A magnesium-neodymium alloy and a method for producing the same
By introducing modified nickel oxide into magnesium alloys, the problem of poor corrosion resistance of magnesium alloys was solved, the corrosion resistance and mechanical properties of magnesium alloys were improved, and the production process was simplified.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- LOUDI XINGXIN ALLOY
- Filing Date
- 2023-10-27
- Publication Date
- 2026-04-17
AI Technical Summary
Magnesium alloys have poor corrosion resistance, which limits their application in structural materials, and the production process is complex, resulting in a long production cycle.
Modified nickel oxide (prepared from graphene oxide, polyaniline, nickel oxide, silane coupling agent and aluminum) is used to improve the corrosion resistance of magnesium alloys. The modified nickel oxide is uniformly distributed on the surface of the magnesium alloy through specific smelting, casting and heat treatment processes to form a protective layer.
It significantly improves the corrosion resistance and mechanical properties of magnesium alloys, shortens the production cycle, and improves the plasticity of the alloys.
Abstract
Description
Technical Field
[0001] This invention belongs to the field of magnesium alloy technology, specifically a magnesium-neodymium alloy and its preparation method. Background Technology
[0002] Magnesium alloys possess advantages such as low density, high specific strength, high specific stiffness, and high damping; therefore, their application in lightweight fields such as automobiles, medical equipment, and aerospace vehicles is increasing. However, as structural materials, magnesium alloys have poor corrosion resistance, which significantly limits their applications. Therefore, improving the corrosion resistance of magnesium alloys will greatly broaden their practical applications.
[0003] Magnesium alloys exhibit poor corrosion resistance due to their low self-corrosion potential in actual solutions, making them highly susceptible to chemical and electrochemical reactions. Furthermore, magnesium alloys readily undergo micro-galvanic corrosion with second-phase or impurity elements (such as iron), further reducing their corrosion resistance and shortening their service life. This limits their widespread application, making the improvement of magnesium alloy corrosion resistance a significant research priority. Corrosion resistance can typically be improved through surface treatment and alloying. However, the production process of magnesium alloy sheets is complex, requiring a series of steps including smelting, casting, heat treatment, extrusion, and rolling, resulting in a long production cycle and relatively poor corrosion resistance. Summary of the Invention
[0004] The purpose of this invention is to provide a magnesium-neodymium alloy to solve at least one aspect of the problems and defects mentioned in the background art.
[0005] The present invention also provides a method for preparing the above-mentioned magnesium-neodymium alloy.
[0006] Specifically, the first aspect of this invention discloses a magnesium-neodymium alloy, comprising the following raw materials:
[0007] Magnesium ingots, neodymium, yttrium, and modified nickel oxide;
[0008] The modified nickel oxide comprises the following raw materials:
[0009] Graphene oxide, polyaniline, nickel oxide, silane coupling agent, and aluminum.
[0010] According to one technical solution of the magnesium-neodymium alloy technology of the present invention, at least the following beneficial effects are achieved:
[0011] In this invention, modified nickel oxide is prepared using graphene oxide, polyaniline, nickel oxide, silane coupling agent, and aluminum. Since both graphene oxide and nickel oxide have a layered structure, the layered structures interact under the action of the silane coupling agent, which helps to improve the stability of nickel oxide in the magnesium alloy matrix, thereby improving the corrosion resistance of the matrix.
[0012] During the preparation of magnesium alloys, polyaniline and graphene oxide are transformed into carbon materials. These carbon materials can effectively strengthen the magnesium matrix, thereby improving the mechanical properties of the magnesium alloy. At the same time, carbon materials can also act as a barrier to dislocation movement, preventing dislocations from moving in the metal and thus strengthening the metal. In addition, refining the grains can improve the plasticity of the alloy.
[0013] According to some embodiments of the present invention, the magnesium-aluminum alloy comprises the following raw materials in parts by weight:
[0014] 10 parts magnesium ingot, 0.2 to 0.4 parts neodymium, 0.6 to 0.9 parts yttrium, and 0.5 to 1 part modified nickel oxide.
[0015] According to some embodiments of the present invention, the magnesium ingot is composed of the following components in weight fractions:
[0016] Al 2.5%–3%, Zn 0.3%–0.5%, Mn 0.1%–0.2% and the balance being magnesium.
[0017] According to some embodiments of the present invention, the modified nickel oxide comprises the following raw materials in parts by weight:
[0018] 10 parts graphene oxide, 10 to 20 parts polyaniline, 5 to 10 parts nickel oxide, 0.5 to 1 part silane coupling agent, and 3 to 8 parts aluminum.
