CN105648297A - Preparation method for high-entropy alloy composite material with externally-added nanometer ceramic phase reinforced and toughened - Google Patents
Preparation method for high-entropy alloy composite material with externally-added nanometer ceramic phase reinforced and toughened Download PDFInfo
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- 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
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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
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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
- 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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- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
Abstract
The invention discloses a preparation method for high-entropy alloy composite material with an externally-added nanometer ceramic phase reinforced and toughened. High-entropy alloy particles are adopted as the matrix phases, nanometer ceramic is externally added, the externally-added nanometer ceramic phase is segregated at the crystal boundary of solid solutions so as to be reinforced, the tough face-centered cubic solid solutions are extruded for forming deformation twins, and therefore combination of the strength and the plasticity of the high-entropy alloy composite material is realized, and the high-entropy alloy composite material high in strength and plasticity is prepared. The high-entropy alloy composite material high in strength and plasticity without machining allowances is remarkable in strength, high in hardness and excellent in compression strength and plasticity.
Description
Technical field
The invention belongs to metal-base composites technical field, the preparation method being specifically related to a kind of high-entropy alloy composite.
Background technology
Block high-entropy alloy (HEA) has a series of excellent mechanical performances being different from tradition crystal alloy such as high intensity, high rigidity, low elastic modelling quantity and big elastic strain limit so that it is considered as the structural material of great potential. But, high fragility makes HEA material when not having obvious room temperature macroscopic view plastic deformation, and calamitous fracture occurs in the way of catastrophic failure; The processing of material is brought extreme difficulties by high fragility, high rigidity. These all seriously govern HEA as advanced configuration material large-scale application in engineering. Therefore, brittleness at room temperature, processing difficulties problem have been developed as the important bottleneck of HEA materials application.
The problem of brittleness at room temperature and processing difficulties for improving HEA material, researcheres, by adding different metallic elements, adopt arc cast to prepare the block materials of dendritic segregation, and this is wherein obvious to add Cu effect, and its compression plastic strain reaches within 8%. Subsequently, Zhang Yong et al. prepares the high entropy alloy material with columanar structure by directional solidification technique, and its compressive ductility increases; Wang Yanping etc. adopt arc cast to be prepared for the CrFeCoNiCuAl high-entropy alloy-base composite material (HEAMCs) that interior raw 10vol.%TiC granule strengthens, and TiC becomes graininess to be evenly distributed on matrix, and size is about several micron. The compressive strength of CrFeCoNiCuTi-TiC composite and hardness can respectively reach 2040MPa and 746HV, compression plasticity about 12%. But the acquisition of the plasticity of above-mentioned high entropy alloy material, is not that to considerably reduce intensity be exactly improving in plasticity and inconspicuous.
Summary of the invention
It is an object of the invention to provide a kind of high-entropy alloy composite, while keeping its excellent in strength and hardness, improve the plasticity of composite.
The high-entropy alloy composite of the present invention, using high-entropy alloy granule as matrix phase, additional nano ceramics simultaneously, make additional nano ceramics phase segregation at solid solution grain boundaries, generation ceramic phase strengthens, and the face-centered cubic solid solution of toughness causes extruding simultaneously, forms deformation twin, thus what realize high-entropy alloy composite moulds by force combination, prepare the high-entropy alloy composite of high-strength and high ductility.
The preparation method that described additional nano ceramics strengthens toughening high-entropy alloy composite mutually, specifically includes following preparation process:
1. carry out proportioning according to the predetermined composition of composite, choose high-purity alloy powder and suitable nano-ceramic powder.Described alloy powder atomic formula is: AlxFeCrCoyNi(Cu)mTiz, wherein 0��x��0.7,0��z��0.7, x+z=0.7,1��y��1.5, m is 0 or 1.
The purity of described Al, Fe, Cr, Co, Ni, Cu, Ti metal dust > 99.9%, granularity��45 ��m.
Described nano-ceramic powder is Al2O3, TiC, SiC, purity > 99.9%, granularity��100nm. With the volume of alloy powder for 100%, the volume of nano-ceramic powder is 1 ~ 20%.
2. adopting high energy ball mill alloy powder and nano-ceramic powder to be mixed and mechanical alloying under argon atmosphere, dry grind rotating speed 400 ~ 500r/min, and the dry grinding time is 40 ~ 50h, wet grinding time 2 ~ 5h, and wet grinding rotating speed is 100 ~ 300r/min; After wet grinding, open vacuum tank, after vacuum drying 24 ~ 36h, through 50 ~ 100r/min ball milling 1 ~ 2h, prepare high-entropy alloy composite powder.
3. high-entropy alloy-base composite powder is placed in graphite or sintered-carbide die and sinters, pressurization 30-80MPa, heating is to 1000-1150 DEG C, insulation 10-30min, carry out high-entropy alloy powder body densification (equipment choosing vacuum hotpressing stove or spark plasma sintering stove (SPS)), obtain described high-entropy alloy composite.
