CN110273092B - CoCrNi particle reinforced magnesium-based composite material and preparation method thereof - Google Patents
CoCrNi particle reinforced magnesium-based composite material and preparation method thereof Download PDFInfo
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- CN110273092B CN110273092B CN201910707743.5A CN201910707743A CN110273092B CN 110273092 B CN110273092 B CN 110273092B CN 201910707743 A CN201910707743 A CN 201910707743A CN 110273092 B CN110273092 B CN 110273092B
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Abstract
The invention discloses a CoCrNi particle reinforced magnesium matrix composite and a preparation method thereof, wherein the CoCrNi particle reinforced magnesium matrix composite comprises the following components in percentage by mass: 2-15% of CoCrNi alloy powder and the balance of Mg powder or magnesium alloy powder. The high-performance CoCrNi particle toughened magnesium-based composite material is prepared by a discharge plasma furnace sintering technology, CoCrNi particles in the composite material can be uniformly distributed on a magnesium matrix, the binding force of CoCrNi and the magnesium matrix is high, no reactant is generated with the magnesium matrix, the interface between the composite material is not polluted, and the crack expansion in the magnesium alloy can be effectively delayed. The CoCrNi particles have high plasticity, can induce the formation of nano twin crystals when stressed, and enhance the fracture toughness, strength, plasticity and strain resistance of the magnesium-based composite material. The preparation method is simple and easy to operate, the equipment is simple and convenient to operate, the raw materials are cheap and easy to obtain, the cost is low, the industrial large-scale production is easy to realize, and the method has a good application prospect.
Description
Technical Field
The invention relates to the technical field of magnesium alloy composite materials, in particular to a CoCrNi particle reinforced magnesium matrix composite material and a preparation method thereof.
Background
At present, with the rapid development of the industry in China, the magnesium alloy has higher and higher requirements on the application aspect of materials, and the magnesium alloy as a light structural material has a series of characteristics of low density, high specific strength, high specific modulus and the like. Therefore, as a novel metal matrix composite with excellent comprehensive performance, the magnesium matrix composite has great application prospect in high and new technical fields such as aerospace, communication equipment, mechanical manufacturing, automobile industry and the like. However, with the rapid development of the manufacturing industry, higher requirements are put on the properties of the mg-based composite material in various application fields. However, the preparation technology of the magnesium-based composite material still has some problems to be solved. For example, it is difficult to achieve uniform dispersion of the reinforcing phase in the magnesium-based composite material, the reinforcing phase is liable to cause an adverse interfacial reaction with the magnesium matrix, which is chemically active, to form a brittle interfacial reaction layer, and impurities are present in the matrix. These problems have resulted in magnesium-based composites that still suffer from the performance drawbacks of relatively low tensile strength, high coefficient of thermal expansion, and poor dimensional stability.
In order to solve the above problems, scientists at home and abroad also do a lot of work. For example, patent CN200510027718.0 discloses a method for preparing a titanium particle reinforced magnesium-based composite material by powder metallurgy, but the method is carried out by cold pressing and sintering, the sintering process is complicated, the production efficiency is low, the performance of the prepared material is not high, and the application range of the prepared material is limited. The invention patent CN201611013922.1 discloses a magnesium-based composite material with high-entropy alloy as a reinforcing base and a preparation method thereof, wherein the composite material is prepared by taking AlCoCrFeNi high-entropy alloy as the reinforcing base and magnesium alloy as a matrix, respectively weighing and mixing metal powder according to the proportion of the high-entropy alloy, and then smelting the metal powder and a high-purity magnesium alloy ingot in a well furnace under the argon atmosphere. However, the high-entropy alloy adopted by the method is a single-phase solid solution formed by mechanical alloying and mixing five or more components in equal atomic ratio or close to equal atomic ratio after high-energy ball milling, so the ball milling time is long, the single-phase solid solution is obtained by long-time ball milling of element powder, but the single-phase solid solution is difficult to form by ball milling of the element powder, the mechanical alloying cannot be completely carried out, and elementary substances such as Fe, Al, Cr and the like exist in a ball-milled product. The elementary substances can be aggregated together to form large-particle impurities during smelting, the mechanical property of the elementary substances is seriously influenced, the corrosion resistance of the elementary substances is reduced due to galvanic corrosion caused by the existence of Fe, the uniformity of the obtained structure components is difficult to ensure, and the industrial production is difficult to carry out.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a CoCrNi particle reinforced magnesium matrix composite, which solves the problem that the existing magnesium matrix composite is poor in plasticity and strength.