[0019] According to some embodiments of the present invention, the method for preparing nickel oxide includes the following steps:
[0020] The nickel salt and surfactant solution are mixed and reacted, followed by solid-liquid separation, and the solid is collected.
[0021] According to some embodiments of the present invention, the nickel salt is at least one of nickel nitrate and nickel chloride.
[0022] According to some embodiments of the present invention, the surfactant solution is composed of sodium dodecyl sulfate, acid and water.
[0023] According to some embodiments of the present invention, the mass concentration of sodium dodecyl sulfate in the surfactant solution is 3 g / L to 5 g / L.
[0024] According to some embodiments of the present invention, the acid is sulfuric acid.
[0025] According to some embodiments of the present invention, the molar concentration of acid in the surfactant solution is 0.01 mol / L to 0.1 mol / L.
[0026] According to some embodiments of the present invention, the mass-to-volume ratio of the nickel salt and the surfactant solution is 30g-40g:250mL.
[0027] According to some embodiments of the present invention, the silane coupling agent is KH550 or KH560.
[0028] The second aspect of this invention discloses a method for preparing the above-mentioned magnesium-neodymium alloy, comprising the following steps:
[0029] S1. Magnesium ingots, neodymium, and yttrium are melted under a protective atmosphere to obtain a molten liquid;
[0030] The molten liquid is refined to obtain a refined liquid;
[0031] S2. Cast 80% to 90% of the refined liquid to obtain the first magnesium-neodymium alloy ingot;
[0032] Modified nickel oxide was added to the remaining refining liquid to prepare the modified liquid;
[0033] S3. The modified liquid is cast into the first magnesium-neodymium alloy ingot to obtain the second magnesium-neodymium alloy ingot;
[0034] S4. The second magnesium-neodymium alloy ingot is homogenized, cooled for the first time, heat-preserving, hot-extruded, cooled for the second time, aged and air-cooled.
[0035] According to one technical solution of the preparation method of the present invention, at least the following beneficial effects are achieved:
[0036] This invention involves melting magnesium ingots, yttrium, and neodymium to form a solution and then casting it in batches. First, most of the solution is cast to obtain a first magnesium-neodymium alloy ingot. Then, modified nickel oxide is added to the remaining magnesium alloy solution, mixed thoroughly, and cast onto the surface of the first magnesium-neodymium alloy ingot. Utilizing the fluidity of the magnesium alloy solution, the modified nickel oxide is evenly distributed on the surface of the magnesium alloy ingot, thereby forming a protective layer with an embedded layer on the magnesium alloy surface. This gives the magnesium alloy surface high corrosion resistance and can effectively prevent external corrosive substances from penetrating into the magnesium alloy, thus giving the magnesium alloy material excellent corrosion resistance.
[0037] According to some embodiments of the present invention, the melting temperature in step S1 is 650°C to 700°C.
[0038] According to some embodiments of the present invention, the refining process employs a refining agent; the refining agent comprises the following raw materials in weight fractions:
[0039] Magnesium chloride 5%–20%, potassium chloride 15%–35%, sodium chloride 1%–10%, barium chloride 15%–40%, and calcium fluoride 10%–25%.
[0040] This invention significantly reduces the content of MgCl2 that reacts with rare earth elements. To improve slag removal, the proportion of barium salt in the slagging agent is increased, while the proportion of KCl is also increased. This ensures the flux has a low melting point, low viscosity, and good fluidity, reducing the surface tension of the entire flux system. This facilitates the adsorption of non-metallic inclusions in the magnesium melt by the flux, while minimizing the loss of rare earth elements. The addition of calcium fluoride mainly increases the density and viscosity of the flux, enabling the magnesium fluoride produced in the reaction to have a certain slag-forming ability on magnesium oxide.
[0041] According to some embodiments of the present invention, the amount of the refining agent added is 2% to 4%.
[0042] According to some embodiments of the present invention, the homogenization treatment temperature is 510°C to 530°C.
[0043] According to some embodiments of the present invention, the temperature of the heat preservation treatment is 510℃~530℃.
[0044] According to some embodiments of the present invention, the aging treatment includes the following heat preservation section:
[0045] First stage of heat preservation: temperature 90℃~110℃, time 3h~4h;
[0046] Second stage of heat preservation: temperature 200℃~210℃, time 8h~12h;
[0047] Third stage of heat preservation: temperature 170℃~180℃, time 3h~4h.