Adopt XRD, TEM, testing machine for mechanical properties etc. that described high-entropy alloy composite is tested.
The present invention is compared with prior art, its remarkable advantage: make alloy substrate based on the high-entropy alloy matrix of high-ductility face-centered cubic solid solution (FCC) by composition design and preparation technology, additional nano-ceramic particle segregation is on simple solid solution crystal boundary simultaneously, produces ceramic enhancement phase strengthening; In heating, cure under pressure process, FCC phase is produced crimp effect by ceramic phase, form deformation twin, thus what realize high-entropy alloy composite moulds by force combination, prepare the high-entropy alloy composite of high-strength and high ductility or according to the part of dies cavity shape molding.
Accompanying drawing explanation
Fig. 1 is the high-entropy alloy composite TEM figure of the embodiment of the present invention 1 preparation;
Fig. 2 is the mechanical curves of the high-entropy alloy composite of the embodiment of the present invention 1 preparation.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be further described.
It is 99.99% that according to the form below weighs purity, and Al, Fe, Cr, Co, Ni, Cu, Ti alloy powder of granularity��45 ��m and purity are the nano-ceramic powder of 99.99%, granularity��20 ��m.
Table 1 is prepared composite and is selected the quality of metal constituent element, and unit is 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) adopt high energy ball mill by above-mentioned alloy powder and Al under argon atmosphere2O3Mixing and mechanical alloying, dry grinding rotating speed is 450r/min, and dry grind time 45h, wet grinding time 5h, wet grinding rotating speed 200r/min, and preparation has the composite powder of simple solid solution alloy matrix. Specifically comprise the following steps that
A) powder body waiting ball milling is put in rustless steel grinding jar, using stainless steel ball as abrasive body, compare ball milling according to the ball powder quality of 10:1. Before ball milling, first with vacuum machine evacuation 10min, it is filled with 0.5MPa argon afterwards as protective gas; The rotating speed of ball mill is 450r/min, and every 60min needs to adjust direction of rotation once, ball milling 5 hours, 15 hours, 30 hours, 45 hours separately sampled.
B) dehydrated alcohol is added in the ball milling powder of 45 hours and carry out wet grinding 5h. After ball milling terminates, take out ball grinder, vacuum drying oven is opened, then opens ball grinder cover, and reserve certain gap, close upper chamber door after putting it into drying baker, be adjusted to 50 DEG C by temperature after vacuum machine evacuation, take out after drying through 24h.Powder body after super-dry is put in ball mill, with the rotating speed ball milling 1h of 80r/min, takes out stand-by after obtaining the screening of high-entropy alloy composite powder.
(2) being placed in graphite jig by the composite powder after mechanical alloying and be sintered, pressurize 30MPa, and heating, to 1000 DEG C, is incubated 30min, prepares described high-entropy alloy composite, and its alloying component atomic ratio expression formula is Al0.4FeCrCo1.5NiTi0.3(atomic ratio)-8vol%Al2O3��
(3) structure and performance characterization
Fig. 1 is the TEM figure of composite, it is seen then that the granularity alumina particle less than 10nm is gathered in grain boundaries, a large amount of deformation twin tissue occurs, and all has ceramic particle to exist around deformation twin.
Fig. 2 is the compressive stress strain curve of composite, can be seen that the compression yield strength of composite, fracture strength and plastic strain respectively reach 2025 �� 20Mpa, 2250 �� 15MPa and 20 �� 0.50%, micro-hardness average out to 683 �� 16Hv, and in the plastic deformation initial stage deformed, there is obvious twin deformation behavior.
Above-mentioned it turns out that, compare existing high-entropy alloy composite and technique thereof, additional nano ceramics phase Strengthening and Toughening high-entropy alloy microstructure of composite prepared by the present invention is uniform, without casting flaw, achieve the good combination of intensity and plasticity, and may be used for preparing the high-entropy alloy-base composite material part of near-net-shape.
Embodiment 2
Weighing alloy powder and nano-ceramic powder by upper table, adopt identical method in embodiment 1 to prepare high-entropy alloy composite, alloying component is Al0.7FeCrCo1.5Ni (atomic ratio)-TiC5vol%, the room temperature compressed rupture strength of this composite and plastic strain respectively reach 2180MPa and 22.4%.
Embodiment 3
Weighing alloy powder and nano-ceramic powder by upper table, adopt identical method in embodiment 1 to prepare high-entropy alloy composite, alloying component is FeCrCoCuNiTi0.7(atomic ratio)-SiC10vol%, the room temperature compressed rupture strength of this composite and plastic strain respectively reach 2290MPa and 21.4%.
