CN107893184B - A kind of nanometer of Ultra-fine Grained high-entropy alloy and preparation method thereof - Google Patents
A kind of nanometer of Ultra-fine Grained high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of nanometer of Ultra-fine Grained high-entropy alloy and preparation method thereof, the high-entropy alloy is AlxCoCrFeNi (x=0.1 ~ 0.45), the preparation method comprises the following steps: the ingot casting of vacuum melting is carried out homogenization heat treatment, high-entropy alloy ingot casting after above-mentioned heat treatment is carried out to the cold rolling pretreatment of 50% drafts, sample after cold rolling recycles the roll of gear-like to be rolled, obtain the workpiece of distortion wrinkle, the workpiece of wrinkle carries out cold rolling-straightening again, at this moment workpiece obtains second of deformation processing, and workpiece crystal grain under processing repeatedly gradually refines the nanometer Ultra-fine Grained high-entropy alloy for obtaining high-strength and high ductility.Unlimited deflection may be implemented while hardly changing the apparent size of sample in the method for wrinkle-cold rolling provided by the invention, greatly improves intensity, and the workpiece of some particular/special requirements is applicable in very much;And simple process is easily achieved, and can be widely applied to the working condition of high strength and high hardness requirement.
Description
Technical field
The present invention relates to a kind of nanometer of Ultra-fine Grained high-entropy alloys and preparation method thereof, belong to the processing of metal material nano-crystallization
Field.
Background technique
Nanocrystalline (Ultra-fine Grained) material is prepared using the method for large plastometric set, always is the hot spot of metal material research
Content, nanocrystalline material have an intensity, toughness of superelevation, and performance has compared to as-cast structure and enhances significantly.And it prepares nanocrystalline
Method, including rolling, high pressure torsion, etc. channel pressings, sandglass extrusion, wrinkle straightening etc. be always that large plastometric set direction is ground
The main contents studied carefully.Using the method for large plastometric set manufacture it is nanocrystalline be investigation of materials one of hot spot.
Multicomponent alloy is also known as high-entropy alloy, is the alloy system that British scholar Cantor is researched and developed earliest, China's platform
Simple solid solution alloy of the gulf scholar Ye Junwei earliest by multicomponent equimolar than, high entropy of mixing alloy is defined as high-entropy alloy.
High-entropy alloy thus has a series of excellent performances due to the mixing entropic effect and cocktail effect of multicomponent, such as high-intensitive,
High rigidity, high-wear resistance, excellent antioxygenic property and corrosion resistance etc..
Conventional metals are then that alloy property, example are adjusted by microelement alloying based on one or two kinds of elements
Such as steel, nickel base superalloy etc..In fact, high entropy solid solution alloy mutually forms the middle position for being located at alloy phase diagram, have
It is a supplement well for physics metallurgy not in traditional end border solid solution alloy.Meanwhile increasing more new conjunctions
A possibility that golden, opens the frontier of alloy design.
As new alloy material, high-entropy alloy has many performances excellent compared with conventional alloys material, and application field is got over
Carry out great attention that is wider, therefore causing more and more engineers and technicians.The face-centred cubic high-entropy alloy of as cast condition is surrendered
Intensity is relatively low with tensile strength, but has significant work hardening capacity.In the AlxCoCrFeNi of low stacking fault energy
In (x=0.1 ~ 0.45) high-entropy alloy deformation process other than dislocation strengthening, refined crystalline strengthening, there are also significant deformation twinning is strong
Change effect.Obtain the high-entropy alloy of nanocrystalline (Ultra-fine Grained) by the method for large plastometric set, then can be with by aging strengthening model
Optimize the strong plasticity of nanocrystalline (Ultra-fine Grained) high-entropy alloy.
Up to the present, for the research of high-entropy alloy, China Taiwan is in the leading level in the world, especially Taiwan
Tsinghua University and the Industrial Technology Research Institute of Taiwan.That high-entropy alloy is studied on ground earliest in China is University of Science & Technology, Beijing Zhang Yong professor, he studies
Project be mainly lightweight high-entropy alloy.Zhang Yong professor (Y. Zhang, Y.J. Zhou, J.P. Lin, G.L. Chen,
P.K. 10 (2008) 534-538. of Liaw, Advanced Engineering Materials) and City University of Hong Kong Guo
Bright doctor (S. Guo, C.T. Liu, Progress in Natural Science:Materials International
21 (2011) 433-446.) it is proposed respectively from mutually formation rule of the angle of the entropy of mixing and valence electron concentration to high-entropy alloy
Prediction.
The method for preparing nanocrystalline (Ultra-fine Grained) ultra-fine high-entropy alloy at present mainly passes through open die forging, cold rolling and high pressure torsion
Conventional method, the method for open die forging cold rolling and high pressure torsion is all to realize plastic deformation by changing the apparent size of sample,
And cold rolling tends to generate deformation texture, and high pressure torsion is then limited often difficult realization by experimental facilities.
In conclusion preparing the research report of nanocrystalline (Ultra-fine Grained) high-entropy alloy also currently with severe Plastic Deformation Methods
Seldom, the research of nanocrystalline (Ultra-fine Grained) high-entropy alloy with prepare it is very necessary.
