CN111705252A - Al (aluminum)2O3Nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material and preparation method thereof - Google Patents

Al (aluminum)2O3Nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material and preparation method thereof Download PDF

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CN111705252A
CN111705252A CN202010562209.2A CN202010562209A CN111705252A CN 111705252 A CN111705252 A CN 111705252A CN 202010562209 A CN202010562209 A CN 202010562209A CN 111705252 A CN111705252 A CN 111705252A
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composite material
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crconi
entropy alloy
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罗贤
赵爱武
杨延清
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Northwestern Polytechnical University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/001Non-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
    • C22C32/0015Non-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
    • C22C32/0026Matrix based on Ni, Co, Cr or alloys thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1051Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Abstract

The invention relates to Al2O3A nano-particle reinforced CrCoNi intermediate entropy alloy based composite material comprises 2.5-7.5 wt% of Al2O3Nano powder and the balance of Cr, Co and Ni; the Cr, Co and Ni are in equal atomic ratio. The composite material is prepared by adopting mechanical alloying and spark plasma sintering processes, the preparation process is reasonable and simple, the repeatability of the preparation process is strong, and industrial batch production can be realized. Al can be obtained by the present invention2O3Uniform distribution of nanoparticles, matrix and Al2O3CrCoNi-Al with good grain interface combination, fine matrix grain size and density of more than 97 percent2O3A nanocomposite material. CrCoNi-Al of the invention2O3The nano composite material has excellent compressive yield strength and better plasticity. Containing 2.5-7.5 wt% Al2O3The compressive yield strength of the composite material is 1877-2359MPa, the fracture strain is 9.3-31.6%, and the yield strength of the composite material is improved by 65.4-107.8% compared with that of a pure CrCoNi matrix.

Description

Al (aluminum)2O3Nanoparticle reinforced CrCoNi entropy alloy-based composite material and preparation method thereof
Technical Field
The invention belongs to the field of metal matrix composite materials, and relates to Al2O3A nanoparticle reinforced CrCoNi intermediate entropy alloy based composite material and a preparation method thereof.
Background
According to different entropies, the alloy is divided into high-entropy, medium-entropy and low-entropy alloys, wherein the component design of the high-entropy and medium-entropy alloys breaks through the concept of the traditional alloy and is a single solid solution formed by multiple main elements. Due to its unique composition and structure, medium-entropy, high-entropy alloys exhibit four core effects: high entropy effects, lattice distortion effects, delayed diffusion effects, and "cocktail" effects. The effects endow the medium/high entropy alloy with a plurality of excellent mechanical properties, such as high toughness and plasticity, corrosion resistance, radiation resistance, excellent high/low temperature performance and the like, and have great application prospects in important fields of aerospace, nuclear industry, national defense and military affairs and the like. However, high entropy, medium entropy alloys still suffer from a number of problems, such as higher density (about 8 g/cm)3Above), expensive price, not yet high enough strength as a structural material, etc., thus limiting its wide use. In order to solve the problems, the second-phase ceramic nanoparticles with high hardness, low density and low price are commonly used for improving the strength of the high-entropy and medium-entropy alloy and reducing the density and the cost, namely, the high-entropy and medium-entropy alloy composite material is formed.
