CN114807658B - Magnesium-based composite material and preparation method thereof - Google Patents
Magnesium-based composite material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/227—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by organic binder assisted extrusion
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
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Abstract
The invention discloses a preparation method of a magnesium-based composite material, which comprises the following steps: carrying out plasma-assisted high-energy ball milling on the mixture of the nano-scale ceramic and the graphene to obtain a reinforcement; uniformly mixing the reinforcement and magnesium alloy powder in a volatile solvent to obtain slurry, drying, press-forming, sintering and hot extruding to obtain the magnesium-based composite material; in the step of the plasma-assisted high-energy ball milling, the ball milling time is 0.5-10 h, the voltage of plasma discharge is 15kV, and the current is 0.5-10A. The preparation method of the magnesium-based composite material can obviously improve the strength and toughness of the magnesium alloy.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a magnesium-based composite material and a preparation method thereof.
Background
The magnesium alloy has the advantages of small density, high specific strength, high specific rigidity, good thermal conductivity, good electromagnetic shielding property, easy processing and the like, and is widely applied to the fields of electronic products, aerospace, rail transit and the like. However, most magnesium alloys have close-packed hexagonal crystal structures and have fewer independent sliding systems, so that the magnesium alloys have lower room-temperature ductility and toughness and lower mechanical strength, which all limit the wide application of magnesium alloy materials.
In the prior art, the comprehensive mechanical property of the magnesium alloy material is improved by adding a reinforcement into the magnesium alloy in modes of stirring, casting, extrusion casting, powder metallurgy, mechanical alloying, pressureless infiltration, plasma sintering, friction stir welding and the like. Currently, the commonly used reinforcements mainly include ceramic materials such as silicon carbide, aluminum oxide, silicon dioxide, boron carbide and the like, and carbon materials such as graphene, carbon nanotubes and the like.
Although the mechanical properties of the magnesium alloy material can be improved to a certain extent by adding the reinforcements into the magnesium alloy in the manner described above, the strength and toughness indexes of the finally obtained reinforced magnesium-based composite material are not ideal (the yield strength is 345MPa at most, the tensile strength is 392MPa, and the elongation is 8.2%), and the actual application requirements cannot be met.
Disclosure of Invention
In view of this, the present invention provides a magnesium-based composite material and a method for preparing the same by subjecting Al to plasma-assisted conditions 2 O 3 The ceramic particles and graphene are subjected to high-energy ball milling, and then mixed and sintered with magnesium alloy, so that the prepared magnesium-based composite material has excellent mechanical properties, especially strength and toughness (yield strength is more than 365MPa, tensile strength is more than 441MPa, and elongation is more than 8.5%).
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a preparation method of a magnesium-based composite material comprises the following steps:
carrying out plasma-assisted high-energy ball milling on a mixture of nano-scale ceramic and graphene to obtain a reinforcement;
uniformly mixing the reinforcement and magnesium alloy powder in a volatile solvent to obtain slurry, drying, press-forming, sintering and hot extruding to obtain the magnesium-based composite material;
in the step of the plasma-assisted high-energy ball milling, the ball milling time is 0.5-10 h, the voltage of plasma discharge is 15kV, and the current is 0.5-10A.
The inventor finds out through intensive research that the reason for poor mechanical properties of the magnesium alloy material obtained by adding the reinforcement into the magnesium alloy is as follows: the reinforcement reacts with magnesium in the magnesium alloy, for example, the aluminum oxide ceramic reacts with magnesium to form 3Mg + Al 2 O 3 Reaction of =2Al +3MgO, and further precipitation of Mg on interface of magnesium alloy and ceramic 17 Al 12 Eutectic precipitates, which reduce the bond strength between the alumina and the magnesium alloy matrix. Then generating 2Mg + SiO with magnesium as silicon oxide ceramic 2 Reaction of Si +2MgO, further reaction of magnesium with the reaction product silicon 2Mg + Si =Mg 2 Si，Mg 2 Si precipitates reduce the interface bonding strength of silicon oxide and the magnesium alloy matrix. In the process of compounding the carbon materials such as graphene and graphene oxide with the magnesium alloy, due to lack of atomic layer bonding (no bonding between chemical bonds between the magnesium matrix and graphene/graphene oxide), the carbon materials and the magnesium alloy in the composite material are easy to break at the interface, and the strength is low.
