CN113563089A - Method for recovering nano ceramic particles in magnesium-based composite material - Google Patents
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Abstract
A method for recovering nano ceramic particles in a magnesium-based composite material relates to the field of nano material manufacturing. The invention aims to solve the problem of waste of a large amount of resources because the high-content reinforcement in the nano ceramic particle reinforced magnesium matrix composite cannot be reused after the nano ceramic particle reinforced magnesium matrix composite loses efficacy. The invention heats and melts the magnesium-based composite material which contains the ineffective nano ceramic particles; mixing and grinding sodium chloride, potassium chloride and calcium fluoride, adding the mixture into a magnesium alloy melt, stirring, standing, and cooling a crucible containing a metal melt and a molten salt by water. And finally, soaking the cast ingot in the aqueous solution for a period of time to obtain a suspension containing the nano ceramic particles. And washing the suspension for multiple times to recover the nano ceramic particles. The invention is a simple and efficient reinforcement recycling technology. Has great economic benefit for recycling the nano ceramic particles with high added value. The invention is applied to the field of material recovery.
Description
Technical Field
The invention belongs to the field of nano material manufacturing, and particularly relates to a method for recovering nano ceramic particles in a magnesium-based composite material.
Background
Magnesium is the lightest metal structure material, and the density of pure magnesium is 1.7g/cm3. Magnesium has high specific stiffness and specific strength, good damping performance and electromagnetic shielding performance and good biocompatibility, and has abundant reserves on the earth, so that magnesium and magnesium alloy have great potential for improving energy efficiency and improving the overall performance of a system in the aspects of aviation, automobiles, national defense, 3C products and biomedical treatment. However, magnesium and magnesium alloys have low absolute strength, poor creep resistance, and poor corrosion resistance at room temperature and low temperature, which in turn largely limit the wide application of magnesium alloys. These disadvantages of magnesium alloys can be ameliorated by preparing a composite material by incorporating reinforcement into the magnesium alloy. In recent years, the metal matrix composite material formed by combining the nano ceramic particles and the metal matrix and realizing excellent interface combination through regulating and controlling the tissue process has high strength, high modulus and good dimensional stability, and has wide application prospect in the fields of automobiles, aerospace, electronic communication and the like. However, as the related art matures, a great deal of composite material failure must result. The preparation process of the nano reinforcement in the composite material is very complicated. The cost of the nano-ceramic particles is enormous. The recycling of high levels of nano-ceramic particles in composite materials will therefore become increasingly important. This will help to reduce the cost of the nano-ceramic particles while effectively alleviating the waste of resources. However, at present, no technology for recycling the nano reinforcement in the composite material exists. The development of a simple and efficient recovery technology of the nano ceramic particles in the magnesium-based composite material has great value.
Disclosure of Invention
The invention aims to provide a method for solving the problem of waste of a large amount of resources caused by the fact that after a nano ceramic particle reinforced magnesium-based composite material loses efficacy, a high-content reinforcement body in the nano ceramic particle reinforced magnesium-based composite material cannot be reused. Thereby providing a method for recycling the nano ceramic particles in the magnesium-based composite material, which has simple process flow, low cost and feasibility and meets the requirement of environmental protection.
The invention relates to a method for recovering nano ceramic particles in a magnesium-based composite material, which is carried out according to the following steps:
firstly, heating and melting the waste or failed nano ceramic particle reinforced magnesium-based composite material in a crucible at a temperature 30-100 ℃ higher than the melting point of a matrix magnesium alloy;
secondly, mixing and grinding sodium chloride, potassium chloride and calcium fluoride, then gradually adding the ground mixture into the magnesium alloy melt in the crucible, mechanically stirring the mixture to promote the mixed salt and the metal melt to be fully mixed, stopping stirring after the mixed salt is completely melted, and standing;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano ceramic particles and the mixed salt;
fourthly, soaking the ingot solidified in the previous step in an aqueous solution for 3-15 hours to obtain a suspension containing the nano ceramic particles, and filtering the suspension to remove a salt solution to obtain the nano ceramic particles;
and fifthly, washing the nano ceramic particles in distilled water, filtering, repeating the washing and filtering steps for 3-5 times, and drying to obtain clean nano ceramic particles.
Further, the discarded or failed nano ceramic particle reinforced magnesium-based composite material in the step one is heated and melted in the crucible at the temperature of 730 ℃.
Further, the discarded or failed nano ceramic particle reinforced magnesium-based composite material in the step one is heated and melted in the crucible at the temperature of 730 ℃.
Further, in the second step, the mass ratio of the sodium chloride to the potassium chloride to the calcium fluoride is 4-6: 3-5: 1.
Further, in the second step, the mass ratio of the sodium chloride to the potassium chloride to the calcium fluoride is 5:4: 1.
Further, in the second step, the mass ratio of the sodium chloride to the potassium chloride to the calcium fluoride is 3-5: 1, and magnesium chloride accounting for 10% of the total mass of the mixed salt is added for grinding.
