CN114855231A - Method for plating niobium on magnesium and magnesium alloy - Google Patents
Method for plating niobium on magnesium and magnesium alloy Download PDFInfo
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- CN114855231A CN114855231A CN202210591279.XA CN202210591279A CN114855231A CN 114855231 A CN114855231 A CN 114855231A CN 202210591279 A CN202210591279 A CN 202210591279A CN 114855231 A CN114855231 A CN 114855231A
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- niobium
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a method for plating niobium on magnesium and magnesium alloy, which comprises the following steps: a) preparing electroplating solution, mixing the ionic liquid and the solvent, adding a certain amount of niobium salt into the mixed solution, stirring and mixing to obtain the electroplating solution, and adjusting the pH value of the electroplating solution; the ionic liquid is 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid; b) assembling an electroplating device, taking niobium electrodeposition as an anode, taking the treated magnesium and the treated magnesium alloy as a cathode, and putting the cathode into an electroplating bath; c) and electroplating, wherein after a period of time, the cathode is taken out to obtain the niobium-plated material. According to the method for plating the niobium on the magnesium and the magnesium alloy with the structure, the Nb coating is formed on the surface of the magnesium alloy by adopting an electrodeposition method, so that the performance of the magnesium and the magnesium alloy is improved, the practicability of the magnesium and the magnesium alloy is enhanced, and the ionic liquid used in the electrodeposition process is green and non-corrosive, is environment-friendly and has no pollution.
Description
Technical Field
The invention relates to the technical field of magnesium and magnesium alloy electroplating, in particular to a method for plating niobium on magnesium and magnesium alloy.
Background
Magnesium (Mg), a light silvery white metal, is a potential material for fuel efficiency improvement in the aircraft, automobile, and other industries. However, the main limitation of magnesium and its alloys is its high corrosion rate, very poor corrosion resistance in wet salt environments. Furthermore, it is very susceptible to galvanic corrosion when coupled with another metal. It is therefore necessary to deposit a thin layer of a different metal to enhance the properties of the desired magnesium. These include coating methods for protecting magnesium from corrosion, such as electrochemical plating, conversion coatings, anodization, vapor deposition, organic coatings, and hydride coatings.
Electrodeposition is a process for coating a substrate with a metal that has the desired properties for a particular application by reducing the molten salt in solution to a metallic form at the substrate surface. One of the main advantages of this process is the low investment cost. Magnesium reacts strongly with most acids, dissolves in acidic media, forms local corrosion units on the surface when in electrolytic contact with other metals, causing pitting corrosion, and the metal coating on magnesium must be non-porous or the corrosion rate will increase.
Niobium is a soft rare transition metal, commonly used for the production of high grade steels, which has corrosion resistance and superconducting properties, has many applications in the automotive field, and can withstand the extreme conditions of the nuclear and aerospace industries, however, successful electrodeposition of niobium remains a mystery. Current methods for electrodepositing niobium on other elements include high temperature molten salts where the formation of tightly adhering niobium deposits can be observed on mild steel in a fluorine melt. However, a disadvantage of high temperature molten salts is that both their environment and the electroplating bath are toxic and corrosive and are not environmentally friendly.
Disclosure of Invention
The invention aims to provide a method for plating niobium on magnesium and magnesium alloy, which adopts an electrodeposition method to form a Nb coating on the surface of the magnesium alloy, improves the performance of the magnesium and the magnesium alloy, enhances the practicability of the magnesium and the magnesium alloy, and ensures that the ionic liquid used in the electrodeposition process is green and non-corrosive and is environment-friendly and pollution-free.
In order to achieve the above object, the present invention provides a method for plating niobium on magnesium and its alloy, comprising the steps of:
a) preparing an electroplating solution
Mixing the ionic liquid and the solvent, adding a certain amount of niobium salt into the mixed solution, stirring and mixing to obtain electroplating solution, and adjusting the pH value of the electroplating solution; the ionic liquid is 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid;
b) assembling and electroplating device
Putting the processed magnesium and the processed alloy thereof as a cathode into an electroplating bath by taking niobium electrodeposition as an anode;
c) and electroplating
And after a period of electroplating, taking out the cathode to obtain the niobium-plated material.
Preferably, in step a), the solvent is one or more of water, acetone and dimethyl sulfoxide.
Preferably, in the step a), the concentration of the ionic liquid is 0.1-1M.
Preferably, in step a), the niobium salt is one or more of niobium bromide and niobium chloride.