[0048] According to some embodiments of the present invention, the protective atmosphere consists of carbon dioxide and sulfur hexafluoride.
[0049] According to some embodiments of the present invention, the volume fraction of carbon dioxide in the protective atmosphere is 95% to 99%.
[0050] According to some embodiments of the present invention, the homogenization process takes 15 to 18 hours.
[0051] According to some embodiments of the present invention, the ratio of the cross-sectional area of the extrusion ingot to the cross-sectional area of the extruded magnesium alloy is 20 to 25:1.
[0052] According to some embodiments of the present invention, the final temperature of the first cooling is 60°C to 70°C.
[0053] According to some embodiments of the present invention, the second cooling method is water cooling.
[0054] According to some embodiments of the present invention, the method for preparing the modified nickel oxide includes the following steps:
[0055] The mixture of graphene oxide, polyaniline, nickel oxide, silane coupling agent, aluminum, and water was hydrothermally heated, and the solid and liquid components were separated, washed, and dried.
[0056] According to some embodiments of the present invention, the temperature of the hydrothermal treatment is 150°C to 160°C.
[0057] According to some embodiments of the present invention, the hydrothermal time is 8h to 12h. Detailed Implementation
[0058] The following will describe the concept and technical effects of the present invention clearly and completely with reference to embodiments, so as to fully understand the purpose, features and effects of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are all within the scope of protection of the present invention.
[0059] In the description of this invention, the terms "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0060] Unless otherwise specified in the examples, the procedures should be performed under standard conditions or conditions recommended by the manufacturer. Reagents or instruments whose manufacturers are not specified are all commercially available products.
[0061] In this embodiment of the invention, the polyaniline was purchased from Sigma-Aldrich polyaniline (jadeite alkali polyaniline, product number: 556459).
[0062] In this embodiment of the invention, the graphene oxide was purchased from Suzhou Carbon-rich Graphene's industrial-grade graphene oxide powder (sheet diameter: 1μm~30μm; number of layers: 1~3).
[0063] In embodiments of the present invention, the magnesium ingot is composed of the following components by weight fraction:
[0064] Al 2.8%, Zn 0.4%, Mn 0.15% and balance magnesium.
[0065] The aluminum was purchased from Yuanyang Technology's aluminum powder FLPG1.5 (average particle size D50 (μm): 1.5±0.5).
[0066] Example 1
[0067] This embodiment is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0068] 10 parts magnesium ingot, 0.25 parts neodymium, 0.7 parts yttrium and 0.8 parts modified nickel oxide.
[0069] Modified nickel oxide comprises the following raw materials in parts by weight:
[0070] 10 parts graphene oxide, 12 parts polyaniline, 8 parts nickel oxide, 0.8 parts silane coupling agent (KH560) and 6 parts aluminum.
[0071] The method for preparing nickel oxide consists of the following steps:
[0072] Nickel salt (nickel nitrate) and surfactant solution (composed of sodium dodecyl sulfate, acid (sulfuric acid) and water; the mass concentration of sodium dodecyl sulfate is 4 g / L, the molar concentration of acid is 0.04 mol / L, and the mass-to-volume ratio of nickel salt to surfactant solution is 35 g: 250 mL) were mixed and reacted (the reaction temperature was 95 °C and the reaction time was 60 min). The solid and liquid were separated, the solid was collected and dried.
[0073] The method for preparing modified nickel oxide consists of the following steps:
[0074] Graphene oxide, polyaniline, nickel oxide, silane coupling agent, aluminum, and water (the mass-to-volume ratio of graphene oxide to water is 1 g: 250 mL) were mixed and sonicated (30 min). After sonication, hydrothermal treatment was performed (hydrothermal temperature was 150 °C, and hydrothermal time was 10 h). After hydrothermal treatment, solid-liquid separation was performed, the solid phase was collected, and dried.
[0075] The preparation method of magnesium-neodymium alloy in this embodiment consists of the following steps:
[0076] S1. Magnesium ingots, neodymium, and yttrium are melted in a protective atmosphere (composed of carbon dioxide and sulfur hexafluoride, with a carbon dioxide volume fraction of 98%) to obtain a molten liquid.
[0077] The molten liquid is refined to obtain a refined liquid (at a temperature of 690℃);
[0078] The refining process involves adding a refining agent (2% by weight); the refining agent consists of the following raw materials by weight fraction:
[0079] The formula consists of 10% magnesium chloride, 30% potassium chloride, 10% sodium chloride, 30% barium chloride, and 20% calcium fluoride.