In recent years, the preparation technology of the high-entropy alloy-based composite material is rapidly developed. For example, in patent CN 105734324A "preparation of powder metallurgy high-entropy alloy-based composite material", a micron TiB prepared by gas atomization method and spark plasma sintering process is introduced2A technique for enhancing high entropy alloys. But micron-sized TiB2The particles are distributed in the matrix grain boundary, and stress concentration is firstly generated at the grain boundary in the stress process, so that the composite material is easy to lose efficacy, and the plasticity of the high-entropy alloy is greatly reduced. Also, for example, in CN 110257684A "preparation method of FeCrCoMnNi high entropy alloy based composite Material" mechanical alloying and spark plasma sintering are adoptedPreparing TiC nano-particle reinforced FeCrCoMnNi high-entropy alloy. However, the composite material has limited strength improvement (compressive yield strength is increased from 169.3MPa to 563.6MPa), and the plasticity is not high (the breaking strain is about 10%). Research has shown that, compared with high-entropy alloy with four-principal element or five-principal element FCC structure, the entropy alloy in three-principal element CrCoNi has relatively less reports about the composite material of the entropy alloy in CrCoNi, and the dense CrCoNi-Y prepared by mechanical alloying, spark plasma sintering and heat treatment process is introduced in CN 108421985A2O3Composite materials, but Y is not specifically reported2O3Influence on the properties of the composite, and Y2O3Is also relatively high (5.01 g/cm)3) (ii) a And Al2O3The nano-ceramic particles have a low density (3.9 g/cm)3) High hardness, low price and the like, and has excellent chemical stability, and the Al does not react with the matrix generally, but at present2O3Reinforced CrCoNi mid-entropy alloy-based composite material is reported.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides Al2O3The nanoparticle reinforced CrCoNi intermediate entropy alloy-based composite material and the preparation method thereof aim at the problems of high density, high cost, low strength and the like of high entropy and intermediate entropy alloys and the defects of the preparation process of the current intermediate/high entropy alloy composite material.
Technical scheme
Al (aluminum)2O3The nano particle reinforced CrCoNi intermediate entropy alloy base composite material is characterized in that the component is 2.5-7.5 wt% of Al2O3Nano powder and the balance of Cr, Co and Ni; the Cr, Co and Ni are in equal atomic ratio.
The Cr, Co and Ni adopt powder.
The purity of the Cr, Co and Ni is more than or equal to 99.5 wt%.
The grain sizes of the Cr, Co and Ni are less than or equal to 48 mu m.
The Al is2O3The purity of the nano powder is more than or equal to 99.8 wt%.
The Al is2O3The particle size of the nano powder is 30-50 nm.
The Al is2O3The nanopowder is α -Al2O3And (4) nano powder.
One kind of Al2O3The preparation method of the nanoparticle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized by comprising the following steps:
step 1, mechanical alloying: al is put in an operation box protected by high-purity argon2O3Respectively and sequentially adding the nano powder and Cr, Co and Ni powder into a stainless steel tank, adding a stainless steel ball and 2.5 wt% of alcohol of the powder mass as a process control agent, then installing the sealed stainless steel ball milling tank on an omnibearing planetary ball mill, and carrying out ball milling at room temperature to prepare uniformly mixed composite material powder;
step 2, die filling and cold pressing: stacking graphite paper on the inner wall of a graphite mold, then loading composite powder into the graphite mold in an operation box protected by high-purity argon, stacking the graphite paper on the upper end and the lower end, then mounting a graphite pressure head, and carrying out cold pressing compaction at the pressure of 15-20 MPa;
and 3, spark plasma sintering: sleeving a graphite felt on a graphite mould filled with composite powder, and sintering and forming by using spark plasma sintering equipment; the sintering process comprises the steps of preserving heat and pressure for 5-20 min under the protection of vacuum or high-purity argon and at 950-1100 ℃/20-40 MPa to finish sintering, then cooling the furnace to room temperature, taking out the mold, and demolding to obtain the CrCoNi-Al2O3A nanocomposite material.
The ball-material ratio of the added stainless steel balls is 10: 1.
The ball milling in the step 1 is performed at room temperature at a speed of 200-400 rpm for 10-50 h.
Advantageous effects
The invention provides Al2O3Nano-particle reinforced CrCoNi intermediate entropy alloy base composite materialThe material and the preparation method adopt low-density, high-hardness and low-price Al2O3The nano-particle reinforced CrCoNi intermediate entropy alloy provides a method for preparing a high-performance intermediate entropy alloy composite material, provides technical guidance for developing a low-density and high-strength high-entropy and intermediate entropy alloy composite material, and promotes engineering application in the field of high-entropy and intermediate entropy alloys.
