CN110592452A - High-strength magnesium rare earth alloy material and preparation method thereof - Google Patents
High-strength magnesium rare earth alloy material and preparation method thereof Download PDFInfo
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- CN110592452A CN110592452A CN201910957480.3A CN201910957480A CN110592452A CN 110592452 A CN110592452 A CN 110592452A CN 201910957480 A CN201910957480 A CN 201910957480A CN 110592452 A CN110592452 A CN 110592452A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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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
- 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
- C23C18/02—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 thermal decomposition
- C23C18/12—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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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
- 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
- C23C18/02—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 thermal decomposition
- C23C18/12—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
Abstract
The invention discloses a high-strength magnesium rare earth alloy material and a preparation method thereof, wherein the high-strength magnesium rare earth alloy material comprises a magnesium rare earth alloy body and a corrosion-resistant film layer on the surface of the magnesium rare earth alloy body, and the magnesium alloy body comprises the following chemical element components in percentage by mass: 2.5-3.5% of lanthanum, 1.5-2.5% of cerium, 0.5-1.0% of carbon, 0.2-0.4% of manganese, 0.10-0.30% of vanadium, 0.25-0.50% of gadolinium, 0.3-0.6% of yttrium and the balance of magnesium. The cathode of the electrolytic cell is characterized in that magnesium ions in magnesium chloride are firstly subjected to electron reduction to form magnesium metal, then the magnesium metal is further oxidized and replaced by rare earth elements in rare earth chloride, so that a uniform and compact magnesium rare earth alloy body is formed, in order to improve the corrosion resistance of the magnesium rare earth alloy body, a corrosion-resistant film layer is further coated on the surface of the magnesium rare earth alloy body, the magnesium rare earth alloy body has good salt water corrosion resistance, and the practical application temperature of the magnesium rare earth alloy body can be obviously improved.
Description
Technical Field
The invention relates to the technical field of high-strength rare earth alloys, in particular to a high-strength magnesium rare earth alloy material and a preparation method thereof.
Background
The magnesium alloy is the lightest metal structure material in engineering application, has the advantages of high specific strength, high specific rigidity, easy processing, easy recovery and the like, and has huge application market in the fields of spaceflight, war industry, electronic communication, transportation and the like. The rare earth element is one of the most effective elements for improving the performance of the magnesium alloy, but because the melting points and the densities of magnesium and the rare earth elements are different, the composition segregation of the rare earth element in the alloy is easy to cause when the magnesium and the rare earth elements are doped, and the adoption of an electrolytic method is a common method for preparing the magnesium-rare earth intermediate alloy.
Therefore, the invention mainly solves the problem that the magnesium rare earth alloy has poor practical application effects in corrosion resistance, hardness, high temperature resistance and the like due to uneven distribution of all components in the magnesium rare earth alloy.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-strength magnesium rare earth alloy material and a preparation method thereof, and mainly solves the problem that the magnesium rare earth alloy has poor practical application effects in corrosion resistance, hardness, high temperature resistance and the like due to uneven distribution of components in the magnesium rare earth alloy.
The invention solves the technical problems through the following technical means:
a high-strength magnesium rare earth alloy material comprises a magnesium rare earth alloy body and a corrosion-resistant film layer on the surface of the magnesium rare earth alloy body; the magnesium alloy body comprises the following chemical element components in percentage by mass: 2.5-3.5% of lanthanum, 1.5-2.5% of cerium, 0.5-1.0% of carbon, 0.2-0.4% of manganese, 0.10-0.30% of vanadium, 0.25-0.50% of gadolinium, 0.3-0.6% of yttrium and the balance of magnesium;
the corrosion-resistant film layer is a cerium oxide doped yttrium oxide stabilized zirconia coating.
