CN107460481A - A kind of preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat - Google Patents
A kind of preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat Download PDFInfo
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- CN107460481A CN107460481A CN201610391986.9A CN201610391986A CN107460481A CN 107460481 A CN107460481 A CN 107460481A CN 201610391986 A CN201610391986 A CN 201610391986A CN 107460481 A CN107460481 A CN 107460481A
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- magnesium alloy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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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
- C25D11/30—Anodisation of magnesium or alloys based thereon
Abstract
The invention provides a kind of preparation method of magnesium alloy differential arc oxidation chemical nickel plating composite coating, comprise the following steps：（1）Surface by micro-arc oxidation is carried out to magnesium alloy substrate, forms Micro-Arc Oxidized Ceramic Coating；（2）Magnesium alloy substrate after differential arc oxidation is put into the s of sensitized treatment 200 400 in the sensitizing solution being made up of 10 20 g/L stannous chlorides and 30 50 ml/L hydrochloric acid at room temperature；（3）The magnesium alloy substrate after sensitized treatment is put at room temperature the s of activation process 100 200 in 28 g/L Presence of Silver Nitrate Activator liquid of pellucidity is adjusted to ammoniacal liquor；（4）Magnesium alloy substrate after sensitization plays and activation process is put into the chemical plating fluid being made up of 10 25 g/L nickel sulfates, 10 20 g/L sodium hydroxides, 5 15 g/L sodium hypophosphites, 15 35 g/L EDTA and 15 30 g/L ammonium acid fluorides, adjust its pH to 12 13, chemical plating temperature is 30 50 DEG C, and the time is 40 80 min；（5）The magnesium alloy differential arc oxidation chemical nickel plating composite coating prepared is rinsed with deionized water, spontaneously dried.
Description
Technical field
The present invention relates to a kind of preparation method of differential arc oxidation-chemical plating composite coating, especially a kind of preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat.
Background technology
Magnesium alloy is that the alloy that other elements form is added by base metal of magnesium, is mainly used in the industrial departments such as Aeronautics and Astronautics, transport, chemical industry, rocket.Corrosion resistance difference is to hinder one of wide variety of major reason of magnesium alloy, to improve corrosion resistance, the research of a large amount of relevant Mg alloy surface processing existing at present.Differential arc oxidation processing is a kind of emerging process of surface treatment, the technology imparts the ceramic protection film of magnesium alloy, aluminium alloy and titanium alloy growth in situ, the film layer can possess excellent corrosion resistance, wearability, good film-substrate cohesion etc., it is more superior compared to anode oxide film, the service life of alloy is substantially increased, and complex-shaped part can be handled and ceramic membrane in uniform thickness can be obtained.The performance studies such as existing at present substantial amounts of technical study and the anti-corrosion, wearability of film layer about the influence to film performance such as bath composition and concentration, electrical parameter.However, differential arc oxidation film layer not yet really solves the etching problem of magnesium alloy, this is mainly limited by the active characteristic of matrix magnesium alloy in itself.
To solve the etching problem of magnesium alloy, it is necessary to which the process of surface treatment that some are possessed to different characteristics is combined, and carries out Combined Processing.Chemical plating is to reduce the metal ion in plating solution using a kind of suitable reducing agent and be deposited on the chemical reduction procedure on matrix.It has advantages below：Can be in material surface Direct precipitation coating；The coating for having fine covering power is obtained on complex surface；The coating of different functionalities, such as hardness, wearability, corrosion resistance can be obtained；It is also used as prime coat of other coating etc..
The content of the invention
To solve above-mentioned deficiency present in magnesium alloy materials differential arc oxidization technique, the invention provides a kind of preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat.
To reach goal of the invention, the technical solution adopted in the present invention is：
A kind of preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat, it is characterised in that including procedure below：
（1）Surface by micro-arc oxidation is carried out to magnesium alloy substrate, forms Micro-Arc Oxidized Ceramic Coating；
（2）Magnesium alloy substrate after differential arc oxidation is put into sensitized treatment 200-400 s in the sensitizing solution being made up of 10-20 g/L stannous chlorides and 30-50 ml/L hydrochloric acid at room temperature；
（3）The magnesium alloy substrate after sensitized treatment is put at room temperature activation process 100-200 s in the 2-8 g/L Presence of Silver Nitrate Activator liquid of pellucidity are adjusted to ammoniacal liquor；
（4）Magnesium alloy substrate after sensitization plays and activation process is put into the chemical plating fluid being made up of 10-25 g/L nickel sulfates, 10-20 g/L sodium hydroxides, 5-15 g/L sodium hypophosphites, 15-35 g/L EDTA and 15-30 g/L ammonium acid fluorides, adjust its pH to 12-13, chemical plating temperature is 30-50 DEG C, and the time is 40-80 min；
（5）The Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat prepared is rinsed with deionized water, spontaneously dried.
The step（2）In preferable sensitizing solution composition be：The g/L of stannous chloride 15, the ml/L of hydrochloric acid 40.
The step（3）In preferable activating solution composition be：The g/L of silver nitrate 4.
