CN105648297B - A kind of additional nano ceramics mutually enhances toughening high-entropy alloy composite material and preparation method thereof - Google Patents

A kind of additional nano ceramics mutually enhances toughening high-entropy alloy composite material and preparation method thereof Download PDF

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CN105648297B
CN105648297B CN201610030517.4A CN201610030517A CN105648297B CN 105648297 B CN105648297 B CN 105648297B CN 201610030517 A CN201610030517 A CN 201610030517A CN 105648297 B CN105648297 B CN 105648297B
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entropy alloy
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CN105648297A (en
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杨少锋
张炎
韦维
杨堃
刘明
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Nanjing Institute of Technology
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    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C19/00—Alloys based on nickel or cobalt
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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
    • 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
    • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
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    • C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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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
    • C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • C22C32/0063—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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Abstract

The invention discloses a kind of additional nano ceramics mutually to enhance toughening high-entropy alloy composite material and preparation method thereof, using high-entropy alloy particle as matrix phase, additional nano ceramics simultaneously, make additional nano ceramics phase segregation in solid solution grain boundaries, ceramic phase enhancing is generated, while the face-centered cubic solid solution of toughness is caused to squeeze, forms deformation twin, to realize that the strong modeling of high-entropy alloy composite material combines, the high-entropy alloy composite material of high-strength and high ductility is prepared.The high-entropy alloy composite material of the tough no machining allowance of height, the composite material have significant high-intensitive, high rigidity and excellent compressive strength and plasticity.