[0080] S2. Cast 85% of the refined liquid to obtain the first magnesium-neodymium alloy ingot;
[0081] Modified nickel oxide was added to the remaining refining liquid to prepare the modified liquid;
[0082] S3. The modified liquid is cast into the first magnesium-neodymium alloy ingot to obtain the second magnesium-neodymium alloy ingot;
[0083] S4. Homogenize the second magnesium-neodymium alloy ingot (temperature 520℃, time 18h), first cooling (water cooling, final temperature 70℃), heat treatment (temperature 520℃, time 40min), hot extrusion (the ratio of the cross-sectional area of the extruded ingot to the cross-sectional area of the extruded magnesium alloy is 23:1), second cooling (water quenching), aging treatment and air cooling.
[0084] The aging treatment consists of the following insulation sections:
[0085] First stage of insulation: temperature 100℃, time 3.5h;
[0086] Second stage insulation: temperature 210℃, time 10 hours;
[0087] Third stage of heat preservation: temperature 170℃, time 4 hours.
[0088] Example 2
[0089] This embodiment is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0090] 10 parts magnesium ingot, 0.2 parts neodymium, 0.9 parts yttrium and 0.5 parts modified nickel oxide.
[0091] Modified nickel oxide comprises the following raw materials in parts by weight:
[0092] 10 parts graphene oxide, 10 parts polyaniline, 10 parts nickel oxide, 1 part silane coupling agent (KH560) and 8 parts aluminum.
[0093] The method for preparing nickel oxide consists of the following steps:
[0094] Nickel salt (nickel nitrate) and surfactant solution (composed of sodium dodecyl sulfate, acid (sulfuric acid) and water; the mass concentration of sodium dodecyl sulfate is 4 g / L, the molar concentration of acid is 0.04 mol / L, and the mass-to-volume ratio of nickel salt to surfactant solution is 35 g: 250 mL) were mixed and reacted (the reaction temperature was 95 °C and the reaction time was 60 min). The solid and liquid were separated, the solid was collected and dried.
[0095] The method for preparing modified nickel oxide consists of the following steps:
[0096] Graphene oxide, polyaniline, nickel oxide, silane coupling agent, aluminum and water were mixed and sonicated (30 min). After sonication, hydrothermal treatment was performed (hydrothermal temperature 150℃, hydrothermal time 10 h). After hydrothermal treatment, solid-liquid separation was performed, the solid phase was collected and dried.
[0097] The preparation method of magnesium-neodymium alloy in this embodiment consists of the following steps:
[0098] S1. Magnesium ingots, neodymium, and yttrium are melted in a protective atmosphere (composed of carbon dioxide and sulfur hexafluoride, with a carbon dioxide volume fraction of 98%) to obtain a molten liquid.
[0099] The molten liquid is refined to obtain a refined liquid (at a temperature of 690℃);
[0100] The refining process involves adding a refining agent (2% by weight); the refining agent consists of the following raw materials by weight fraction:
[0101] The formula consists of 10% magnesium chloride, 30% potassium chloride, 10% sodium chloride, 30% barium chloride, and 20% calcium fluoride.
[0102] S2. Cast 85% of the refined liquid to obtain the first magnesium-neodymium alloy ingot;
[0103] Modified nickel oxide was added to the remaining refining liquid to prepare the modified liquid;
[0104] S3. The modified liquid is cast into the first magnesium-neodymium alloy ingot to obtain the second magnesium-neodymium alloy ingot;
[0105] S4. Homogenize the second magnesium-neodymium alloy ingot (temperature 520℃, time 18h), first cooling (water cooling, final temperature 70℃), heat treatment (temperature 520℃, time 40min), hot extrusion (the ratio of the cross-sectional area of the extruded ingot to the cross-sectional area of the extruded magnesium alloy is 23:1), second cooling (water quenching), aging treatment and air cooling.
[0106] The aging treatment consists of the following insulation sections:
[0107] First stage of insulation: temperature 90℃, time 4 hours;
[0108] Second stage insulation: temperature 200℃, time 12 hours;
[0109] Third stage of heat preservation: temperature 180℃, time 3 hours.
[0110] Example 3
[0111] This embodiment is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0112] 10 parts magnesium ingot, 0.4 parts neodymium, 0.6 parts yttrium and 0.5 parts modified nickel oxide.