Preferably, in the step a), the pH value is adjusted by using choline chloride in the pH adjusting process, and the pH value is controlled to be 2-4.
Preferably, in step b), the cathode treatment process is to remove an oxide layer on the surface of the cathode.
Preferably, in the step c), the bath voltage is 0.7-3V and the electroplating time is 0.3-2 h in the electroplating process.
The invention has the beneficial effects that:
1 the niobium-plated magnesium material obtained by the method is compact and has good adhesiveness;
2. the method has good economy, and the clean production is realized by using the non-corrosive ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroborate salt bath in the process;
3. the method realizes the improvement of excellent magnesium and magnesium alloy, greatly improves the corrosion resistance of the magnesium and magnesium alloy, and provides good prospect for the industrial application of the magnesium and magnesium alloy.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a micrograph of the substrate surface after 96h of the salt test at 5% salt concentration, a) magnesium alloy without niobium plating b) magnesium alloy with niobium plating.
Detailed Description
The present invention will be further described with reference to examples, in which various chemicals and reagents are commercially available unless otherwise specified.
Example 1
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with acetone to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 4; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5h of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1.
Example 2
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with acetone to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 2.5; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5h of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1
Example 3
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with dimethyl sulfoxide to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 4; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5h of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1.
Example 4
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with dimethyl sulfoxide to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 2.5; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5h of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1
Example 5
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with water to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 4; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5h of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1
Example 6
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with water to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 3; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5 of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1
Example 7
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with water to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 2.5; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5 of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1.
Example 8
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with water to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 2.5; putting the niobium electrodeposition as an anode and the treated magnesium as a cathode into an electroplating bath; and after 0.5 of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1.
Example 9
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with water to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 1.5; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 0.5 of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1
Example 10
Mixing ionic liquid 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid with water to prepare a mixed solution with the ionic liquid concentration of 0.2M, adding a certain amount of niobium bromide into the mixed solution, controlling the niobium concentration to be 0.01M, stirring and mixing the mixed solution to obtain an electroplating solution, and adding choline chloride to adjust the pH value of the electroplating solution to 2.5; putting the processed magnesium alloy AZ31 as a cathode into an electroplating bath by taking niobium electrodeposition as an anode; and after 2 hours of electroplating, taking out the cathode to obtain the niobium-plated material. The niobium content is shown in Table 1.
TABLE 1 data on niobium content of niobium-plated materials of examples 1-10
As can be seen from examples 1-10, the best method for coating niobium on magnesium and magnesium alloy thereof, which is adopted by the invention, is water, the pH value is controlled to be 2.5, the electroplating time is 0.5 hour, and the best magnesium alloy with a niobium coating can be obtained, wherein the niobium content is 34 percent.
And (3) performance testing:
1. the corrosion resistance of the magnesium alloy with niobium and the corrosion resistance of the magnesium alloy AZ31 obtained in example 7 were tested by a dynamic electrochemical test method using a potentiometer. The test results are shown in Table 2.
TABLE 2 Corrosion resistance test result data
As can be seen from Table 2, the corrosion rate for the Nb-coated magnesium alloy is 0.00111 mm/year, while the corrosion rate for the Mg AZ31 coupon is 0.1458 mm/year, indicating that the uncoated magnesium alloy coupon corrodes faster than the niobium-coated magnesium coupon, and thus the coating matrix protects the coupon from corrosion.
2. The magnesium and niobium alloys and AZ31 from example 8 were tested for corrosion resistance by a salt spray test, specifically by placing the magnesium and niobium alloys and AZ31 in a salt environment using a 5% strength salt spray for 96 hours, which resulted in significant corrosion of the uncoated magnesium alloy surface and became very rough and fragmented, whereas the niobium coated coupons were not corroded.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (7)
1. A method for plating niobium on magnesium and magnesium alloy is characterized by comprising the following steps:
a) preparing an electroplating solution
Mixing the ionic liquid and the solvent, adding a certain amount of niobium salt into the mixed solution, stirring and mixing to obtain electroplating solution, and adjusting the pH value of the electroplating solution; the ionic liquid is 1-butyl-2, 3-dimethyl imidazole tetrafluoroboric acid;
b) assembling and electroplating device
Putting the processed magnesium and the processed alloy thereof as a cathode into an electroplating bath by taking niobium electrodeposition as an anode;
c) and electroplating
And after a period of electroplating, taking out the cathode to obtain the niobium-plated material.
2. The method for coating magnesium and its alloy with niobium as claimed in claim 1, wherein: in the step a), the solvent is one or a mixture of water, acetone and dimethyl sulfoxide.