The preparation method of the magnesium-based composite material provided by the invention comprises the steps of firstly carrying out plasma-assisted high-energy ball milling on a mixture of the nano-scale ceramic and the graphene, and limiting the voltage, the current and the ball milling time of plasma discharge, so that in the plasma discharge process, the nano-scale ceramic and the graphene can be subjected to chemical reaction to form a whole (ceramic particles are subjected to glow oxygen plasma treatment, the surface activity is increased, and can be subjected to reaction to form C-O chemical bonds when being subjected to plasma discharge treatment with the graphene/graphene oxide so as to be combined into a whole), when the obtained reinforcement is compounded with the magnesium alloy, on one hand, the reaction of the ceramic and the magnesium can be prevented, on the other hand, the defect of poor interface bonding property caused by the direct combination of the graphene and the magnesium alloy can be avoided, when the whole formed by the nano-scale ceramic and the graphene is compounded with the magnesium alloy, the interface bonding force is strong, the subsequent steps of press molding, sintering, hot extrusion and the like are combined, and the comprehensive performance, especially the strength and the toughness of the magnesium-based composite material can be obviously improved.
If non-nanoscale ceramics are adopted, even if high-energy ball milling is carried out, a large number of large-angle crystal boundaries exist in the prepared magnesium-based composite material, the mechanical property of the magnesium-based composite material is seriously influenced, and the added ceramics and graphene cannot play a role in strengthening. If the ball milling speed, time and current are too low, plasma discharge is insufficient, and the generated energy is insufficient to enable graphene/graphene oxide to react with ceramic particles; if the ball milling speed, time and current are too large, the reaction is too violent, the graphene is seriously damaged, a small block structure is formed, and the enhancement effect cannot be achieved.
Optionally, in the step of plasma-assisted high-energy ball milling, the rotation speed of ball milling is 200-800 r/min, and the diameter of the grinding ball is 1-20 mm.
Optionally, the mass ratio of the nanoscale ceramic to the graphene is 10 (0.1-1);
the mass ratio of the mixture of the nano-scale ceramic and the graphene to the grinding ball is (0.1-5): 30.
Optionally, the particle size of the nano-scale ceramic is 10-500 nm.
By limiting the mass ratio of the nanoscale ceramic to the graphene and combining the mass ratio of the mixture of the nanoscale ceramic and the graphene to the grinding balls, the reaction activity of the whole formed by the nanoscale ceramic and the graphene can be obviously reduced, and the bonding strength of the interface when the whole is compounded with the magnesium alloy powder is obviously improved. If the using amounts of the graphene and the magnesium matrix are not within the limited range, the graphene and the ceramic particles do not react completely, excessive ceramic or graphene exists, simple ceramic and the magnesium matrix react strongly to form a second phase, so that the performance of the material is reduced, and the simple graphene is easy to break the magnesium composite material at the cross section, so that the performance of the material is poor.
Optionally, in the step of plasma-assisted high-energy ball milling, inert gas such as argon is used as a medium.
Optionally, the nano-scale ceramic is nano Al 2 O 3 At least one of ceramics, nano silicon nitride ceramics and nano silicon dioxide ceramics.
Optionally, the mass ratio of the reinforcement to the magnesium alloy powder is 1 (15-20);
the mass volume ratio of the mixture of the reinforcement body and the magnesium alloy powder to the volatile solvent is 1g (1-3) mL.
By limiting the mass ratio of the reinforcement to the magnesium alloy powder and combining the mass-volume ratio of the mixture of the reinforcement and the magnesium alloy powder to the volatile solvent (ethanol, ethyl acetate, n-hexane and the like can be selected), the dosage of the volatile solvent is reduced, the reinforcement and the magnesium alloy powder can be uniformly mixed, and the compactness and the performance uniformity of the final composite material are improved.
Optionally, the drying temperature is 70-90 ℃, and the drying time is 15-30 h.