The step（4）In preferable chemical plating fluid composition be：The g/L of nickel sulfate 20, the g/L of sodium hydroxide 15, sodium hypophosphite 10 g/L, EDTA 20 g/L, the g/L of ammonium acid fluoride 20.
Magnesium alloy surface micro-arc oxidation process is：
（1）Magnesium alloy substrate is pre-processed, basic step includes：Sand paper is polished, oil removing, sodium hydroxide and nitric acid rinsing liquid（3:1）Rinsing, ultrasonic wave deionized water are cleaned 40 min, dried in vacuum environment；
（2）Sample is arranged on microarc oxidation equipment provided, sample is immersed in treatment fluid as anode, rustless steel container with cooling system is as negative electrode, electrolyte is 15 g/L sodium metasilicate, 4 g/L potassium hydroxide, 2g/L sodium fluorides, pattern is constant current mode, electric current is 2A, and preparation time is 15 min, and temperature control is at 25 DEG C or so；
（3）The magnesium alloy differential arc oxidation sample prepared is rinsed with deionized water, spontaneously dried.
Beneficial effects of the present invention are：（1）The defects of the defects of differential arc oxidation-chemical nickel plating composite coating is far fewer than traditional differential arc oxidation film layer, improves corrosion resisting property；（2）Prepared coating forms conductive capability, can expand application of the magnesium alloy in the field for possessing conductive requirement；（3）Raw material is cheap, common, and technique is simple, cost is low, and course of reaction is easily controlled, beneficial to industrialized production.
Brief description of the drawings
Fig. 1 is Mg alloy surface pattern：（a）Differential arc oxidation film layer；（b）Differential arc oxidation-chemical nickel plating composite coating.
Fig. 2 is dynamic potential polarization curve figure：（a）AZ31 magnesium alloys；（b）Micro-Arc Oxidized Ceramic Coating；（c）Differential arc oxidation-chemical nickel plating composite coating.
Embodiment
With reference to concrete mode, the present invention is described further, it is clear that described embodiment is only the part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made belongs to the scope of the present invention.
Embodiment 1：
Material prepares：Sensitizing solution：The g/L of stannous chloride 15, the ml/L of hydrochloric acid 40；Activating solution：The g/L of silver nitrate 4；Chemical plating fluid：The g/L of nickel sulfate 20, the g/L of sodium hydroxide 15, sodium hypophosphite 10 g/L, EDTA 20 g/L, the g/L of ammonium acid fluoride 20；AZ31 magnesium alloys by Microarc Oxidation Surface Treatment.
Magnesium alloy substrate after differential arc oxidation is put into sensitizing solution at room temperature and handles 360 s, then it is put at room temperature in activating solution and handles 180 s, then will be put into through sensitization plays and activation process magnesium alloy substrate in chemical plating fluid, adjusts its pH to 12, for temperature control at 45 DEG C or so, the time is 60 min.
Embodiment 2：
Material prepares：Sensitizing solution：The g/L of stannous chloride 15, the ml/L of hydrochloric acid 40；Activating solution：The g/L of silver nitrate 4；Chemical plating fluid：The g/L of nickel sulfate 25, the g/L of sodium hydroxide 20, sodium hypophosphite 12 g/L, EDTA 20 g/L, the g/L of ammonium acid fluoride 25；AZ31 magnesium alloys by Microarc Oxidation Surface Treatment.
Magnesium alloy substrate after differential arc oxidation is put into sensitizing solution at room temperature and handles 400 s, then it is put at room temperature in activating solution and handles 200 s, then will be put into through sensitization plays and activation process magnesium alloy substrate in chemical plating fluid, adjusts its pH to 12, for temperature control at 40 DEG C or so, the time is 50 min.
Embodiment 3：
Material prepares：Sensitizing solution：The g/L of stannous chloride 10, the ml/L of hydrochloric acid 30；Activating solution：The g/L of silver nitrate 8；Chemical plating fluid：The g/L of nickel sulfate 20, the g/L of sodium hydroxide 15, sodium hypophosphite 5g/L, EDTA 35 g/L, ammonium acid fluoride 15g/L；AZ31 magnesium alloys by Microarc Oxidation Surface Treatment.
Magnesium alloy substrate after differential arc oxidation is put into sensitizing solution at room temperature and handles 300 s, then it is put at room temperature in activating solution and handles 150 s, it will be put into again through sensitization plays and activation process magnesium alloy substrate in chemical plating fluid, adjust its pH to 12, for temperature control at 50 DEG C or so, the time is 55 min.
Embodiment 4：
Material prepares：Sensitizing solution：The g/L of stannous chloride 15, the ml/L of hydrochloric acid 50；Activating solution：The g/L of silver nitrate 2；Chemical plating fluid：The g/L of nickel sulfate 15, the g/L of sodium hydroxide 10, sodium hypophosphite 15 g/L, EDTA 15 g/L, the g/L of ammonium acid fluoride 30；AZ31 magnesium alloys by Microarc Oxidation Surface Treatment.