[0113] Modified nickel oxide comprises the following raw materials in parts by weight:
[0114] 10 parts graphene oxide, 20 parts polyaniline, 10 parts nickel oxide, 1 part silane coupling agent (KH560), and 3 parts aluminum.
[0115] The method for preparing nickel oxide consists of the following steps:
[0116] Nickel salt (nickel nitrate) and surfactant solution (composed of sodium dodecyl sulfate, acid (sulfuric acid) and water; the mass concentration of sodium dodecyl sulfate is 4 g / L, the molar concentration of acid is 0.04 mol / L, and the mass-to-volume ratio of nickel salt to surfactant solution is 35 g: 250 mL) were mixed and reacted (the reaction temperature was 95 °C and the reaction time was 60 min). The solid and liquid were separated, the solid was collected and dried.
[0117] The method for preparing modified nickel oxide consists of the following steps:
[0118] Graphene oxide, polyaniline, nickel oxide, silane coupling agent, aluminum and water were mixed and sonicated (30 min). After sonication, hydrothermal treatment was performed (hydrothermal temperature 150℃, hydrothermal time 10 h). After hydrothermal treatment, solid-liquid separation was performed, the solid phase was collected and dried.
[0119] The preparation method of magnesium-neodymium alloy in this embodiment consists of the following steps:
[0120] S1. Magnesium ingots, neodymium, and yttrium are melted in a protective atmosphere (composed of carbon dioxide and sulfur hexafluoride, with a carbon dioxide volume fraction of 98%) to obtain a molten liquid.
[0121] The molten liquid is refined to obtain a refined liquid (at a temperature of 690℃);
[0122] The refining process involves adding a refining agent (2% by weight); the refining agent consists of the following raw materials by weight fraction:
[0123] The formula consists of 10% magnesium chloride, 30% potassium chloride, 10% sodium chloride, 30% barium chloride, and 20% calcium fluoride.
[0124] S2. Cast 85% of the refined liquid to obtain the first magnesium-neodymium alloy ingot;
[0125] Modified nickel oxide was added to the remaining refining liquid to prepare the modified liquid;
[0126] S3. The modified liquid is cast into the first magnesium-neodymium alloy ingot to obtain the second magnesium-neodymium alloy ingot;
[0127] S4. Homogenize the second magnesium-neodymium alloy ingot (temperature 520℃, time 18h), first cooling (water cooling, final temperature 70℃), heat treatment (temperature 520℃, time 40min), hot extrusion (the ratio of the cross-sectional area of the extruded ingot to the cross-sectional area of the extruded magnesium alloy is 23:1), second cooling (water quenching), aging treatment and air cooling.
[0128] The aging treatment consists of the following insulation sections:
[0129] First stage of insulation: temperature 110℃, time 3 hours;
[0130] Second stage insulation: temperature 200℃, time 10 hours;
[0131] Third stage of heat preservation: temperature 170℃, time 4 hours.
[0132] Example 4
[0133] This embodiment is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0134] 10 parts magnesium ingot, 0.3 parts neodymium, 0.7 parts yttrium and 0.9 parts modified nickel oxide.
[0135] Modified nickel oxide comprises the following raw materials in parts by weight:
[0136] 10 parts graphene oxide, 17 parts polyaniline, 7 parts nickel oxide, 0.7 parts silane coupling agent (KH560) and 5 parts aluminum.
[0137] The method for preparing nickel oxide consists of the following steps:
[0138] Nickel salt (nickel nitrate) and surfactant solution (composed of sodium dodecyl sulfate, acid (sulfuric acid) and water; the mass concentration of sodium dodecyl sulfate is 4 g / L, the molar concentration of acid is 0.04 mol / L, and the mass-to-volume ratio of nickel salt to surfactant solution is 35 g: 250 mL) were mixed and reacted (the reaction temperature was 95 °C and the reaction time was 60 min). The solid and liquid were separated, the solid was collected and dried.
[0139] The method for preparing modified nickel oxide consists of the following steps:
[0140] Graphene oxide, polyaniline, nickel oxide, silane coupling agent, aluminum and water were mixed and sonicated (30 min). After sonication, hydrothermal treatment was performed (hydrothermal temperature 150℃, hydrothermal time 10 h). After hydrothermal treatment, solid-liquid separation was performed, the solid phase was collected and dried.