Optionally, the pressure in the step of compression molding is 400-600 MPa, the pressure maintaining time is 10-30 min,
the pressure of the sintering step is 50-150 MPa, the temperature is 200-300 ℃, and the pressure maintaining time is 0.5-1 h;
the extrusion temperature of the hot extrusion step is 200-300 ℃, the extrusion ratio (20-30) is 1, and the extrusion rate is 0.05-0.1 mm/s.
Optionally, before performing plasma-assisted high-energy ball milling on the mixture of the nanoscale ceramic and the graphene, the method further comprises a step of treating the nanoscale ceramic with oxygen plasma for 2-15 min.
The method comprises the following steps of pretreating the surface of the nano-scale ceramic: and 2-15min after oxygen plasma treatment, the dangling bonds on the surface of the ceramic are greatly increased, the chemical activity of the surface of the ceramic is improved, and the ceramic can easily react with graphene when being subjected to plasma-assisted high-energy ball milling and mixing with the graphene, so that the interface bonding strength of the reinforcement and the magnesium alloy material is further improved.
Optionally, the rf power of the oxygen plasma is 100-500W.
The invention also provides the magnesium-based composite material prepared by the preparation method of the magnesium-based composite material. The side reaction between the reinforcing phase and the magnesium matrix in the magnesium-based composite material is less, and the interface between the reinforcing phase and the magnesium matrix is firmly combined and cannot be broken at the interface.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Any type of existing magnesium alloy (the size is not limited) can meet the implementation of the technical scheme of the invention, and for convenience of comparison, the AZ91 magnesium alloy is adopted in the following examples and comparative examples;
any ceramics having a particle size in the nanometer range can be satisfactory for the implementation of the present invention, and for the sake of comparison at that time, ceramics having a particle size of 10 to 500nm are used in the following examples and comparative examples.
In the following examples and comparative examples, grinding balls having a particle size of 1 to 20mm were used.
Example 1
This example provides a magnesium-based composite material, which is prepared as follows:
pretreatment of the ceramic: mixing nano-grade Al 2 O 3 Treating ceramic particles (average particle diameter of 200 nm) with glow oxygen plasma with radio frequency power of 200W for 2min to obtain surface modified nanoscale Al 2 O 3 Ceramic particles;
preparation of the reinforcement: weighing the surface-modified nanoscale Al 2 O 3 Placing the ceramic particles and the graphene in a ball milling tank according to the mass ratio of 10.7, and performing plasma-assisted high-energy ball milling to obtain a reinforcement; the plasma-assisted high-energy ball milling is characterized in that an electrode bar and a front cover plate are respectively connected with the positive pole and the negative pole of a plasma power supply, a ball milling tank is vacuumized through a vacuum valve, and then argon is filled, so that the pressure value in the ball milling tank reaches the value of connecting the plasma power supply. Setting the voltage of a plasma power supply to be 15kV and the current to be 10A, and then starting the ball mill; the ball milling time is 0.5h, the ball milling rotating speed is 600r/min, and the nano-grade Al 2 O 3 The mass ratio of the mixture of the ceramic and the graphene to the grinding ball is 2;
mixing and compression molding: putting the reinforcement and magnesium alloy powder into a beaker according to the mass ratio of 1;
wherein the mass-volume ratio of the mixture of the reinforcement and the magnesium alloy powder to the volatile solvent absolute ethyl alcohol is 1g;
sintering and hot extrusion: and (2) putting the compact composite block blank into a vacuum hot-pressing sintering furnace for hot-pressing sintering (the sintering pressure is 150MPa, the temperature is 300 ℃, and the pressure maintaining time is 0.7 h), and then carrying out hot extrusion (the extrusion temperature is 250 ℃, the extrusion ratio is 25, and the extrusion rate is 0.05 mm/s) to obtain the magnesium-based composite material (bar material).
