (70mass%) 0.6vol% | ||
| Citric acid 5.2g/L | ||
| Ammonium bifluoride 10g/L | ||
| Inferior sodium phosphate 20g/L | ||
| Ammoniacal liquor (30mass%) 3.9vol% | ||
| Bath temperature: 77-82 ℃ | ||
| PH value of solution value: 5.5-6.3 (25 ℃) | ||
| 02 | Copper sulfate 150g/L | CN?1952215A |
| Diethylenetriamine 120ml/L | ||
| Ammonium sulfate 20g/L | ||
| Ammoniacal liquor 30ml/L | ||
| Hydrofluoric acid (40%) 20ml/L | ||
| Bath temperature: 50-60 ℃ | ||
| PH value of solution value: 8.0-9.5 | ||
| Cathode current density: 20-60mA/cm 2 |
Embodiment 1
By concentration 40g/L preparation NaF solution 2L, obtain differential arc oxidation electrolytic solution with distilled water.By the prescription requirement preparation chemical plating bath of No. 01 plating technology in the table 1, and adjust bath pH value to 6.0.With line be cut into AZ91D, the AM60B of 50mm * 50mm * 2mm and pure magnesium sample respectively through silicon carbide paper from coarse to fine polish successively uniform and smooth to outward appearance, with carry out dehydrated alcohol rinsing and scouring after lead is connected, to immerse the differential arc oxidation electrolytic solution under the room temperature after the distilled water rinsing, sinusoidal ac constant voltage 200V differential arc oxidation is handled 2min again.Take out the back with tap water and distilled water rinsing successively, be immersed in temperature then and be controlled in 80 ± 2 ℃ the plating bath, do not have and added under the stirring state electroless plating plating 3 hours.Take out the back with tap water, distilled water rinsing successively, dry up.
It is even, smooth to obtain outward appearance, the complete coating of band grey metal glossy.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 2
Remove differential arc oxidation electrolytic solution and change the 100g/L sodium radio-phosphate,P-32 solution into, the differential arc oxidation condition becomes simple alternating current constant voltage 150V to be handled outside the 60min, and other is with embodiment 1.
It is even, smooth to obtain outward appearance, the complete coating of band grey metal glossy.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 3
Remove differential arc oxidation electrolytic solution and become 5g/L Sodium Fluoride, 20g/L sodium radio-phosphate,P-32 solution, the differential arc oxidation condition becomes outside the simple alternating current constant voltage 250V treatment time 1min, and other is with embodiment 1.
It is even, smooth to obtain outward appearance, the complete coating of band grey metal glossy.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 4
Remove the differential arc oxidation concentration of electrolyte and become 1g/L sodium phosphate, 5g/L sodium hydroxide, the differential arc oxidation condition becomes outside the simple alternating current constant voltage 300V treatment time 10min, and other is with embodiment 1.
It is even, smooth to obtain outward appearance, the complete coating of band grey metal glossy.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 5
Remove the differential arc oxidation concentration of electrolyte and become 1g/L Sodium Fluoride, 2g/L sodium hydroxide, the differential arc oxidation condition becomes outside the simple alternating current constant voltage 200V treatment time 2min, and other is with embodiment 1.
It is even, smooth to obtain outward appearance, the complete coating of band grey metal glossy.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 6
Remove the differential arc oxidation concentration of electrolyte and become 5g/L sodium phosphate, 5g/L Sodium Fluoride, 0.05g/L sodium hydroxide, the differential arc oxidation condition becomes outside the simple alternating current constant voltage 300V treatment time 10sec, and other is with embodiment 1.
It is even, smooth to obtain outward appearance, the complete coating of band grey metal glossy.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 7
Remove the differential arc oxidation condition and become direct current constant current 10mA/cm
2Handle outside the 30min, other is with embodiment 1.
It is even, smooth to obtain outward appearance, the complete coating of band grey metal glossy.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 8
AZ91D, AM60B and the pure magnesium sample that is of a size of 50mm * 50mm * 2mm carried out the differential arc oxidation processing by embodiment 1 respectively, take out the back with tap water, distilled water rinsing successively, immerse then in the plating bath by No. 02 plating technology requirement preparation in the table 1, the control bath pH value is 9.0, temperature is 55 ℃, cathode current density 40mA/cm
2, be counter electrode with the stainless steel, electroplate 1h.Take out the back with tap water, distilled water rinsing successively, dry up.
It is even, smooth to obtain outward appearance, with the complete coating of golden yellow metalluster.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Embodiment 9
Except that the electroless plating plating time changes into the 1h, other carries out differential arc oxidation and electroless plating successively with embodiment 1.Take out the back with tap water, distilled water rinsing successively, immerse then in the plating bath by No. 02 plating technology requirement preparation in the table 1, the control bath pH value is 9.0, and temperature is 55 ℃, cathode current density 40mA/cm
2, be counter electrode with the stainless steel, electroplate 1h.Take out the back with tap water, distilled water rinsing successively, dry up.
It is even, smooth to obtain outward appearance, with the complete coating of golden yellow metalluster.OM and SEM carry out surface and cross-section, find the coating structure densification, no significant defect.Carry out thermal shock test and file test according to GB/T13913-92, the result shows that bonding force is good.