3. The method for coating magnesium and its alloy with niobium as claimed in claim 1, wherein: in the step a), the concentration of the ionic liquid is 0.1-1M.
4. The method of claim 1, wherein the niobium is plated on magnesium and magnesium alloy by the following steps: in the step a), the niobium salt is one or a mixture of niobium bromide and niobium chloride.
5. The method for coating magnesium and its alloy with niobium as claimed in claim 1, wherein: in the step a), in the pH adjusting process, choline chloride is used for adjusting the pH value, and the pH is controlled to be 2-4.
6. The method for coating magnesium and its alloy with niobium as claimed in claim 1, wherein: in the step b), the cathode treatment process is to remove an oxide layer on the surface of the cathode.
7. The method for coating magnesium and its alloy with niobium as claimed in claim 1, wherein: in the step c), the bath voltage is 0.7-3V and the electroplating time is 0.3-2 h in the electroplating process.
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| CN202210591279.XA CN114855231A (en) | 2022-05-27 | 2022-05-27 | Method for plating niobium on magnesium and magnesium alloy |
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| CN202210591279.XA CN114855231A (en) | 2022-05-27 | 2022-05-27 | Method for plating niobium on magnesium and magnesium alloy |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1983078A1 (en) * | 2007-04-17 | 2008-10-22 | Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO | Electrodeposition |
| CN101949044A (en) * | 2010-09-20 | 2011-01-19 | 大连海事大学 | Niobium electro-osmosis method for steel surface in ionic liquid |
| US20130075271A1 (en) * | 2011-09-22 | 2013-03-28 | Sikorsky Aircraft Corporation | Protection of magnesium alloys by aluminum plating from ionic liquids |
| CN108517544A (en) * | 2018-06-14 | 2018-09-11 | 中国兵器工业第五九研究所 | The method of Mg alloy surface processing il electrolyte and magnesium alloy before electroplating of aluminium |
| CN109252195A (en) * | 2018-11-08 | 2019-01-22 | 太原理工大学 | A kind of method of Mg alloy surface ionic liquid electrodeposition aluminium |
| CN112779574A (en) * | 2020-12-14 | 2021-05-11 | 安徽铜冠铜箔集团股份有限公司 | Electroplating solution for enhancing conductivity of electronic copper foil, preparation method and electroplating process |
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- 2022-05-27 CN CN202210591279.XA patent/CN114855231A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1983078A1 (en) * | 2007-04-17 | 2008-10-22 | Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO | Electrodeposition |
| CN101949044A (en) * | 2010-09-20 | 2011-01-19 | 大连海事大学 | Niobium electro-osmosis method for steel surface in ionic liquid |
| US20130075271A1 (en) * | 2011-09-22 | 2013-03-28 | Sikorsky Aircraft Corporation | Protection of magnesium alloys by aluminum plating from ionic liquids |
| CN108517544A (en) * | 2018-06-14 | 2018-09-11 | 中国兵器工业第五九研究所 | The method of Mg alloy surface processing il electrolyte and magnesium alloy before electroplating of aluminium |
| CN109252195A (en) * | 2018-11-08 | 2019-01-22 | 太原理工大学 | A kind of method of Mg alloy surface ionic liquid electrodeposition aluminium |
| CN112779574A (en) * | 2020-12-14 | 2021-05-11 | 安徽铜冠铜箔集团股份有限公司 | Electroplating solution for enhancing conductivity of electronic copper foil, preparation method and electroplating process |
Non-Patent Citations (4)
| Title |
|---|
| ANIL MAHAPATRO等: "Electrodeposition of Niobium on Magnesium Using Green Ionic Liquids", 《ECS TRANSACTIONS》, vol. 59, no. 19, pages 77 - 81 * |
| JEHANZEB HAKIM: "FABRICATION OF NIOBIUM COATED MAGNESIUM ALLOY FOR AUTOMOTIVE & AEROSPACE APPLICATIONS", Retrieved from the Internet <URL:https://soar.wichita.edu/handle/10057/11342> * |
| XINGLI ZOU: "Electrodeposition of Zn, Cu, and Zn-Cu Alloys from Deep Eutectic Solvents", PROGRESS AND DEVELOPMENTS IN IONIC LIQUIDS, pages 263 - 282 * |
| 曹彩红: "【emim】OTf离子液体中镀铌不锈钢双极板在 PEMFC环境中的电化学行为", 稀有金属材料与工程, vol. 42, no. 3, pages 569 - 573 * |
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