The invention also provides a preparation method of the CoCrNi particle reinforced magnesium matrix composite, and solves the problems of complex preparation method, long production process time and high cost of the existing magnesium matrix composite.
In order to solve the technical problems, the invention adopts the following technical scheme: a CoCrNi particle reinforced magnesium matrix composite material comprises the following components in percentage by mass: 2-15% of CoCrNi alloy powder and the balance of Mg powder or magnesium alloy powder. By selecting the proportion, the CoCrNi alloy can be directly subjected to mechanical ball milling, the CoCrNi is randomly distributed on an Mg matrix, the mixed powder subjected to ball milling is directly sintered in a discharge plasma furnace without cold pressing and sintering to obtain a finished product, the sintering process is simple, and the sintered product has high strength and plasticity.
Preferably, the particle size of the CoCrNi alloy powder is 75-200 μm; the particle size of the Mg powder or the magnesium alloy powder is 60-80 mu m.
The invention also provides a preparation method of the CoCrNi particle reinforced magnesium matrix composite, which comprises the following steps:
1) proportioning the components, and then ball-milling and mixing CoCrNi alloy powder and Mg powder or magnesium alloy powder for 1-4 h to prepare alloy powder;
2) and (2) preparing the powder obtained in the step 1) into an original billet by spark plasma sintering, and machining the original billet into a blank with a proper size.
The invention adopts Spark Plasma Sintering (SPS), the sintering method utilizes the action of strong pulse current to promote the solidification of the material, has the characteristics of high temperature rise speed, low sintering temperature and the like, can effectively reduce the sintering temperature of the magnesium alloy, has short heat preservation time of a sample at a high temperature stage, and can effectively reduce the reduction of the material density caused by the Kerkadall effect.
Preferably, the number of ball milling revolutions is 50-100 rpm/min, and the ball milling time is 2-4 h.
Preferably, the ball milling medium in the ball milling is argon, so that the magnesium powder is prevented from contacting with air and being oxidized in the ball milling process, and the ball milling efficiency is improved.
Preferably, the ball-to-material ratio in the ball milling is 5-10: 1, the ball-to-material ratio is the ratio of the mass of the milling balls (ball milling media) to the mass of the materials (total amount of alloy powder), if the ball-to-material ratio is too small, the ball milling strength cannot be achieved, and the impact milling effect in the ball milling process cannot be achieved; if the ball-to-material ratio is too large, impact and friction among grinding balls and between the grinding balls and a ball-milling tank are increased, useless power loss can be caused, power consumption during ball milling is increased, yield is reduced, abrasion of the ball-milling tank can be aggravated, metal consumption is increased, consumed metal is also introduced into materials as impurities, and the ball-to-material ratio is better to be 5:1 in the same ball-milling time.
Preferably, the temperature is increased to 450-550 ℃ at the heating rate of 40-60 ℃/min during spark plasma sintering, the temperature is kept for 10-30 min, and then the temperature is reduced to room temperature at 50 ℃/min. The pressure during the spark plasma sintering is 50-80 MPa, and preferably 75 MPa.
The sintering pressure and temperature have a great influence on the compactness of the sintered body structure. The particles are deformed or broken due to the over-high sintering pressure, and the requirement on equipment is higher; and the density of a pressed compact is insufficient due to too low sintering pressure, the densification of a sintered body is difficult to complete, pores exist among particles, and a sintered block is difficult to form. Therefore, the invention preferably selects a sintering pressure of 75MPa which can be satisfied by the equipment and can complete the densification of the sintered body. The too high sintering temperature or the too long heat preservation time can cause the coarse grains and reduce the mechanical property of the composite material; the internal stress caused by the sintering process cannot be fully released due to the excessively low sintering temperature or the excessively short heat preservation time; under the sintering condition of the invention, the composite material sintered block with fine crystal grains and excellent performance can be obtained. The cooling rate is 50 ℃/min in the SPS sintering process, the growth of crystal grains can be well controlled by rapid cooling, and the mechanical property of the composite material is improved.
Compared with the prior art, the invention has the following beneficial effects:
1. the magnesium-based composite material structure contains a matrix structure of fine alpha-Mg and CoCrNi particles with the size of about 100 mu m randomly distributed in the matrix structure, wherein the CoCrNi particles are composed of a solid solution CoCrNi phase, and the CoCrNi phase can induce the formation of nano twin crystals when stressed, so that the strain resistance of the magnesium-based composite material is enhanced; the CoCrNi alloy has high binding force with the magnesium matrix, no reactant is generated with the magnesium matrix, the interface between the composite materials is not polluted, the crack expansion in the magnesium alloy can be effectively delayed, and the fracture toughness, the strength and the plasticity of the composite materials are further improved.