Description

A kind of additional nano ceramics mutually enhances toughening high-entropy alloy composite material and preparation method thereof
Technical field
The invention belongs to metal-base composites technical fields, and in particular to a kind of preparation side of high-entropy alloy composite material Method.
Background technique
Block high-entropy alloy (HEA) has high intensity, high rigidity, low elasticity modulus and big elastic strain limit etc. one Series is different from the excellent mechanical performance of traditional crystal alloy, so that it is considered as the structural material of great potential.However, high Brittleness makes HEA material in the case where not obvious room temperature macroscopic view plastic deformation, and calamity occurs in a manner of catastrophic failure Fracture；High brittleness, high rigidity bring extreme difficulties to the processing of material.These all seriously restrict HEA as advanced knot Large-scale application of the structure material in engineering.Therefore, brittleness at room temperature, processing difficulties problem have been developed as HEA material application Important bottleneck.
The problem of brittleness at room temperature and processing difficulties to improve HEA material, researchers are by adding different metal members Element prepares the block materials of dendritic segregation using arc cast, among these with obvious, the compression plastic strain that adds Cu effect Reach within 8%.Then, Zhang Yong et al. prepares the high entropy alloy material with columanar structure by directional solidification technique, Compressive ductility increases；Wang Yanping etc. is prepared for interior raw 10vol.%TiC particle enhancing using arc cast CrFeCoNiCuAl high-entropy alloy-base composite material (HEAMCs), TiC is evenly distributed on matrix at graininess, and size is about Several microns.The compressive strength and hardness of CrFeCoNiCuTi-TiC composite material can respectively reach 2040MPa and 746HV, Compression plasticity about 12%.But the acquisition of the plasticity of above-mentioned high entropy alloy material, be not considerably reduce intensity be exactly improve mould Property aspect be not obvious.
Summary of the invention
The purpose of the present invention is to provide a kind of high-entropy alloy composite material, the same of its excellent in strength and hardness is being kept When, improve the plasticity of composite material.
High-entropy alloy composite material of the invention, using high-entropy alloy particle as matrix phase, while additional nano ceramics, make Additional nano ceramics phase segregation generates ceramic phase enhancing in solid solution grain boundaries, while making to the face-centered cubic solid solution of toughness At extruding, deformation twin is formed, to realize that the strong modeling of high-entropy alloy composite material combines, the high entropy for preparing high-strength and high ductility is closed Metal/composite material.
The additional nano ceramics mutually enhances the preparation method of toughening high-entropy alloy composite material, specifically includes following preparation Step:
1. being matched according to the predetermined ingredient of composite material, high-purity alloy powder and nano-ceramic powder appropriate are chosen Body.The alloy powder atomic formula are as follows: AlxFeCrCoyNi(Cu)mTiz, wherein 0≤x≤0.7,0≤z≤0.7, x+z= 0.7,1≤y≤1.5, m are 0 or 1.
The purity of Al, Fe, Cr, Co, Ni, Cu, Ti metal powder > 99.9 %, granularity≤45 μm.
The nano-ceramic powder is Al2O3, TiC, SiC, purity > 99.9%, granularity≤100nm.With the body of alloy powder Product is 100% meter, and the volume of nano-ceramic powder is 1 ~ 20%.
2. alloy powder and nano-ceramic powder are mixed using high energy ball mill under argon atmosphere and machinery closes Aurification, dry grind 400 ~ 500r/min of revolving speed, and the dry grinding time is 40 ~ 50h, and 2 ~ 5h of wet-milling time, wet-milling revolving speed is 100 ~ 300r/ min；After wet-milling, vacuum tank is opened, after being dried in vacuo 24 ~ 36h, through 50 ~ 100r/min, 1 ~ 2h of ball milling, high-entropy alloy is prepared Composite powder.
It is sintered 3. high-entropy alloy-base composite powder is placed in graphite or sintered-carbide die, pressurize 30-80MPa, heating To 1000-1150 DEG C, 10-30min is kept the temperature, carrying out high-entropy alloy powder densification, (equipment choosing vacuum hotpressing stove waits Ionic discharge sintering furnace (SPS)), obtain the high-entropy alloy composite material.
The high-entropy alloy composite material is tested using XRD, TEM, testing machine for mechanical properties etc..
Compared with prior art, the present invention its remarkable advantage: designing and preparing technique by ingredient makes alloy substrate with height High-entropy alloy matrix based on plasticity face-centered cubic solid solution (FCC), while additional nano-ceramic particle segregation is in simple solid solution On body crystal boundary, generates ceramic enhancement phase and strengthen；During heating, cure under pressure, ceramic phase generates extrusion deformation effect to FCC phase It answers, forms deformation twin, to realize that the strong modeling of high-entropy alloy composite material combines, the high-entropy alloy for preparing high-strength and high ductility is multiple Condensation material or according to the molding part of mold inner-cavity shape.
Detailed description of the invention
Fig. 1 is high-entropy alloy composite material TEM figure prepared by the embodiment of the present invention 1；
Fig. 2 is the mechanical curves of high-entropy alloy composite material prepared by the embodiment of the present invention 1.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing.
It is 99.99% that according to the form below, which weighs purity, Al, Fe, Cr, Co, Ni, Cu, Ti alloy powder and purity of granularity≤45 μm For 99.99% nano-ceramic powder, granularity≤20 μm.
Table 1 prepares the quality that composite material selects metal constituent element, unit g.
Alloying element Al Fe Cr Co Cu Ni Ti Al2O3 TiC SiC
Embodiment 1 10.8 56 52 59 0 59 14.4 12.03 0 0
Embodiment 2 18.9 56 52 88.5 0 59 0 0 9.85 0
Embodiment 3 0 56 52 59 64 59 33.6 0 0 15.04
Embodiment 1
(1) use high energy ball mill by above-mentioned alloy powder and Al under argon atmosphere2O3Mixing and mechanical alloy Change, dry grinding revolving speed is 450r/min, and dry grind time 45h, wet-milling time 5h, wet-milling revolving speed 200r/min, and preparation has simple solid The composite powder of solution alloy matrix.Specific step is as follows:
A) powder for waiting ball milling is put into stainless steel grinding jar, using stainless steel ball as abrasive body, according to the ball of 10:1 Powder quality compares ball milling.Before ball milling, 10min first is vacuumized with vacuum machine, is filled with 0.5MPa argon gas later as protective gas；Ball The revolving speed of grinding machine is 450r/min, and to need to adjust direction of rotation primary by every 60min, ball milling 5 hours, 15 hours, it is 30 small When, 45 hours it is separately sampled.
B) dehydrated alcohol is added in 45 hours powder of ball milling and carries out wet-milling 5h.After ball milling terminates, ball grinder is taken out, Vacuum oven is opened, ball grinder cover is then opened, and reserve certain gap, shuts case after putting it into drying box Door, temperature is adjusted to 50 DEG C after being vacuumized with vacuum machine, is taken out after drying for 24 hours.Powder after dry is put Enter in ball mill, with the revolving speed ball milling 1h of 80r/min, is taken out for use after obtaining the screening of high-entropy alloy composite powder.
(2) composite powder after mechanical alloying is placed in graphite jig and is sintered, pressurize 30MPa, is heated to 1000 DEG C, 30min is kept the temperature, the high-entropy alloy composite material is made, alloying component atomic ratio expression formula is Al0.4FeCrCo1.5NiTi0.3(atomic ratio) -8vol% Al2O3。
(3) structure and performance characterization
Fig. 1 is that the TEM of composite material schemes, it is seen then that alumina particle of the granularity less than 10nm is gathered in grain boundaries, occurs A large amount of deformation twin tissues, and with the presence of ceramic particle around deformation twin.
Fig. 2 is the compressive stress strain curve of composite material, it can be seen that the compression yield strength of composite material, fracture Intensity and plastic strain respectively reach 2025 ± 20 Mpa, 2250 ± 15 MPa and 20 ± 0.50%, and micro-hardness is put down It is 683 ± 16Hv, and there is apparent twin deformation behavior in the plastic deformation initial stage of deformation.
It is above-mentioned it turns out that, compare existing high-entropy alloy composite material and its technique, the present invention prepared by outer Ghana Rice ceramic phase Strengthening and Toughening high-entropy alloy microstructure of composite is uniform, and no casting flaw realizes the good combination of intensity and plasticity, And it can be used for preparing the high-entropy alloy-base composite material part of near-net-shape.
Embodiment 2
Alloy powder and nano-ceramic powder are weighed by upper table, high-entropy alloy is prepared using identical method in embodiment 1 Composite material, alloying component Al0.7FeCrCo1.5Ni (atomic ratio)-TiC5vol%, the room temperature compression failure of the composite material Intensity and plastic strain respectively reach 2180MPa and 22.4%.
Embodiment 3
Alloy powder and nano-ceramic powder are weighed by upper table, high-entropy alloy is prepared using identical method in embodiment 1 Composite material, alloying component FeCrCoCuNiTi0.7(atomic ratio)-SiC10vol%, the room temperature compression failure of the composite material Intensity and plastic strain respectively reach 2290MPa and 21.4%.