Example 2
This example provides a magnesium-based composite material, which is prepared as follows:
pretreatment of the ceramic: mixing nano-scale Al 2 O 3 Treating ceramic particles (average particle diameter of 10 nm) with glow oxygen plasma with radio frequency power of 100W for 10min to obtain surface modified nanoscale Al 2 O 3 Ceramic particles;
preparation of the reinforcement: weighing the surface-modified nanoscale Al 2 O 3 Placing the ceramic particles and the graphene in a ball milling tank according to the mass ratio of 10.1, and performing plasma-assisted high-energy ball milling to obtain a reinforcement; the plasma-assisted high-energy ball milling is characterized in that an electrode bar and a front cover plate are respectively connected with the positive pole and the negative pole of a plasma power supply, a ball milling tank is vacuumized through a vacuum valve, and then argon is filled, so that the pressure value in the ball milling tank reaches the value of connecting the plasma power supply. Setting the voltage of a plasma power supply to be 15kV and the current to be 0.5A, and then starting the ball mill; the ball milling time is 2 hours, the ball milling rotating speed is 800r/min, and the nano-grade Al 2 O 3 The mass ratio of the mixture of the ceramic and the graphene to the grinding ball is 0.1;
mixing and compression molding: putting the reinforcement and magnesium alloy powder into a beaker according to the mass ratio of 1;
wherein the mass-volume ratio of the mixture of the reinforcement and the magnesium alloy powder to the volatile solvent absolute ethyl alcohol is 1g;
sintering and hot extrusion: and (2) putting the compact composite block blank into a vacuum hot-pressing sintering furnace for hot-pressing sintering (the sintering pressure is 50MPa, the temperature is 200 ℃, the pressure maintaining time is 1 h), and then carrying out hot extrusion (the extrusion temperature is 200 ℃, the extrusion ratio is 20, and the extrusion rate is 0.1 mm/s) to obtain the magnesium-based composite material (bar material).
Example 3
This example provides a magnesium-based composite material, which is prepared as follows:
pretreatment of the ceramic: mixing nano-scale Al 2 O 3 Treating ceramic particles (average particle diameter of 500 nm) with glow oxygen plasma with radio frequency power of 500W for 15min to obtain surface modified nanoscale Al 2 O 3 Ceramic particles;
preparation of the reinforcement: weighing the surface-modified nanoscale Al 2 O 3 Placing the ceramic particles and the graphene in a ball milling tank according to a mass ratio of 10; the plasma-assisted high-energy ball milling is characterized in that an electrode bar and a front cover plate are respectively connected with the positive pole and the negative pole of a plasma power supply, a ball milling tank is vacuumized through a vacuum valve, and then argon is filled, so that the pressure value in the ball milling tank reaches the value of connecting the plasma power supply. Setting the voltage of a plasma power supply to be 15kV and the current to be 2A, and then starting the ball mill; the ball milling time is 10 hours, the ball milling rotating speed is 200r/min, and the nano-grade Al 2 O 3 The mass ratio of the mixture of the ceramic and the graphene to the grinding ball is 5;
mixing and compression molding: putting the reinforcement and magnesium alloy powder into a beaker according to the mass ratio of 1;
wherein the mass-volume ratio of the mixture of the reinforcement and the magnesium alloy powder to the volatile solvent absolute ethyl alcohol is 1g to 3mL;
sintering and hot extrusion: and (2) putting the compact composite block blank into a vacuum hot-pressing sintering furnace for hot-pressing sintering (the sintering pressure is 100MPa, the temperature is 250 ℃, and the pressure maintaining time is 0.5 h), and then carrying out hot extrusion (the extrusion temperature is 300 ℃, the extrusion ratio is 30, and the extrusion rate is 0.08 mm/s) to obtain the magnesium-based composite material (bar material).
Example 4
The preparation method of the mg-based composite material provided in this example is similar to that of example 1, and the difference is only that the type of the ceramic is different, and the nano-silicon nitride ceramic is used in this example.
Example 5
The preparation method of the mg-based composite material provided in this example is similar to that of example 1, except that the type of the ceramic is different, and the nano-scale silica ceramic is used in this example.
Example 6
The magnesium-based composite material provided in this example was prepared in a similar manner to example 1, except that the pretreatment step of the ceramic was omitted in this example.