Claims (4)
1. an additional nano ceramics strengthens toughening high-entropy alloy composite material and preparation method thereof mutually, it is characterised in that comprise the following steps:
1. carry out proportioning according to the predetermined composition of composite, choose alloy powder and nano-ceramic powder; Described alloy powder atomic formula is AlxFeCrCoyNi(Cu)mTiz, wherein 0��x��0.7,0��z��0.7, x+z=0.7,1��y��1.5, m is 0 or 1;
2. high energy ball mill is adopted above-mentioned alloy powder and nano-ceramic powder to be mixed and mechanical alloying under argon atmosphere, wherein dry grinding rotating speed 400 ~ 500r/min, the dry grinding time is 40 ~ 50h, wet grinding time 2 ~ 5h, wet grinding rotating speed 100 ~ 300r/min; After wet grinding, open vacuum tank, after vacuum drying 24 ~ 36h, through 50 ~ 100r/min ball milling 1 ~ 2h, prepare high-entropy alloy composite powder;
3. being placed in by above-mentioned high-entropy alloy-base composite powder in graphite or sintered-carbide die and sinter, pressurize 30 ~ 80MPa, and heating, to 1000 ~ 1150 DEG C, is incubated 10 ~ 30min, carries out high-entropy alloy powder body densification, obtain described high-entropy alloy composite.
2. additional nano ceramics according to claim 1 strengthens toughening high-entropy alloy composite material and preparation method thereof mutually, it is characterised in that described Al, Fe, Cr, Co, Ni, Cu, Ti metal dust purity > 99.9%, granularity��45 ��m.
3. additional nano ceramics according to claim 1 strengthens toughening high-entropy alloy composite material and preparation method thereof mutually, it is characterised in that described nano-ceramic powder is Al2O3, TiC, SiC, purity > 99.9%, granularity��100nm.
4. additional nano ceramics according to claim 1 strengthens toughening high-entropy alloy composite material and preparation method thereof mutually, it is characterised in that with the volume of alloy powder for 100%, and the volume of described nano-ceramic powder is 1 ~ 20%.
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Cited By (25)
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| CN105908049A (en) * | 2016-06-20 | 2016-08-31 | 中国科学院兰州化学物理研究所 | High-entropy alloy self-lubricating composite material and preparation method thereof |
| CN106854080A (en) * | 2016-11-15 | 2017-06-16 | 中南大学 | A kind of preparation method of fine and close Ultra-fine Grained boron carbide ceramics material reduction sintering temperature |
| CN107142475A (en) * | 2017-04-22 | 2017-09-08 | 南京工程学院 | A kind of laser cladding strengthens new A lFeCrCoNiTi alloy-base composite materials coating and preparation method with TiC |
| CN108213422A (en) * | 2017-12-20 | 2018-06-29 | 中南大学 | A kind of preparation method of carbon containing high-entropy alloy composite material |
| CN108380892A (en) * | 2018-04-03 | 2018-08-10 | 武汉理工大学 | A kind of ceramics/high-entropy alloy laminated material and preparation method thereof |
| CN108842106A (en) * | 2018-07-13 | 2018-11-20 | 中南大学 | A kind of gauge ring and its preparation method and application |
| CN109022988A (en) * | 2018-09-21 | 2018-12-18 | 四川煜兴新型材料科技有限公司 | A kind of preparation method of tungsten base high-specific-gravity alloy material |
| CN109175380A (en) * | 2018-09-29 | 2019-01-11 | 甘肃顺域新材料科技有限公司 | A kind of laser gain material manufacturing method of wear-resistant high-entropy alloy gear |
| CN109338199A (en) * | 2018-09-19 | 2019-02-15 | 西安交通大学 | A kind of high-entropy alloy and preparation method thereof of ceramic particle enhancing |
| CN109694979A (en) * | 2017-10-20 | 2019-04-30 | 南京理工大学 | Vacuum induction melting prepares high-entropy alloy-base composite material and its method |
| CN109706367A (en) * | 2019-01-30 | 2019-05-03 | 河南一工钻业有限公司 | Multi-principal high-entropy alloy material and its application in screw tap processing |
| US20190194786A1 (en) * | 2017-12-22 | 2019-06-27 | Up Scientech Materials Corp. | Hardfacing Material |
| CN110004349A (en) * | 2019-02-13 | 2019-07-12 | 昆明理工大学 | A kind of carbon nanotube enhancing high-entropy alloy composite material and preparation method |
| CN110629059A (en) * | 2018-06-25 | 2019-12-31 | 南京理工大学 | Heterogeneous high-entropy alloy material and preparation method thereof |
| CN111705252A (en) * | 2020-06-18 | 2020-09-25 | 西北工业大学 | Al (aluminum)2O3Nano-particle reinforced CrCoNi intermediate entropy alloy-based composite material and preparation method thereof |
| CN111748721A (en) * | 2020-07-08 | 2020-10-09 | 重庆师范大学 | High-entropy alloy/metal glass composite material and preparation method thereof |
| CN112831679A (en) * | 2019-11-22 | 2021-05-25 | 南京理工大学 | Two-phase enhanced high-entropy alloy-based composite material and preparation method 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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