Compared with the prior art, the invention has the following advantages:
(1) the invention adopts mechanical alloying and spark plasma sintering process to prepare the composite material, the preparation process is reasonable and simple, the repeatability of the preparation process is strong, and the industrialized mass production can be realized.
(2) Al can be obtained by the present invention2O3Uniform distribution of nanoparticles, matrix and Al2O3CrCoNi-Al with good grain interface combination, fine matrix grain size and density of more than 97 percent2O3A nanocomposite material.
(3) CrCoNi-Al of the invention2O3The nano composite material has excellent compressive yield strength and better plasticity. Containing 2.5-7.5 wt% Al2O3The compressive yield strength of the composite material is 1877-2359MPa, the fracture strain is 9.3-31.6%, and the yield strength of the composite material is improved by 65.4-107.8% compared with that of a pure CrCoNi matrix.
(4) CrCoNi-Al in contrast to the pure matrix CrCoNi2O3The density of the nano composite material can be reduced by 2.6-7.5%, and Al2O3The price of the alloy is lower than that of Cr, Co and Ni.
Drawings
FIG. 1 is CrCoNi-Al2O3XRD analysis of the nanocomposite.
FIGS. 2(a) and (b) are graphs containing 0.0 wt% and 2.5 wt% Al, respectively2O3EBSD-IPF map of the composite.
FIG. 3(a) shows a composition containing 2.5 wt% of Al2O3TEM bright field image of the composite material, FIG. 3(b) is CrCoNi/Al2O3HRTEM of the interface.
FIG. 4 shows a graph containing 2.5 wt% Al2O3Scanning Transmission (STEM) photographs of the composite material and the corresponding energy spectrum analysis results of the distribution of each element surface.
FIG. 5 is CrCoNi-Al2O3The nanocomposite material was analyzed for properties, wherein (a) is density, (b) is vickers hardness, and (c) is a compressive engineering stress-strain curve.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
preparation of CrCoNi-Al in the inventive example2O3The technological process of the nano composite material mainly comprises the steps of mechanical alloying of element powder, die filling and cold pressing, spark plasma sintering and the like. The specific process comprises the following steps:
(1) starting powder material
Purity of original powder Cr, Co and Ni is more than or equal to 99.5 wt%, particle size is less than or equal to 48 mu m, α -Al2O3The purity of the nano powder is more than or equal to 99.8 wt%, and the particle size is 30-50 nm.
(2) Mechanical alloying
Firstly, Al with the component of 2.5-7.5 wt% is put in an operation box protected by high-purity argon2O3Respectively adding the nano powder and Cr, Co and Ni powder with equal atomic ratio into a stainless steel tank in sequence, and adding Al2O3The nano particles are directly added into the mixed powder of Cr, Co and Ni to make hard Al2O3Embedding the particles into a metal matrix with good plasticity in a ball milling process so as to enable the particles to be uniformly distributed in the matrix, adding stainless steel balls (ball-to-material ratio is 10:1) and alcohol with the mass of 2.5 wt% of powder as a process control agent (preventing cold welding on a tank body and the stainless steel balls), finally installing a sealed stainless steel ball milling tank on an all-directional planetary ball mill, and carrying out ball milling at the room temperature at the speed of 200-400 rpm for 10-50 h to prepare the uniformly mixed composite material powder.
(3) Die filling and cold pressing
Firstly, stacking graphite paper with the thickness of 2mm on the inner wall of a graphite mould, then loading the composite powder into the graphite mould in an operation box protected by high-purity argon, stacking the graphite paper on the upper end and the lower end, then loading a graphite pressure head, and finally carrying out cold pressing compaction by using the pressure of 15-20 MPa.