Comparative example 1
The preparation method of the magnesium-based composite material provided by the comparative example is similar to that of the example 1, and the difference is that no graphene is added into the reinforcement in the comparative example, and the preparation steps of the specific reinforcement are as follows:
weighing the surface-modified nanoscale Al 2 O 3 Ceramic particles (with the average particle size of 200 nm) are placed in a ball milling tank, and are subjected to plasma-assisted high-energy ball milling to obtain a reinforcement; the plasma-assisted high-energy ball milling is characterized in that an electrode bar and a front cover plate are respectively connected with the positive pole and the negative pole of a plasma power supply, a ball milling tank is vacuumized through a vacuum valve, and then argon is filled, so that the pressure value in the ball milling tank reaches the value of connecting the plasma power supply. Setting the voltage of a plasma power supply to be 15kV and the current to be 10A, and then starting the ball mill; the ball milling time is 0.5h, the ball milling rotating speed is 600r/min, and the nano-grade Al 2 O 3 The mass ratio of the ceramic to the grinding ball is 2.
Comparative example 2
The preparation method of the magnesium-based composite material provided by the comparative example is similar to that of the example 1, and is only different in that graphene is not added into the reinforcement, and the concrete preparation steps of the reinforcement in the comparative example are as follows:
weighing the surface-modified nanoscale Al 2 O 3 Ceramic particles (with the average particle size of 200 nm) are placed in a ball milling tank, and are subjected to plasma-assisted high-energy ball milling to obtain a reinforcement; the plasma-assisted high-energy ball milling is characterized in that an electrode bar and a front cover plate are respectively connected with the positive electrode and the negative electrode of a plasma power supply, a ball milling tank is vacuumized through a vacuum valve, and then argon is filled, so that the pressure value in the ball milling tank reaches the value of connecting the plasma power supply. Setting the voltage of a plasma power supply to be 15kV and the current to be 10A, and then starting the ball mill; the ball milling time is 0.5h, the ball milling rotating speed is 120r/min, and the nano-grade Al 2 O 3 The mass ratio of the ceramic to the grinding ball is 2.
Comparative example 3
The magnesium-based composite material provided by the present comparative example was prepared in a similar manner to example 1 except that the current of the plasma discharge was different, and the current of the plasma discharge in the present comparative example was 0.3A.
Comparative example 4
The preparation method of the mg-based composite material provided in the present comparative example is similar to that of example 1, except that the ball milling time is different, and the ball milling time is 10.5h in the present comparative example.
Experimental example 1
The magnesium-based composite materials prepared in the examples and the comparative examples were subjected to mechanical property and friction resistance tests, and the specific test methods and test results are shown below.
The mechanical test method is as follows:
and preparing a standard tensile sample by referring to GBT228-2002 for the magnesium-based composite material bar, and carrying out corresponding mechanical property test.
The abrasion resistance test method is as follows:
the wear resistance test is carried out on an M2000 type wear machine, the lower roller of the wear machine is made of GCr15 steel, the hardness is HRC61, the rotating speed is 200r/min, and the pressure is 300N. The wear resistance is evaluated by a weighing method, the size of the magnesium-based composite material is 7mm multiplied by 30mm, before a wear resistance test, the magnesium-based composite material (a sample for short) is cleaned by absolute ethyl alcohol, and is dried by a blower, then the mass M1 of the sample is measured by an electronic balance (the mass is measured for 3 times in sequence and the average value is taken), the sample is cleaned by the absolute ethyl alcohol after being pre-ground for 3min, and is dried by the blower, and then the mass M2 of the sample is measured by the electronic balance again (the mass is measured for 3 times in sequence and the average value is taken); after further wearing for 15min, the above process was repeated to measure M3 (3 times in sequence, and an average value was taken), and the wear loss M = M2-M3 of the final sample.