Further, in the second step, the mass ratio of the sodium chloride to the potassium chloride to the calcium fluoride is 4:4:1, and the magnesium chloride accounting for 10% of the total mass of the mixed salt is added for grinding.
And further, adding mixed salt into the magnesium alloy melt in the third step, stirring for 10-20 min, and standing for 30-40 min.
And further, adding mixed salt into the magnesium alloy melt in the third step, stirring for 20min, and standing for 30 min.
Further, in the fourth step, the ingot solidified in the last step is soaked in the aqueous solution for 5-10 hours.
Further, the failed nano ceramic particle reinforced magnesium-based composite material is a nano silicon carbide reinforced magnesium-based composite material or a titanium carbide and silicon carbide mixed reinforced magnesium-based composite material.
The invention has the following beneficial effects:
the invention provides a new idea for recycling high-added-value nano ceramic particles, and the green extraction and utilization of the nano ceramic particles in the magnesium melt in large batch can be directly realized by utilizing the difference of wettability of mixed molten salt, the magnesium melt and the nano ceramic particles and the driving of surface tension and gravity. There is no mature recovery technology for nano ceramic particles in metal matrix, and it is usually necessary to use acid solution extraction process to obtain nano ceramic particles in metal matrix, which is expensive and causes surface damage and destruction of particles during soaking in acid solution. In addition, such processes also pose serious environmental pollution problems. The invention utilizes the adsorption effect of the reinforcement on the mixed molten salt, realizes the extraction of the reinforcement in one step, does not weaken the quality of the reinforcement in the recovery process, has very low cost and is very suitable for being popularized to industrial production. In addition, in the related technology, the properties of the molten salt melt are effectively changed by adopting the multi-element mixed metal salt, and meanwhile, the melting point of the molten salt is effectively reduced by selecting the multi-principal-element metal salt, so that the experiment is easy to operate.
Drawings
FIG. 1 is a macroscopic optical topography of the metal salt of example 1 after addition to the composite melt and solidification;
FIG. 2 is a graph of the morphology of titanium carbide in a metal mixed salt of example 1;
FIG. 3 is a graph of the element distribution of FIG. 2; wherein, the images b-g are element distribution spectrograms of the area of the image a;
FIG. 4 is a morphology chart of the titanium carbide powder washed by the scheme of example 1.
Detailed Description
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the invention, and that various changes in form and details may be made therein without departing from the spirit and scope of the invention in practice.
To make the objects, aspects and advantages of the embodiments of the present invention more apparent, the following detailed description clearly illustrates the spirit of the disclosure, and any person skilled in the art, after understanding the embodiments of the disclosure, may make changes and modifications to the technology taught by the disclosure without departing from the spirit and scope of the disclosure.
The exemplary embodiments of the present invention and the description thereof are provided to explain the present invention and not to limit the present invention.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1
The method for recovering the nano ceramic particles in the magnesium-based composite material comprises the following steps:
firstly, heating and melting a scrapped or failed nano titanium carbide particle reinforced magnesium-based composite material member in a crucible at 700 ℃ to obtain a magnesium alloy melt;
mixing and grinding three metal salts of sodium chloride, potassium chloride and calcium fluoride according to a ratio of 4:4:1, then sequentially adding the three metal salts into the magnesium alloy melt, gradually stirring for 10min, standing for 30min after the mixed salts are completely melted, and promoting titanium carbide particles to spontaneously move from the magnesium alloy matrix to the mixed molten salt;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the titanium carbide particles and the mixed salt;
fourthly, soaking the cast ingot in the water solution for 3 to 5 hours to completely dissolve the crystal salt on the surface of the cast ingot into the water solution to obtain suspension containing the nano titanium carbide particles
Fifthly, washing and drying for multiple times to obtain clean nano titanium carbide particles.
FIG. 1 macroscopic optical appearance of a metal salt after addition to a composite melt to solidify. The solidified samples were found to have distinct top and bottom delamination characteristics. And at the same time, the part containing the mixed salt in the upper part is completely converted into black, which indicates that the ceramic particles in the magnesium-based composite material are transferred from the magnesium matrix to the mixed salt.
FIG. 2 shows the morphology of titanium carbide in a metal mixed salt; FIG. 3(b-g) is a diagram showing the distribution of elements in the region of FIG. (a). Significant Mg, Na, K, Cl elements can be found in the mixed molten salt, indicating that the upper part is the mixed molten metal zone. Meanwhile, the C and Ti elements are obviously enriched. Shows that the nano titanium carbide ceramic particles are extracted by the molten salt
FIG. 3 shows the morphology of the washed titanium carbide powder. The feasibility of extracting the nano ceramic particles in the magnesium-based composite material is proved.