Magnesium alloy substrate after differential arc oxidation is put into sensitizing solution at room temperature and handles 250 s, then it is put at room temperature in activating solution and handles 150 s, it will be put into again through sensitization plays and activation process magnesium alloy substrate in chemical plating fluid, adjust its pH to 12, for temperature control at 30 DEG C or so, the time is 80 min.
Using ISM-6510 type ESEMs（SEM）The surface microscopic topographic of sample is determined, uses electrochemical apparatus（Electrochemical
Workstation, CS 350）Potentiodynamic polarization test is carried out to sample.
（1）SEM is analyzed：It can be seen that from Fig. 1 SEM pictures, Mg alloy surface after differential arc oxidation has many micropores, the differential arc oxidation coating passes through after chemical nickel plating, surface micropore greatly reduces, illustrate that the defects of chemical plating is for differential arc oxidation film layer is reduced to play a significant role, and then its corrosion resistance can be improved.
（2）Electrochemical analysis：From figure 2 it can be seen that the corrosion resistance of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat greatly improves compared with differential arc oxidation film layer.
Claims (4)
1. a kind of preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat, it is characterised in that including procedure below：
（1）Surface by micro-arc oxidation is carried out to magnesium alloy substrate, forms Micro-Arc Oxidized Ceramic Coating；
（2）Magnesium alloy substrate after differential arc oxidation is put into sensitized treatment 200-400 s in the sensitizing solution being made up of 10-20 g/L stannous chlorides and 30-50 ml/L hydrochloric acid at room temperature；
（3）The magnesium alloy substrate after sensitized treatment is put at room temperature activation process 100-200 s in the 2-8 g/L Presence of Silver Nitrate Activator liquid of pellucidity are adjusted to ammoniacal liquor；
（4）Magnesium alloy substrate after sensitization plays and activation process is put into the chemical plating fluid being made up of 10-25 g/L nickel sulfates, 10-20 g/L sodium hydroxides, 5-15 g/L sodium hypophosphites, 15-35 g/L EDTA and 15-30 g/L ammonium acid fluorides, adjust its pH to 12-13, chemical plating temperature is 30-50 DEG C, and the time is 40-80 min；
（5）The Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat prepared is rinsed with deionized water, spontaneously dried.
2. the preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat according to claim 1, it is characterised in that step（2）In sensitizing solution composition be：The g/L of stannous chloride 15, the ml/L of hydrochloric acid 40.
3. the preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat according to claim 1, it is characterised in that step（3）In activating solution composition be：The g/L of silver nitrate 4.
4. the preparation method of Microarc Oxidation-Electroless Plating of Magnesium Alloy nickel composite coat according to claim 1, it is characterised in that step（4）In chemical plating fluid composition be：The g/L of nickel sulfate 20, the g/L of sodium hydroxide 15, sodium hypophosphite 10 g/L, EDTA 20 g/L, the g/L of ammonium acid fluoride 20.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186522A (en) * | 2021-05-26 | 2021-07-30 | 西南科技大学 | Tin salt sensitization activation method for titanium alloy surface chemical plating |
| CN114703529A (en) * | 2022-04-06 | 2022-07-05 | 内蒙古工业大学 | Magnesium alloy with super-hydrophobic MAO-LDH composite membrane layer and preparation method thereof |
| CN115522245A (en) * | 2022-08-12 | 2022-12-27 | 中国航空无线电电子研究所 | Corrosion-resistant magnesium alloy airborne avionics chassis |
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| CN101298200A (en) * | 2007-04-30 | 2008-11-05 | 比亚迪股份有限公司 | Magnesium alloy composite material and preparation thereof |
| CN103554826A (en) * | 2013-11-04 | 2014-02-05 | 四川大学 | Platable polyformaldehyde composition and preparation method and electroplating method thereof |
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| CN101298200A (en) * | 2007-04-30 | 2008-11-05 | 比亚迪股份有限公司 | Magnesium alloy composite material and preparation thereof |
| CN103554826A (en) * | 2013-11-04 | 2014-02-05 | 四川大学 | Platable polyformaldehyde composition and preparation method and electroplating method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186522A (en) * | 2021-05-26 | 2021-07-30 | 西南科技大学 | Tin salt sensitization activation method for titanium alloy surface chemical plating |
| CN113186522B (en) * | 2021-05-26 | 2022-01-28 | 西南科技大学 | Tin salt sensitization activation method for titanium alloy surface chemical plating |
| CN114703529A (en) * | 2022-04-06 | 2022-07-05 | 内蒙古工业大学 | Magnesium alloy with super-hydrophobic MAO-LDH composite membrane layer and preparation method thereof |
| CN114703529B (en) * | 2022-04-06 | 2023-12-08 | 内蒙古工业大学 | Magnesium alloy with super-hydrophobic MAO-LDH composite membrane layer and preparation method thereof |
| CN115522245A (en) * | 2022-08-12 | 2022-12-27 | 中国航空无线电电子研究所 | Corrosion-resistant magnesium alloy airborne avionics chassis |
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Application publication date: 20171212 |