Preferably, the high-strength magnesium rare earth alloy material comprises the following chemical element components in percentage by mass: 3.2% of lanthanum, 1.6% of cerium, 0.6% of carbon, 0.3% of manganese, 0.15% of vanadium, 0.30% of gadolinium, 0.4% of yttrium and the balance of magnesium;
preferably, the thickness of the corrosion-resistant film layer is 10-50 μm.
A preparation method of a high-strength magnesium rare earth alloy material comprises the following steps,
(1) preparing anhydrous rare earth chloride: the method comprises the following steps of (1) dehydrating chlorinated lanthanum-cerium mixed rare earth for 2-5 hours at a high temperature of 200-250 ℃ in a vacuum dehydration furnace to obtain dehydrated chlorinated rare earth;
(2) preparing magnesium rare earth alloy by electrolysis: adopting a graphite crucible as an electrolytic cell, simultaneously taking the graphite crucible as an anode, taking molybdenum as a cathode, and using potassium chloride, sodium chloride, calcium chloride, magnesium chloride and the obtained rare earth chloride as electrolyte, wherein the electrolysis temperature is 700-800 ℃, the current is 180-320A, the electrolysis time is 1.5-2.5 h, and obtaining a magnesium rare earth alloy body at the cathode after the electrolysis is finished;
(3) pretreatment: preparing the magnesium rare earth alloy body obtained in the step (2) into a workpiece model, degreasing the workpiece model by using acetone, soaking the workpiece model in 6% sodium hydroxide solution at 70 ℃ for 10-15 min, and finally washing the workpiece model by water and then drying the workpiece model by air;
(4) preparing corrosion-resistant film sol: using n-propanol as a solvent, preparing 0.5mol/L zirconium n-propoxide and 0.5mol/L yttrium nitrate, stirring at 50 ℃ to form sol, and then adding 0.5mol/L cerous nitrate in an equal volume to obtain the composite corrosion-resistant film layer sol.
(5) Coating a corrosion-resistant film layer by using sol: and (3) coating the corrosion-resistant film layer sol obtained in the step (4) on the surface of the magnesium rare earth alloy body obtained in the step (3) by adopting a dip-coating method, and preserving heat for 1.0-1.5 hours at the temperature of 150 ℃ to obtain the magnesium rare earth alloy.
Preferably, the preparation method of the high-strength magnesium rare earth alloy material comprises the following steps of 25-35% of lanthanum compound and 10-25% of cerium compound in the lanthanum-cerium mixed rare earth.
Preferably, the preparation method of the high-strength magnesium rare earth alloy material comprises the following steps of mixing potassium chloride, sodium chloride, calcium chloride, magnesium chloride and rare earth chloride in a mass ratio of 1:3:4.5:200: 20.
The invention has the advantages that: magnesium ions in magnesium chloride are firstly obtained at the cathode of the electrolytic cell and are reduced into magnesium metal, and then the magnesium metal is further oxidized and replaced with rare earth elements in rare earth chloride, so that a uniform and compact magnesium rare earth alloy body is formed, and the magnesium rare earth alloy body has better requirements on hardness and toughness; in order to improve the corrosion resistance of the magnesium rare earth alloy body, the surface of the magnesium rare earth alloy body is coated with a corrosion-resistant film layer, so that the magnesium rare earth alloy body has good salt water corrosion resistance, and the actual application temperature of the magnesium rare earth alloy body can be obviously improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b):
a high-strength magnesium rare earth alloy material comprises the following chemical element components in percentage by mass: 3.2% of lanthanum, 1.6% of cerium, 0.6% of carbon, 0.3% of manganese, 0.15% of vanadium, 0.30% of gadolinium, 0.4% of yttrium and the balance of magnesium; the corrosion-resistant film layer is a cerium oxide doped yttrium oxide stabilized zirconia coating.
Preferably, the thickness of the corrosion-resistant film layer is 20 microns.