Example 2
The method for recovering the nano ceramic particles in the magnesium-based composite material comprises the following steps:
firstly, heating and melting the failed nano silicon carbide particle reinforced magnesium-based composite material member in a crucible at 700 ℃;
secondly, mixing four metal salts of sodium chloride, potassium chloride, magnesium chloride and calcium fluoride according to a ratio of 4:4: 1: 1 proportion, then adding the mixture to the magnesium alloy melt in turn and stirring the mixture gradually for 10 min. Standing for 30min after the mixed salt is completely melted to promote the reinforcement to move from the magnesium alloy matrix to the mixed molten salt spontaneously;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano silicon carbide particles and the mixed salt;
soaking the ingot in the aqueous solution for 10 hours to completely dissolve the crystal salt on the surface of the ingot into the aqueous solution to obtain a suspension containing nano silicon carbide particles;
fifthly, washing and drying for multiple times to obtain clean nano silicon carbide particles.
Example 3
The method for recovering the nano ceramic particles in the magnesium-based composite material comprises the following steps:
firstly, heating and melting a failed nano titanium carbide particle reinforced magnesium-based composite material member in a crucible at 700 ℃;
secondly, mixing four metal salts of sodium chloride, potassium chloride, magnesium chloride and calcium fluoride according to a ratio of 4:4: 1: 1 proportion, then adding the mixture to the magnesium alloy melt in turn and stirring the mixture gradually for 10 min. Standing for 30min after the mixed salt is completely melted to promote the reinforcement to move from the magnesium alloy matrix to the mixed molten salt spontaneously;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano titanium carbide and the mixed salt;
fourthly, soaking the cast ingot in the water solution for 10 hours to completely dissolve the crystal salt on the surface of the cast ingot into the water solution to obtain suspension containing the nano titanium carbide
Fifthly, washing and drying for multiple times to obtain clean nano titanium carbide.
Claims (10)
1. The method for recovering the nano ceramic particles in the magnesium-based composite material is characterized by comprising the following steps of:
firstly, heating and melting the waste or failed nano ceramic particle reinforced magnesium-based composite material in a crucible at a temperature 30-100 ℃ higher than the melting point of a matrix magnesium alloy;
secondly, mixing and grinding sodium chloride, potassium chloride and calcium fluoride, then adding the ground mixture into a magnesium alloy melt in a crucible, mechanically stirring the mixture to promote the mixed salt and the metal melt to be fully mixed, stopping stirring after the mixed salt is completely melted, and standing;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano ceramic particles and the mixed salt;
fourthly, soaking the ingot solidified in the previous step in an aqueous solution for 3-15 hours to obtain a suspension containing the nano ceramic particles, and filtering the suspension to remove a salt solution to obtain the nano ceramic particles;
and fifthly, washing the nano ceramic particles in distilled water, filtering, repeating the washing and filtering steps for 3-5 times, and drying to obtain clean nano ceramic particles.
2. The method as claimed in claim 1, wherein the step one of melting the waste or failed mg-based composite material reinforced with nano ceramic particles in the crucible by heating at 730 ℃.
3. The method for recycling the nano ceramic particles in the magnesium-based composite material as claimed in claim 1, wherein the mass ratio of the sodium chloride, the potassium chloride and the calcium fluoride in the second step is 4-6: 3-5: 1.
4. The method as claimed in claim 3, wherein the mass ratio of sodium chloride, potassium chloride and calcium fluoride in the second step is 5:4: 1.
5. The method as claimed in claim 1, wherein the mass ratio of sodium chloride, potassium chloride and calcium fluoride in the second step is 3-5: 1, and magnesium chloride is added in an amount of 10% by mass of the total mixed salt to grind the magnesium-based composite material.
6. The method as claimed in claim 1, wherein the mass ratio of sodium chloride, potassium chloride and calcium fluoride in the second step is 4:4:1, and magnesium chloride is added in an amount of 10% by mass of the total mixed salt to grind the magnesium-based composite material.
7. The method for recycling the nano ceramic particles in the magnesium-based composite material as claimed in claim 1, wherein the step three is to add the mixed salt into the magnesium alloy melt and stir for 10-20 min, and the standing time is 30-40 min.
8. The method as claimed in claim 1, wherein the step three is carried out by adding mixed salt into the magnesium alloy melt, stirring for 20min, and standing for 30 min.
9. The method as claimed in claim 1, wherein the ingot solidified in the previous step is immersed in the aqueous solution for 5-10 hours.
10. The method as claimed in claim 1, wherein the failed nano ceramic particle reinforced Mg-based composite is nano silicon carbide reinforced Mg-based composite or mixture of titanium carbide and silicon carbide reinforced Mg-based composite.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114522965A (en) * | 2022-03-12 | 2022-05-24 | 湖北智烨新能科技有限公司 | Green and environment-friendly recycling method for new energy material |
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2021
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Patent Citations (8)
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| US5080715A (en) * | 1990-11-05 | 1992-01-14 | Alcan International Limited | Recovering clean metal and particulates from metal matrix composites |
| JPH07138668A (en) * | 1992-11-04 | 1995-05-30 | Shikoku Chem Corp | Method for recovering aluminum from aluminum-based composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114522965A (en) * | 2022-03-12 | 2022-05-24 | 湖北智烨新能科技有限公司 | Green and environment-friendly recycling method for new energy material |
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