TABLE 1 test results
| Tensile yield strength/MPa | Maximum tensile strength/MPa | Maximum elongation/% | Abrasion loss per gram | |
| Example 1 | 456 | 538 | 10.7 | 5.1×10 -4 |
| Example 2 | 435 | 521 | 10.1 | 6.6×10 -4 |
| Example 3 | 431 | 519 | 10.1 | 6.8×10 -4 |
| Example 4 | 415 | 494 | 9.6 | 8.6×10 -4 |
| Example 5 | 410 | 487 | 9.7 | 8.8×10 -4 |
| Example 6 | 365 | 441 | 8.5 | 3.5×10 -3 |
| Comparative example 1 | 277 | 325 | 5.8 | 9.8×10 -3 |
| Comparative example 2 | 321 | 376 | 7.2 | 5.8×10 -3 |
| Comparative example 3 | 327 | 385 | 7.7 | 5.7×10 -3 |
| Comparative example 4 | 311 | 364 | 6.9 | 6.4×10 -3 |
According to the data in the above table, the preparation method of the magnesium-based composite material provided by the invention has the advantages that the mixture of the nano-scale ceramic and the graphene is subjected to plasma-assisted high-energy ball milling, the voltage, the current and the ball milling time of plasma discharge are limited, so that the nano-scale ceramic and the graphene are subjected to chemical reaction to form a whole in the plasma discharge process, the interface bonding force of the whole is strong when the whole is compounded with the magnesium alloy, and the comprehensive properties, particularly the strength and the toughness of the prepared magnesium-based composite material can be remarkably improved by combining the following steps of compression molding, sintering, hot extrusion and the like, and the abrasion loss is small. If the nanometer ceramic is pretreated by glow oxygen plasma preferentially, the mechanical property of the prepared magnesium-based composite material can be further improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. The preparation method of the magnesium-based composite material is characterized by comprising the following steps:
treating the nano-scale ceramic by adopting oxygen plasma for 2-15min, and carrying out plasma-assisted high-energy ball milling on the mixture of the nano-scale ceramic and graphene to obtain a reinforcement;
uniformly mixing the reinforcement and magnesium alloy powder in a volatile solvent to obtain slurry, drying, press-forming, sintering and hot extruding to obtain the magnesium-based composite material;
in the step of plasma-assisted high-energy ball milling, the ball milling time is 0.5 to 10h, the voltage of plasma discharge is 15kV, and the current is 0.5 to 10A;
in the step of plasma-assisted high-energy ball milling, the rotating speed of ball milling is 200 to 800r/min, and the diameter of a grinding ball is 1 to 20mm;
the mass ratio of the nano-scale ceramic to the graphene is 10 (0.1 to 1);
the mass ratio of the mixture of the nano-scale ceramic and the graphene to the grinding ball is (0.1 to 5): 30;
the nano-scale ceramic is nano Al 2 O 3 At least one of ceramics, nano silicon nitride ceramics and nano silicon dioxide ceramics;
the mass ratio of the reinforcement to the magnesium alloy powder is 1 (15 to 20);
the mass-volume ratio of the mixture of the reinforcement body and the magnesium alloy powder to the volatile solvent is 1g (1~3) mL.
2. The process for producing a magnesium-based composite material as claimed in claim 1, wherein the drying temperature is from 70 to 90 ℃ and the drying time is from 15 to 30h.
3. The method for preparing the magnesium-based composite material according to claim 1, wherein the pressure in the press molding step is 400 to 600MPa, and the dwell time is 10 to 30min;
the pressure in the sintering step is 50 to 150MPa, the temperature is 200 to 300 ℃, and the pressure maintaining time is 0.5 to 1h;
the extrusion temperature in the hot extrusion step is 200-300 ℃, the extrusion ratio is (20-30): 1, and the extrusion rate is 0.05-0.1mm/s.
4. The method for preparing the magnesium-based composite material according to claim 1, wherein the radio frequency power of the oxygen plasma is 100 to 500W.
5. A magnesium-based composite material obtained by the method for preparing a magnesium-based composite material as claimed in any one of claims 1 to 4.
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| CN108754264A (en) * | 2018-07-09 | 2018-11-06 | 哈尔滨工业大学 | A kind of graphene and self-formed from reaction nano magnesia Particles dispersed enhancing magnesium-based composite material and preparation method thereof |
| CN111057923A (en) * | 2019-12-17 | 2020-04-24 | 西安理工大学 | GR/N-SiCPComposite reinforced magnesium-based composite material and preparation method thereof |
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| JP2017152691A (en) * | 2016-02-24 | 2017-08-31 | 三菱マテリアル株式会社 | Method of manufacturing magnesium-based thermoelectric conversion material, method of manufacturing magnesium-based thermoelectric conversion element, magnesium-based thermoelectric conversion material, magnesium-based thermoelectric conversion element, and thermoelectric converter |
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