Obviously, the Sodium Fluoride in the above-mentioned differential arc oxidation electrolytic solution can be with following compounds or its mixture replacing: lithium fluoride, Potassium monofluoride, Neutral ammonium fluoride or ammonium bifluoride.
Sodium phosphate can be with following compounds or its mixture replacing: the alkali metal salts or ammonium salt of other alkali metal salts or ammonium salt of phosphoric acid, tetra-sodium, tripolyphosphate, four polyphosphoric acids and hexa metaphosphoric acid.
Sodium hydroxide can be with following compounds or its mixture replacing: lithium hydroxide, potassium hydroxide.
Claims (3)
1. the preparation method of magnesium and magnesium alloy surface coating is characterized in that: comprise the following steps:
A) surface dressing to magnesium and magnesium alloy polish successively, polishing and skimming treatment;
B) differential arc oxidation immerses magnesium and magnesium alloy in the differential arc oxidation electrolytic solution for preparing, and energising is carried out surface ceramic deposition and handled; Described electrolytic solution is group water solution, concentration of sodium fluoride 1-40g/L wherein, and sodium phosphate concentration 1-100g/L, both can independent or composite use, or further to add concentration be that the sodium hydroxide of 0.05-10g/L uses;
C) electroless plating will be through b) magnesium and the magnesium alloy of step differential arc oxidation immerse the chemical plating fluid for preparing, and control bath pH value and temperature are carried out the electroless plating plating;
D) electroplating will be through b) step differential arc oxidation or c) magnesium and the magnesium alloy of step chemical plating immerse the electroplate liquid for preparing, and control cathode current density and bath pH value and temperature are electroplated plating.
2. the preparation method of a kind of magnesium according to claim 1 and magnesium alloy surface coating is characterized in that: magnesium and magnesium alloy are through b) wash after the step differential arc oxidation, directly carry out c after the washing) step chemical plating or d) step electroplates.
3. the preparation method of a kind of magnesium according to claim 1 and magnesium alloy surface coating is characterized in that: after described each operation of a) step surface dressing, and c) step chemical plating or d) after step electroplates, magnesium and magnesium alloy are washed.
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|---|---|---|---|
| CN2007100316502A CN101161866B (en) | 2007-11-23 | 2007-11-23 | Method for preparing magnesium and magnesium alloy surface coating |
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|---|---|---|---|
| CN2007100316502A CN101161866B (en) | 2007-11-23 | 2007-11-23 | Method for preparing magnesium and magnesium alloy surface coating |
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| CN101161866A CN101161866A (en) | 2008-04-16 |
| CN101161866B true CN101161866B (en) | 2011-03-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2757642C1 (en) * | 2021-02-15 | 2021-10-19 | Федеральное государственное бюджетное учреждение науки Институт физической химии и электрохимии им. А.Н. Фрумкина Российской академии наук (ИФХЭ РАН) | Coating for the protection of magnesium and its alloys from corrosion and a method for its production |
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| SG157239A1 (en) * | 2008-05-14 | 2009-12-29 | Fulita Internat Entpr Pte Ltd | A process for forming coatings on metallic surfaces |
| CN102234802B (en) * | 2010-04-21 | 2012-12-05 | 中国科学院金属研究所 | Method for preparing multilayer high corrosion resistant-wear resistant composite protective coating on magnesium alloy surface |
| CN102234803B (en) * | 2010-05-07 | 2012-10-03 | 中国科学院金属研究所 | Preparation method of composite coating on magnesium alloy plasma oxide ceramic surface |
| TWI515333B (en) * | 2014-03-17 | 2016-01-01 | 柯惠蘭 | Method for forming protective coating layer of magnesium alloy and protective coating layer of magnesium alloy therefrom |
| CN104073857A (en) * | 2014-06-18 | 2014-10-01 | 华南理工大学 | Preparation method of nanoimprint nickel seal |
| CN105543920B (en) * | 2015-12-10 | 2017-11-28 | 嘉瑞科技（惠州）有限公司 | Magnesium alloy differential arc oxidation layer surface prepares the processing method of conductive coating |
| CN105772672B (en) * | 2016-04-27 | 2018-07-24 | 东莞市锐准精密金属有限公司 | The molding of magnesium alloy tableware and surface ceramic deposition processing method and its product |
| CN106884196A (en) * | 2017-03-20 | 2017-06-23 | 苏连明 | A kind of portable magnesium alloy slotless microarc oxidation treatment process and equipment |
| CN112064037A (en) * | 2020-10-13 | 2020-12-11 | 贵州电网有限责任公司 | Preparation method of corrosion-resistant magnesium alloy sacrificial anode |
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2007
- 2007-11-23 CN CN2007100316502A patent/CN101161866B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2757642C1 (en) * | 2021-02-15 | 2021-10-19 | Федеральное государственное бюджетное учреждение науки Институт физической химии и электрохимии им. А.Н. Фрумкина Российской академии наук (ИФХЭ РАН) | Coating for the protection of magnesium and its alloys from corrosion and a method for its production |
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