[0141] The preparation method of magnesium-neodymium alloy in this embodiment consists of the following steps:
[0142] S1. Magnesium ingots, neodymium, and yttrium are melted in a protective atmosphere (composed of carbon dioxide and sulfur hexafluoride, with a carbon dioxide volume fraction of 98%) to obtain a molten liquid.
[0143] The molten liquid is refined to obtain a refined liquid (at a temperature of 690℃);
[0144] The refining process involves adding a refining agent (2% by weight); the refining agent consists of the following raw materials by weight fraction:
[0145] The formula consists of 10% magnesium chloride, 30% potassium chloride, 10% sodium chloride, 30% barium chloride, and 20% calcium fluoride.
[0146] S2. Cast 85% of the refined liquid to obtain the first magnesium-neodymium alloy ingot;
[0147] Modified nickel oxide was added to the remaining refining liquid to prepare the modified liquid;
[0148] S3. The modified liquid is cast into the first magnesium-neodymium alloy ingot to obtain the second magnesium-neodymium alloy ingot;
[0149] S4. Homogenize the second magnesium-neodymium alloy ingot (temperature 520℃, time 18h), first cooling (water cooling, final temperature 70℃), heat treatment (temperature 520℃, time 40min), hot extrusion (the ratio of the cross-sectional area of the extruded ingot to the cross-sectional area of the extruded magnesium alloy is 23:1), second cooling (water quenching), aging treatment and air cooling.
[0150] The aging treatment consists of the following insulation sections:
[0151] First stage of insulation: temperature 110℃, time 3 hours;
[0152] Second stage insulation: temperature 200℃, time 10 hours;
[0153] Third stage of heat preservation: temperature 170℃, time 4 hours.
[0154] Example 5
[0155] This embodiment is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0156] 10 parts magnesium ingot, 0.22 parts neodymium, 0.65 parts yttrium and 0.6 parts modified nickel oxide.
[0157] Modified nickel oxide comprises the following raw materials in parts by weight:
[0158] 10 parts graphene oxide, 10 parts polyaniline, 5 parts nickel oxide, 0.5 parts silane coupling agent (KH560) and 3 parts aluminum.
[0159] The method for preparing nickel oxide consists of the following steps:
[0160] Nickel salt (nickel nitrate) and surfactant solution (composed of sodium dodecyl sulfate, acid (sulfuric acid) and water; the mass concentration of sodium dodecyl sulfate is 4 g / L, the molar concentration of acid is 0.04 mol / L, and the mass-to-volume ratio of nickel salt to surfactant solution is 35 g: 250 mL) were mixed and reacted (the reaction temperature was 95 °C and the reaction time was 60 min). The solid and liquid were separated, the solid was collected and dried.
[0161] The method for preparing modified nickel oxide consists of the following steps:
[0162] Graphene oxide, polyaniline, nickel oxide, silane coupling agent, aluminum and water were mixed and sonicated (30 min). After sonication, hydrothermal treatment was performed (hydrothermal temperature 150℃, hydrothermal time 10 h). After hydrothermal treatment, solid-liquid separation was performed, the solid phase was collected and dried.
[0163] The preparation method of magnesium-neodymium alloy in this embodiment consists of the following steps:
[0164] S1. Magnesium ingots, neodymium, and yttrium are melted in a protective atmosphere (composed of carbon dioxide and sulfur hexafluoride, with a carbon dioxide volume fraction of 98%) to obtain a molten liquid.
[0165] The molten liquid is refined to obtain a refined liquid (at a temperature of 690℃);
[0166] The refining process involves adding a refining agent (2% by weight); the refining agent consists of the following raw materials by weight fraction:
[0167] The formula consists of 10% magnesium chloride, 30% potassium chloride, 10% sodium chloride, 30% barium chloride, and 20% calcium fluoride.
[0168] S2. Cast 85% of the refined liquid to obtain the first magnesium-neodymium alloy ingot;
[0169] Modified nickel oxide was added to the remaining refining liquid to prepare the modified liquid;
[0170] S3. The modified liquid is cast into the first magnesium-neodymium alloy ingot to obtain the second magnesium-neodymium alloy ingot;
[0171] S4. Homogenize the second magnesium-neodymium alloy ingot (temperature 520℃, time 18h), first cooling (water cooling, final temperature 70℃), heat treatment (temperature 520℃, time 40min), hot extrusion (the ratio of the cross-sectional area of the extruded ingot to the cross-sectional area of the extruded magnesium alloy is 23:1), second cooling (water quenching), aging treatment and air cooling.