2. The invention takes CoCrNi alloy powder and Mg powder as raw materials, the CoCrNi particles consist of a solid solution fcc phase, and a matrix consists of alpha-Mg with the diameter of about 20 mu m, the crystal grains with the two sizes present a 'bimodal' structure, and the performance of the magnesium-based composite material can be obviously improved; and through ball milling and discharge plasma sintering technology, the medium entropy alloy CoCrNi particles can be uniformly distributed on the magnesium matrix, the binding force of the medium entropy alloy CoCrNi particles and the magnesium matrix is high, the CoCrNi alloy has higher plasticity, and the crack expansion in the magnesium alloy can be effectively delayed, so that the fracture toughness, strength and plasticity of the composite material are improved, therefore, compared with the common magnesium-based composite material, the magnesium-based composite material prepared by the invention has higher bending strength, compressive strength, hardness and interface strength, wherein the compressive strength can reach 369MPa, and therefore, the magnesium-based composite material is expected to have huge application prospects in high and new technical fields such as aerospace, communication equipment, mechanical manufacturing and automobile industry.
3. The invention directly mixes the CoCrNi alloy powder and the Mg powder, does not introduce other impurities due to preparation of the reinforced phase, and has single reinforced phase component and no other defects. And then sintering by a discharge plasma furnace to distribute the CoCrNi on the Mg matrix. The preparation method is simple and easy to operate, the preparation process flow is simple, the production period is short, the equipment operation is simple and convenient, compared with the high-entropy alloy, the raw materials are cheap and easy to obtain, the production cost is greatly reduced, the industrial large-scale production is facilitated, the problems of high cost and long production process time of the cold pressing sintering method are solved, and the method has good application prospect and economic benefit.
Drawings
Fig. 1 is a microstructure view of a magnesium-based composite material prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples.
CoCrNi particle reinforced magnesium-based composite material and preparation method thereof
Example 1
1) Weighing 2.0g of CoCrNi powder with the medium entropy alloy size of 100 mu m and 98.0g of AZ91 alloy powder with the size of 50 mu m;
2) putting the raw materials weighed in the step 1) into a ball mill, adding 500g of stainless steel balls, vacuumizing and filling argon, repeating for two or three times, and then performing ball milling at the rotating speed of 50r/min for 2 hours, and uniformly mixing the powder to obtain mixed powder;
3) sintering the mixed powder obtained in the step 2) in SPS equipment, heating to 500 ℃ at a heating rate of 50 ℃/min, preserving heat for 10min, cooling to room temperature at 50 ℃/min to finally obtain the magnesium-based composite material, and preparing the composite material into a sample to obtain a prefabricated sample.
The magnesium-based composite material obtained in this example was observed under a scanning electron microscope, and the results are shown in fig. 1.
As can be seen from the figure, the sintered structure mainly takes a black alpha-Mg phase as a matrix, the gray color distributed on the matrix is a solid solution CoCrNi phase with the size of about 100 mu m, and AZ91 is tightly combined with the CoCrNi phase interface without obvious interface defects.
Example 2
1) Weighing 5.0g of CoCrNi powder with the medium entropy alloy size of 200 mu m and 95.0g of AZ91 alloy powder with the medium entropy alloy size of 60 mu m;
2) putting the raw materials weighed in the step 1) into a ball mill, adding 500g of stainless steel balls, vacuumizing and filling argon, repeating for two or three times, and then performing ball milling at the rotating speed of 50r/min for 2 hours, and uniformly mixing the powder to obtain mixed powder;
3) sintering the mixed powder obtained in the step 2) in SPS equipment, heating to 500 ℃ at a heating rate of 50 ℃/min, preserving heat at 75MPa for 10min, cooling to room temperature at 50 ℃/min to finally obtain the magnesium-based composite material, and preparing the composite material into a sample to obtain a prefabricated sample.
Example 3
1) Weighing 10.0g of CoCrNi powder with the medium entropy alloy size of 120 mu m and 90.0g of AZ91 alloy powder with the medium entropy alloy size of 70 mu m;
2) putting the raw materials weighed in the step 1) into a ball mill, adding 500g of stainless steel balls, vacuumizing and filling argon, repeating for two or three times, and then performing ball milling at the rotating speed of 50r/min for 2 hours, and uniformly mixing the powder to obtain mixed powder;
3) sintering the mixed powder obtained in the step 2) in SPS equipment, heating to 500 ℃ at a heating rate of 50 ℃/min, preserving heat at 75MPa for 10min, cooling to room temperature at 50 ℃/min to finally obtain the magnesium-based composite material, and preparing the composite material into a sample to obtain a prefabricated sample.