Claims (4)

1. a kind of additional nano ceramics mutually enhances toughening high-entropy alloy composite material and preparation method thereof, which is characterized in that step are as follows:
1. being matched according to the predetermined ingredient of composite material, alloy powder and nano-ceramic powder are chosen；The alloy powder is former Minor is AlxFeCrCoyNi(Cu)mTiz, wherein x is 0.7, z 0, y 1.5, m 0；Or x is 0, z 0.7, y 1, m It is 1；
2. above-mentioned alloy powder and nano-ceramic powder are mixed using high energy ball mill under argon atmosphere and machinery closes Aurification, wherein dry grinding 400~500r/min of revolving speed, the dry grinding time be 40~50h, 2~5h of wet-milling time, wet-milling revolving speed 100~ 300r/min；After wet-milling, vacuum tank is opened, after being dried in vacuo 24~36h, through 50~100r/min, 1~2h of ball milling, is prepared High-entropy alloy composite powder；
It is sintered 3. above-mentioned high-entropy alloy-base composite powder is placed in graphite or sintered-carbide die, pressurize 30~80MPa, heating To 1000~1150 DEG C, 10~30min is kept the temperature, high-entropy alloy powder densification is carried out, it is compound to obtain the high-entropy alloy Material.
2. additional nano ceramics according to claim 1 mutually enhances toughening high-entropy alloy composite material and preparation method thereof, special Sign is, Al, Fe, Cr, Co, Ni, Cu, Ti metal powder purity > 99.9%, granularity≤45 μm.
3. additional nano ceramics according to claim 1 mutually enhances toughening high-entropy alloy composite material and preparation method thereof, special Sign is that the nano-ceramic powder is Al2O3, TiC, SiC, purity > 99.9%, granularity≤100nm.
4. additional nano ceramics according to claim 1 mutually enhances toughening high-entropy alloy composite material and preparation method thereof, special Sign is, is in terms of 100% by the volume of alloy powder, the volume of the nano-ceramic powder is 1~20%.
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