(4) Spark plasma sintering
And (3) sleeving a graphite felt on the graphite mould filled with the composite powder, and sintering and forming by using spark plasma sintering equipment. The sintering process is that under the protection of vacuum or high-purity argon, the sintering is completed under the conditions of 900-1100 ℃/20-40 MPa of heat preservation and pressure maintaining for 5-20 min, and then the mold is taken out after the furnace is cooled to the room temperature.
(5) Demoulding
Demoulding after sintering to obtain corresponding CrCoNi-Al2O3A nanocomposite material.
Example 1
(1) Weighing Cr, Co and Ni powder with equal atomic ratio and α -Al with 2.5 wt% in an operation box protected by high-purity argon2O3Nano powder, wherein the purity of Cr, Co and Ni powder is more than or equal to 99.5 wt%, the particle size is less than or equal to 48 mu m, and Al2O3The purity of the powder is more than or equal to 99.8 wt%, and the particle size is 30-50 nm. Then sequentially adding the powder, stainless steel balls (ball-to-material ratio is 10:1) and alcohol with the mass of 2.5 wt% of the powder into a stainless steel ball milling tank, finally installing the sealed stainless steel tank on an omnibearing planetary ball mill, and carrying out ball milling for 50h at the speed of 200rpm at room temperature to prepare the uniformly mixed and prealloyed CrCoNi-2.5 wt% Al2O3And (3) compounding the powder.
(2) Stacking graphite paper with the thickness of 2mm on the inner wall of a graphite mould with the inner diameter of phi 30mm, then loading the composite powder into the graphite mould in an operation box protected by high-purity argon, stacking the graphite paper on the upper end and the lower end, then loading a graphite pressure head, and finally cold pressing by using the pressure of 15-20 MPa.
(3) The graphite mould filled with the composite powder is sleeved with graphite felt, then the graphite mould is put into LABOX-330 type spark plasma sintering equipment and vacuumized, then the sintering is finished after heat preservation is carried out for 10min at the temperature of 1000 ℃ and under the pressure of 30MPa, finally the mould is taken out after the furnace is cooled to the room temperature, and the block composite material with the size of about phi 30mm multiplied by 7mm can be obtained after demoulding.
(4) CrCoNi-2.5 wt% Al obtained by mechanical alloying and spark plasma sintering process2O3The composite material is mainly formed by FCCPhase and small amount of α -Al2O3Composition, as shown in figure 1. From FIG. 2, 0.0 wt% and 2.5 wt% of Al can be found2O3The grain sizes of the matrix of the composite material with the contents of 1.55 +/-0.95 mu m and 0.37 +/-0.21 mu m are respectively reduced by 76.1 percent compared with the pure matrix, which shows that the added Al2O3The nano particles can effectively refine the matrix grains. From FIGS. 3 and 4, Al is shown2O3Nano particles are dispersed and distributed, chemical components are uniformly distributed, Al2O3Has good metallurgical bonding with the matrix.
(5) CrCoNi-2.5 wt% Al prepared by this process2O3The composite material has excellent comprehensive properties: the density was 97.5%, the hardness was 520.7 + -15.0 HV, the compressive yield strength was 1877MPa, the compressive fracture strength was 2723MPa, and the fracture strain was 31.6%, as shown in FIG. 5. Visible Al2O3The mechanical property of the entropy alloy in the CrCoNi is obviously improved by adding the nano particles.
Example 2
(1) Weighing Cr, Co and Ni powder with equal atomic ratio and α -Al with 5.0 wt% in an operation box protected by high-purity argon2O3Nano powder, wherein the purity of Cr, Co and Ni powder is more than or equal to 99.5 wt%, the particle size is less than or equal to 48 mu m, and Al2O3The purity of the powder is more than or equal to 99.8 wt%, and the particle size is 30-50 nm. Then sequentially adding the powder, stainless steel balls (ball-to-material ratio is 10:1) and alcohol with the mass of 2.5 wt% of the powder into a stainless steel ball milling tank, finally installing the sealed stainless steel tank on an omnibearing planetary ball mill, and carrying out ball milling at the speed of 400rpm for 10 hours at room temperature to prepare the uniformly mixed and prealloyed CrCoNi-5.0 wt% Al2O3And (3) compounding the powder.