A preparation method of a high-strength magnesium rare earth alloy material comprises the following steps,
(1) preparing anhydrous rare earth chloride: the raw material is chlorinated lanthanum-cerium mixed rare earth, and the chlorinated lanthanum-cerium mixed rare earth is dehydrated for 3 hours in a vacuum dehydration furnace at the high temperature of 220 ℃ to obtain dehydrated chlorinated rare earth;
(2) preparing magnesium rare earth alloy by electrolysis: adopting a graphite crucible as an electrolytic cell, simultaneously taking the graphite crucible as an anode and taking metal molybdenum as a cathode, wherein the electrolyte comprises potassium chloride, sodium chloride, calcium chloride, magnesium chloride and the obtained rare earth chloride in the step (1), the electrolysis temperature is 700 ℃, the current is 280A, the electrolysis time is 2.0h, and obtaining a magnesium rare earth alloy body at the cathode after the electrolysis is finished;
(3) pretreatment: preparing the magnesium rare earth alloy body obtained in the step (2) into a workpiece model, degreasing the workpiece model by using acetone, soaking the workpiece model in 6% sodium hydroxide solution at 70 ℃ for 10-15 min, and finally washing the workpiece model by water and then drying the workpiece model by air;
(4) preparing corrosion-resistant film sol: using n-propanol as a solvent, preparing 0.5mol/L zirconium n-propoxide and 0.5mol/L yttrium nitrate, stirring at 50 ℃ to form sol, and then adding 0.5mol/L cerous nitrate in an equal volume to obtain the composite corrosion-resistant film layer sol.
(5) Coating a corrosion-resistant film layer by using sol: and (3) coating the corrosion-resistant film layer sol obtained in the step (4) on the surface of the magnesium rare earth alloy body obtained in the step (3) by adopting a dip-coating method, and preserving heat for 1.2 hours at the temperature of 150 ℃ to obtain the magnesium rare earth alloy.
Preferably, the preparation method of the high-strength magnesium rare earth alloy material comprises the following steps of mixing 30% of lanthanum compound and 18% of cerium compound in the lanthanum-cerium mixed rare earth.
Preferably, the preparation method of the high-strength magnesium rare earth alloy material comprises the following steps of mixing potassium chloride, sodium chloride, calcium chloride, magnesium chloride and rare earth chloride in a mass ratio of 1:3:4.5:200: 20.
In the present invention, the calcium chloride content contributes to an increase in the electrolyte density, allowing the alloy to float to the upper part of the electrolytic cell without depositing to the bottom of the electrolytic cell.
The electrolysis temperature is relatively low, and the low temperature not only saves energy consumption, but also can reduce the loss of magnesium, increase the yield of the magnesium-rare earth alloy, improve the current efficiency and simultaneously increase the rare earth content in the alloy.
Magnesium ions in magnesium chloride are firstly obtained at the cathode of the electrolytic cell and are reduced into magnesium metal, and then the magnesium metal is further oxidized and replaced by rare earth elements in rare earth chloride, so that a uniform and compact magnesium rare earth alloy body is formed, and the magnesium rare earth alloy body has better requirements on hardness and toughness.
In order to improve the corrosion resistance of the magnesium rare earth alloy body, a corrosion-resistant film layer is coated on the surface of the magnesium rare earth alloy body, the film layer is a coating of cerium oxide doped yttrium oxide stabilized zirconia, the coating is compact and uniform, a large number of particle clusters are formed, and the normal thickness is 30 micrometers, so that the film layer has excellent corrosion resistance, and experiments prove that the film layer has good salt water corrosion resistance, has a good protection effect on a substrate under a high-temperature condition, and can obviously improve the actual application temperature of the magnesium rare earth alloy body.