[0172] The aging treatment consists of the following insulation sections:
[0173] First stage of insulation: temperature 90℃, time 3 hours;
[0174] Second stage insulation: temperature 200℃, time 8 hours;
[0175] Third stage of heat preservation: temperature 170℃, time 3 hours.
[0176] Comparative Example 1
[0177] This comparative example is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0178] 10 parts magnesium ingot, 0.22 parts neodymium, 0.65 parts yttrium and 0.6 parts modified nickel oxide.
[0179] Modified nickel oxide comprises the following raw materials in parts by weight:
[0180] 10 parts graphene oxide, 10 parts polyaniline, 5 parts nickel oxide, and 3 parts aluminum.
[0181] The preparation method of nickel oxide is as described in Example 5.
[0182] The method for preparing modified nickel oxide consists of the following steps:
[0183] Graphene oxide, polyaniline, nickel oxide, aluminum and water were mixed and sonicated (30 min). After sonication, hydrothermal treatment was performed (hydrothermal temperature 150℃, hydrothermal time 10 h). After hydrothermal treatment, solid-liquid separation was performed, the solid phase was collected and dried.
[0184] The preparation method of the magnesium-neodymium alloy in this comparative example is the same as that in Example 5.
[0185] Comparative Example 2
[0186] This comparative example is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0187] 10 parts magnesium ingot, 0.22 parts neodymium, 0.65 parts yttrium and 0.6 parts modified nickel oxide.
[0188] Modified nickel oxide comprises the following raw materials in parts by weight:
[0189] 10 parts graphene oxide, 5 parts nickel oxide and 3 parts aluminum.
[0190] The preparation method of nickel oxide is as described in Example 5.
[0191] The method for preparing modified nickel oxide consists of the following steps:
[0192] Graphene oxide, nickel oxide, aluminum and water were mixed and sonicated (30 min). After sonication, hydrothermal treatment was performed (hydrothermal temperature 150℃, hydrothermal time 10 h). After hydrothermal treatment, solid-liquid separation was performed, the solid phase was collected and dried.
[0193] The preparation method of the magnesium-neodymium alloy in this comparative example is the same as that in Example 5.
[0194] Comparative Example 3
[0195] This comparative example is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0196] 10 parts magnesium ingot, 0.22 parts neodymium, 0.65 parts yttrium and 0.6 parts modified nickel oxide.
[0197] Modified nickel oxide comprises the following raw materials in parts by weight:
[0198] 10 parts graphene oxide, 10 parts polyaniline, and 5 parts nickel oxide.
[0199] The preparation method of nickel oxide is as described in Example 5.
[0200] The method for preparing modified nickel oxide consists of the following steps:
[0201] After mixing graphene oxide, polyaniline, nickel oxide and water, the mixture was sonicated (30 min). After sonication, the mixture was hydrothermally heated (150 °C for 10 h). After hydrothermal heating, the solid and liquid phases were separated, the solid phase was collected and dried.
[0202] The preparation method of the magnesium-neodymium alloy in this comparative example is the same as that in Example 5.
[0203] Comparative Example 4
[0204] This comparative example is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0205] 10 parts magnesium ingot, 0.22 parts neodymium, 0.65 parts yttrium and 0.6 parts modified nickel oxide.
[0206] Modified nickel oxide comprises the following raw materials in parts by weight:
[0207] 10 parts graphene oxide and 5 parts nickel oxide.
[0208] The preparation method of nickel oxide is as described in Example 5.
[0209] The method for preparing modified nickel oxide consists of the following steps:
[0210] After mixing graphene oxide, nickel oxide and water, the mixture was sonicated (30 min). After sonication, the mixture was hydrothermally heated (150 °C for 10 h). After hydrothermal heating, the solid and liquid phases were separated, the solid phase was collected and dried.
[0211] The preparation method of the magnesium-neodymium alloy in this comparative example is the same as that in Example 5.
[0212] Comparative Example 5
[0213] This comparative example is a magnesium-neodymium alloy, comprising the following raw materials in parts by weight:
[0214] 10 parts magnesium ingot, 0.22 parts neodymium, 0.65 parts yttrium and 0.6 parts nickel oxide.
[0215] The preparation method of nickel oxide is as described in Example 5.
[0216] Hydrogen evolution rate: Magnesium-neodymium alloy samples obtained in Examples 1-5 and Comparative Examples 1-5 were immersed in a 3.5% NaCl solution for 480 h; the test results are shown in Table 1.