(2) Graphite paper with the thickness of 2mm is padded on the inner wall of a graphite mould with the inner diameter of phi 30mm, then powder is filled into the graphite mould in an operation box protected by high-purity argon, the graphite paper is padded on the upper end and the lower end, a graphite pressure head is installed, and finally cold pressing is carried out by using the pressure of 15-20 MPa.
(3) Sleeving a graphite felt on a graphite mould filled with powder, then putting the graphite mould into LABOX-330 discharge plasma sintering equipment, vacuumizing, preserving the heat for 10min at the temperature of 950 ℃ and under the pressure of 30MPa, then completing sintering, finally cooling the furnace to room temperature, taking out the mould, and demoulding to obtain the block composite material with the size of phi 30mm multiplied by 7.5 mm.
(4) CrCoNi-5.0 wt% Al obtained by mechanical alloying and spark plasma sintering process2O3The composite material mainly comprises FCC and a small amount of α -Al2O3Composition, as shown in figure 1. The density of the composite material is 97.4%, the hardness is 585.0 +/-13.6 HV, the compressive yield strength is 2359MPa, the compressive fracture strength is 2788MPa, and the fracture strain is 16.2%, as shown in figure 5. The yield strength of the composite material is increased by 107.8% compared to the pure matrix and still has considerable plasticity.
Example 3
(1) Weighing Cr, Co and Ni powder with equal atomic ratio and 7.5 wt% α -Al in an operation box protected by high-purity argon2O3Nano powder, wherein the purity of Cr, Co and Ni powder is more than or equal to 99.5 wt%, the particle size is less than or equal to 48 mu m, and Al2O3The purity of the powder is more than or equal to 99.8 wt%, and the particle size is 30-50 nm. Then sequentially adding the powder, stainless steel balls (ball-to-material ratio is 10:1) and alcohol with the mass of 2.5 wt% of the powder into a stainless steel ball milling tank, finally installing the sealed stainless steel tank on an all-directional planetary ball mill, and carrying out ball milling at the speed of 300rpm for 40h at room temperature to prepare the uniformly mixed and prealloyed CrCoNi-7.5 wt% Al2O3And (3) compounding the powder.
(2) Stacking graphite paper with the thickness of 2mm on the inner wall of a graphite mould with the inner diameter of phi 30mm, then loading the composite powder into the graphite mould in an operation box protected by high-purity argon, stacking the graphite paper on the upper end and the lower end, then loading a graphite pressure head, and finally cold pressing by using the pressure of 15-20 MPa.
(3) And (3) sleeving a graphite felt on a graphite mould filled with composite powder, putting the graphite mould into LABOX-330 discharge plasma sintering equipment, vacuumizing, preserving the heat at 1100 ℃ and under the pressure of 30MPa for 10min, completing sintering, finally cooling the furnace to room temperature, taking out the mould, and demoulding to obtain the composite block material with the size of phi 30mm multiplied by 8 mm.
(4) CrCoNi-7.5 wt% Al obtained by mechanical alloying and spark plasma sintering process2O3The composite material mainly comprises FCC and a small amount of α -Al2O3Composition, as shown in figure 1. The density of the composite material is 97.2%, the hardness is 602.6 +/-14.2 HV, the compressive yield strength is 1926MPa, the compressive fracture strength is 2103MPa, and the fracture strain is 9.3%, as shown in figure 5. It can be seen that along with Al2O3The content increases and the yield strength of the composite increases and then decreases, since too much reinforcing phase tends to cause agglomeration of nanoparticles and provides more crack sources, thereby leading to premature failure fracture of the material. It can be seen that the reinforcing phase Al2O3The content of (D) should be less than 7.5 wt%.