Example 4
1) Weighing 15.0g of CoCrNi powder with the medium entropy alloy size of 100 mu m and 85.0g of AZ91 alloy powder with the medium entropy alloy size of 50 mu m;
2) putting the raw materials weighed in the step 1) into a ball mill, adding 500g of stainless steel balls, vacuumizing and filling argon, repeating for two or three times, and then performing ball milling at the rotating speed of 50r/min for 2 hours, and uniformly mixing the powder to obtain mixed powder;
3) sintering the mixed powder obtained in the step 2) in SPS equipment, heating to 500 ℃ at a heating rate of 50 ℃/min, preserving heat at 75MPa for 10min, cooling to room temperature at 50 ℃/min to finally obtain the magnesium-based composite material, and preparing the composite material into a sample to obtain a prefabricated sample.
Secondly, product detection
1. The results of texture characterization of the magnesium-based composite material preforms prepared in examples 1 to 4 are shown in table 1.
TABLE 1
As can be seen from Table 1, the magnesium-based composite material prepared by the method has good compressive strength and elongation, wherein the compressive strength can reach 369MPa, and the elongation can reach 5.2%, so that the stability and the wear resistance of the magnesium-based composite material are improved.
The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The CoCrNi particle reinforced magnesium matrix composite is characterized by comprising the following components in percentage by mass: 2-15% of CoCrNi alloy powder and the balance of Mg powder or magnesium alloy powder; the particle size of the CoCrNi alloy powder is 75-200 mu m, the particle size of the Mg powder or the magnesium alloy powder is 60-80 mu m, and the CoCrNi alloy powder is an alpha-Mg matrix structure; the CoCrNi alloy powder consists of a solid solution fcc phase and is uniformly distributed in a matrix structure.
2. The method for preparing a CoCrNi particle reinforced Mg-based composite material as claimed in claim 1, comprising the steps of:
1) mixing the components according to claim 1, and then ball milling and mixing CoCrNi alloy powder and magnesium alloy powder or Mg powder for 1-4 hours to prepare alloy powder;
2) performing spark plasma sintering on the alloy powder obtained in the step 1) to prepare an original billet, and machining the original billet into a blank with a proper size.
3. The method for preparing the CoCrNi particle reinforced magnesium matrix composite material as claimed in claim 2, wherein the ball milling rotation speed is 50-100 rpm, and the ball milling time is 2-4 h.
4. The preparation method of the CoCrNi particle reinforced magnesium matrix composite material as claimed in claim 2, wherein the ball milling medium in the ball milling is argon gas, and the ball material ratio is 5-10: 1.
5. The method for preparing the CoCrNi particle reinforced magnesium matrix composite material as claimed in claim 2, wherein the temperature is raised to 450-550 ℃ at a temperature raising rate of 40-60 ℃/min during spark plasma sintering, the temperature is maintained for 10-30 min, and then the temperature is lowered to room temperature at a rate of 50 ℃/min.
6. The method for preparing CoCrNi particle reinforced Mg-based composite material according to claim 2, wherein the pressure during spark plasma sintering is 50-80 MPa.
7. The method for preparing CoCrNi particle reinforced Mg-based composite material according to claim 6, wherein the pressure during spark plasma sintering is 75 MPa.
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| CN112207279A (en) * | 2020-10-23 | 2021-01-12 | 昆明理工大学 | Preparation method of bicontinuous magnesium-based composite material |
| CN113957294A (en) * | 2021-09-13 | 2022-01-21 | 暨南大学 | CrCoNi intermediate entropy alloy reinforced Al-based composite material and preparation method thereof |
| CN114164364B (en) * | 2021-10-22 | 2022-05-27 | 河海大学 | Magnesium-based composite material toughened and die-added by entropy alloy particles and preparation method thereof |
| CN115287513B (en) * | 2022-08-06 | 2023-12-08 | 陕西天梵镁汇科技有限公司 | Red copper particle reinforced magnesium-based composite material and preparation method thereof |
| CN115807176B (en) * | 2022-12-29 | 2023-08-11 | 中北大学 | Preparation method of magnesium alloy combining spark plasma sintering and free fluid rapid cooling |
| CN116445785A (en) * | 2023-04-20 | 2023-07-18 | 上海交通大学 | Multi-principal element alloy particle reinforced magnesium-based composite material and preparation method thereof |
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