[0217] Table 1. Performance test results of the magnesium-neodymium alloys prepared in Examples 1-5 and Comparative Examples 1-5 of the present invention.
[0218] - Yield strength (MPa) <![CDATA[Hydrogen evolution rate (mL·cm -2 ·day -1 )]]> Example 1 483 0.023 Example 2 476 0.025 Example 3 472 0.028 Example 4 469 0.031 Example 5 461 0.034 Comparative Example 1 414 0.052 Comparative Example 2 426 0.087 Comparative Example 3 398 0.098 Comparative Example 4 346 0.132 Comparative Example 5 325 0.153
[0219] In summary, the modified nickel oxide in this invention is prepared using graphene oxide, polyaniline, nickel oxide, a silane coupling agent, and aluminum. Since both graphene oxide and nickel oxide have layered structures, the layers interact under the action of the silane coupling agent, which helps improve the stability of nickel oxide in the magnesium alloy matrix, thereby enhancing the corrosion resistance of the matrix. Furthermore, polyaniline and graphene oxide are converted into carbon materials during the magnesium alloy preparation process. These carbon materials can significantly strengthen the magnesium matrix, thus improving the mechanical properties of the magnesium alloy. Simultaneously, the carbon materials can act as a barrier to dislocation movement, preventing dislocations from moving and thus strengthening the metal. Additionally, grain refinement can improve the alloy's plasticity.
[0220] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above descriptions are merely specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A magnesium-neodymium alloy, characterized in that, The following raw materials are included in the preparation: 10 parts magnesium ingot, 0.2 to 0.4 parts neodymium, 0.6 to 0.9 parts yttrium, and 0.5 to 1 part modified nickel oxide; The modified nickel oxide comprises the following raw materials in parts by weight: 10 parts graphene oxide, 10 to 20 parts polyaniline, 5 to 10 parts nickel oxide, 0.5 to 1 part silane coupling agent, and 3 to 8 parts aluminum; The method for preparing the modified nickel oxide includes the following steps: The mixture of graphene oxide, polyaniline, nickel oxide, silane coupling agent, aluminum, and water was hydrothermally heated, and the solid and liquid components were separated, washed, and dried.
2. The magnesium-neodymium alloy according to claim 1, characterized in that, The temperature of the hydrothermal treatment is 150℃~160℃.
3. The magnesium-neodymium alloy according to claim 1, characterized in that, The hydrothermal treatment time is 8h~12h.
4. The magnesium-neodymium alloy according to claim 1, characterized in that, The magnesium ingot is composed of the following components by weight fraction: Al 2.5%~3%, Zn 0.3%~0.5%, Mn 0.1%~0.2% and the balance is magnesium.
5. A method for preparing a magnesium-neodymium alloy as described in any one of claims 1 to 4, characterized in that, Includes the following steps: S1. Magnesium ingots, neodymium, and yttrium are melted under a protective atmosphere to obtain a molten liquid; The molten liquid is refined to obtain a refined liquid; S2. Cast 80%~90% of the refined liquid to obtain the first magnesium-neodymium alloy ingot; Modified nickel oxide was added to the remaining refining liquid to prepare the modified liquid; S3. The modified liquid is cast into the first magnesium-neodymium alloy ingot to obtain the second magnesium-neodymium alloy ingot; S4. The second magnesium-neodymium alloy ingot is homogenized, cooled for the first time, heat-preserving, hot-extruded, cooled for the third time, aged and air-cooled.
6. The preparation method according to claim 5, characterized in that, The melting temperature in step S1 is 650℃~700℃.
7. The preparation method according to claim 5, characterized in that, The refining process employs a refining agent; the refining agent comprises the following raw materials by weight fraction: Magnesium chloride 5%~20%, potassium chloride 15%~35%, sodium chloride 1%~10%, barium chloride 15%~40%, and calcium fluoride 10%~25%; The amount of the refining agent added is 2% to 4%.
8. The preparation method according to claim 5, characterized in that, The homogenization process is carried out at a temperature of 510℃ to 530℃.
9. The preparation method according to claim 5, characterized in that, The temperature for the heat preservation treatment is 510℃~530℃.
10. The preparation method according to claim 5, characterized in that, The aging process includes the following insulation sections: First stage of heat preservation: temperature 90℃~110℃, time 3h~4h; Second stage of heat preservation: temperature 200℃~210℃, time 8h~12h; Third stage of heat preservation: temperature 170℃~180℃, time 3h~4h.
Citation Information
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