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A high-strength magnesium rare earth alloy material is characterized in that: the magnesium rare earth alloy coating comprises a magnesium rare earth alloy body and a corrosion-resistant film layer on the surface of the magnesium rare earth alloy body; the magnesium alloy body comprises the following chemical element components in percentage by mass: 2.5-3.5% of lanthanum, 1.5-2.5% of cerium, 0.5-1.0% of carbon, 0.2-0.4% of manganese, 0.10-0.30% of vanadium, 0.25-0.50% of gadolinium, 0.3-0.6% of yttrium and the balance of magnesium;
the corrosion-resistant film layer is a cerium oxide doped yttrium oxide stabilized zirconia coating.
2. The high-strength magnesium rare earth alloy material as set forth in claim 1, wherein: the magnesium alloy body comprises the following chemical element components in percentage by mass: 3.2% of lanthanum, 1.6% of cerium, 0.6% of carbon, 0.3% of manganese, 0.15% of vanadium, 0.30% of gadolinium, 0.4% of yttrium and the balance of magnesium.
3. The high-strength magnesium rare earth alloy material as set forth in claim 1, wherein: the thickness of the corrosion-resistant film layer is 10-50 mu m.
4. A preparation method of a high-strength magnesium rare earth alloy material is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
(1) preparing anhydrous rare earth chloride: the method comprises the following steps of (1) dehydrating chlorinated lanthanum-cerium mixed rare earth for 2-5 hours at a high temperature of 200-250 ℃ in a vacuum dehydration furnace to obtain dehydrated chlorinated rare earth;
(2) preparing magnesium rare earth alloy by electrolysis: adopting a graphite crucible as an electrolytic cell, simultaneously taking the graphite crucible as an anode, taking molybdenum as a cathode, and using potassium chloride, sodium chloride, calcium chloride, magnesium chloride and the obtained rare earth chloride as electrolyte, wherein the electrolysis temperature is 700-800 ℃, the current is 180-320A, the electrolysis time is 1.5-2.5 h, and obtaining a magnesium rare earth alloy body at the cathode after the electrolysis is finished;
(3) pretreatment: preparing the magnesium rare earth alloy body obtained in the step (2) into a workpiece model, degreasing the workpiece model by using acetone, soaking the workpiece model in 6% sodium hydroxide solution at 70 ℃ for 10-15 min, and finally washing the workpiece model by water and then drying the workpiece model by air;
(4) preparing corrosion-resistant film sol: using n-propanol as a solvent, preparing 0.5mol/L zirconium n-propoxide and 0.5mol/L yttrium nitrate, stirring at 50 ℃ to form sol, and then adding 0.5mol/L cerous nitrate in an equal volume to obtain the composite corrosion-resistant film layer sol.
(5) Coating a corrosion-resistant film layer by using sol: and (3) coating the corrosion-resistant film layer sol obtained in the step (4) on the surface of the magnesium rare earth alloy body obtained in the step (3) by adopting a dip-coating method, and preserving heat for 1.0-1.5 hours at the temperature of 150 ℃ to obtain the magnesium rare earth alloy.
5. The method for preparing the high-strength magnesium rare earth alloy material according to claim 4, wherein the method comprises the following steps: the lanthanum compound content in the lanthanum-cerium mixed rare earth is 25-35%, and the cerium compound content is 10-25%.
6. The method for preparing the high-strength magnesium rare earth alloy material according to claim 4, wherein the method comprises the following steps: the mass ratio of the potassium chloride to the sodium chloride to the calcium chloride to the magnesium chloride to the rare earth chloride is 1:3:4.5:200: 20.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115772622A (en) * | 2021-09-06 | 2023-03-10 | 武汉苏泊尔炊具有限公司 | Cooking utensil and preparation method thereof |
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| CN102317486A (en) * | 2008-01-09 | 2012-01-11 | 铸造Crc有限公司 | Magnesium based alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102317486A (en) * | 2008-01-09 | 2012-01-11 | 铸造Crc有限公司 | Magnesium based alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115772622A (en) * | 2021-09-06 | 2023-03-10 | 武汉苏泊尔炊具有限公司 | Cooking utensil and preparation method thereof |
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Application publication date: 20191220 |