Claims (10)

1. Al (aluminum)2O3The nano particle reinforced CrCoNi intermediate entropy alloy base composite material is characterized in that the component is 2.5-7.5 wt% of Al2O3Nano powder and the balance of Cr, Co and Ni; the Cr, Co and Ni are in equal atomic ratio.
2. Al according to claim 12O3The nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized in that: the Cr, Co and Ni adopt powder.
3. Al according to claim 1 or 22O3The nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized in that: the purity of the Cr, Co and Ni is more than or equal to 99.5 wt%.
4. Al according to claim 1, 2 or 32O3The nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized in that: the grain sizes of the Cr, Co and Ni are less than or equal to 48 mu m.
5. Al according to claim 12O3The nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized in that: the Al is2O3The purity of the nano powder is more than or equal to 99.8 wt%.
6. According to the rightAl according to claim 1 or 52O3The nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized in that: the Al is2O3The particle size of the nano powder is 30-50 nm.
7. Al according to claim 1 or 5 or 62O3The nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized in that: the Al is2O3The nanopowder is α -Al2O3And (4) nano powder.
8. Al according to any one of claims 1 to 72O3The preparation method of the nanoparticle reinforced CrCoNi intermediate entropy alloy-based composite material is characterized by comprising the following steps:
step 1, mechanical alloying: al is put in an operation box protected by high-purity argon2O3Respectively and sequentially adding the nano powder and Cr, Co and Ni powder into a stainless steel tank, adding a stainless steel ball and 2.5 wt% of alcohol of the powder mass as a process control agent, then installing the sealed stainless steel ball milling tank on an omnibearing planetary ball mill, and carrying out ball milling at room temperature to prepare uniformly mixed composite material powder;
step 2, die filling and cold pressing: stacking graphite paper on the inner wall of a graphite mold, then loading composite powder into the graphite mold in an operation box protected by high-purity argon, stacking the graphite paper on the upper end and the lower end, then mounting a graphite pressure head, and carrying out cold pressing compaction at the pressure of 15-20 MPa;
and 3, spark plasma sintering: sleeving a graphite felt on a graphite mould filled with composite powder, and sintering and forming by using spark plasma sintering equipment; the sintering process comprises the steps of preserving heat and pressure for 5-20 min under the protection of vacuum or high-purity argon and at 950-1100 ℃/20-40 MPa to finish sintering, then cooling the furnace to room temperature, taking out the mold, and demolding to obtain the CrCoNi-Al2O3A nanocomposite material.
9. The method of claim 8, wherein: the ball-material ratio of the added stainless steel balls is 10: 1.
10. The method of claim 8, wherein: the ball milling in the step 1 is performed at room temperature at a speed of 200-400 rpm for 10-50 h.
CN202010562209.2A 2020-06-18 2020-06-18 Al (aluminum)2O3Nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material and preparation method thereof Pending CN111705252A (en)

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CN113403517A (en) * 2021-05-21 2021-09-17 西北工业大学 Heterostructure CrCoNi-Al2O3Nano composite material and preparation method thereof
CN114653944A (en) * 2022-04-27 2022-06-24 镇江力航新材料科技有限公司 Preparation method of NiCoCr medium-entropy alloy particle reinforced titanium-based composite material
CN114807725A (en) * 2022-05-31 2022-07-29 中国矿业大学 High-entropy alloy-based nano superhard composite material enhanced by inlaid particles and preparation method thereof

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CN112626406A (en) * 2020-12-15 2021-04-09 江西省科学院应用物理研究所 Grain-refined chromium-cobalt-nickel multi-principal-element alloy and preparation process thereof
CN113403517A (en) * 2021-05-21 2021-09-17 西北工业大学 Heterostructure CrCoNi-Al2O3Nano composite material and preparation method thereof
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