Summary of the invention
In order to expand the application field of high-entropy alloy, the present invention provides a kind of nanometer of Ultra-fine Grained high-entropy alloy and its
Preparation method prepares a nanometer Ultra-fine Grained high-entropy alloy using wrinkle-cold rolling plastic deformation mode for the first time.It is subsequent when can pass through
The strong plasticity of the heat treatment method coordination nanometer Ultra-fine Grained high-entropy alloy of effect, recrystallization.
The present invention provides a kind of nanometer of Ultra-fine Grained high-entropy alloys, to have the single-phase face-centred cubic structure of excellent plasticity,
Ingredient is AlxCoCrFeNi represents the molar ratio of each element Al, Co, Cr, Fe, Ni as x:1:1:1:1;Wherein, x=0.1 ~
0.45。
Al, Co, Cr, Fe and Ni raw materials for metallurgy purity that the high-entropy alloy substrate uses are not less than 99.9 %.
The present invention provides the preparation method of a kind of nanometer of Ultra-fine Grained high-entropy alloy, by the alloy smelting raw material A l of use,
Co, Cr, Fe and Ni element carry out accurate weighing proportion according to molar ratio x:1:1:1:1 and purify oxidation on metal surface object;It will match
Good raw material is placed in the slot in the water cooled copper mould melting pond of II type vacuum arc furnace ignition of WK-, vacuumizes-applying argon gas, melting electric current
At 250 ~ 320 amperes, the time 30 ~ 60 seconds, after alloy sufficiently melts, alloy block is overturn, alloy pig is put into water cooling later
In the slot of copper mold, adjusting melting electric current is 250 ~ 320 amperes, after alloy melting is uniform, opens and inhales casting inlet valve, utilize pump
Interior vacuum carries out suction casting, is taken out after alloy mold is cooling to get the high-entropy alloy is arrived.
Further, the preparation method of nanometer Ultra-fine Grained high-entropy alloy, sequentially includes the following steps:
(1) the high-entropy alloy ingot casting for inhaling casting is heat-treated 5 hours uniform equiax crystal of acquisition ingredient in 1100 DEG C of homogenization
Tissue;
(2) alloy for crossing Homogenization Treatments carries out 50% drafts cold rolling pretreatment in CR-140 type milling train;
(3) sample after cold rolling being subjected to wrinkle processing, roll of the workpiece Jing Guo gear-like rolls, workpiece torsional deformation,
And first time deformation processing is obtained without drafts workpiece;Workpiece carries out cold rolling after going out roll, and the workpiece straightening of distortion passes through
Wrinkle 1 or 2 passages are cold rolled to 70% acquisition sheet specimens.
Further, above-mentioned heat treatment carries out in TL-1700 vacuum heat treatment furnace.
Further, the roll of the gear-like are as follows: diameter is 148 mm, and the diameter of circular groove gear is 4.2mm, circular groove it
Between spacing be 2.3mm, roll linear velocity is adjustable.
Beneficial effects of the present invention:
(1) present invention obtains the nanometer Ultra-fine Grained high entropy alloy material of unlimited deflection by wrinkle-cold rolling method, and
And the strong plasticity of the heat treatment method control nano material of recrystallization can be passed through.
(2) method of wrinkle-cold rolling of the present invention may be implemented while hardly changing the apparent size of sample
Unlimited deflection, greatly improves intensity, and the workpiece of some particular/special requirements is applicable in very much.
(3) present invention process is simply easily achieved, and can be widely applied to the working condition of high strength and high hardness requirement.
Detailed description of the invention
Fig. 1 is the schematic diagram of cylindrical rolls used in embodiment 1.
Fig. 2 is the schematic diagram of gear roll used in embodiment 1.
Fig. 3 is in embodiment 1 by the sample of wrinkle processing.
Fig. 4 is the nanocrystalline Al for the wrinkle of process prepared in embodiment 10.1The transmission of CoCrFeNi high-entropy alloy
Electronic Speculum shape appearance figure.
Fig. 5 is the nanocrystalline Al by wrinkle twice prepared in embodiment 10.1The transmission of CoCrFeNi high-entropy alloy
Electronic Speculum shape appearance figure.
Fig. 6 is nanocrystalline Al in embodiment 10.1The stretching engineering stress strain curve of CoCrFeNi high-entropy alloy.
Fig. 7 is Al in embodiment 20.45CoCrFeNi high-entropy alloy stretches engineering stress strain curve.
Fig. 8 is Al in embodiment 20.45The transmission electron microscope organization chart of 700 DEG C of CoCrFeNi high-entropy alloy heat treatment 1 hour
Piece.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1:
A kind of nanocrystalline A0.1The preparation method of CoCrFeNi high-entropy alloy, the specific steps are as follows:
The preparation of sample
(1) the high-entropy alloy ingot casting of 100 × 20 × 3mm of casting is inhaled using II type vacuum arc furnace ignition of WK-.
(2) sample for inhaling casting 1100 DEG C of homogenization of TL-1700 Tubular thermal treatment furnace are placed on to be heat-treated 5 hours.
(3) alloy for crossing Homogenization Treatments is pre- in CR-140 type milling train (using roll shown in Fig. 1) 50% cold rolling of progress
Shown in processing.Cleaning roll and platform surface before rolling, open master switch and power on buttons, adjust button by height and stitch rolling
Thickness is to suitable position (should be greater than sample thickness).Drafts should not be too large when rolling, and each drafts is small no more than five
Lattice, every pressure once need repeat-rolling repeatedly (at least ten times).
(4) the gear roll shown in Fig. 2 of the sample after cold rolling is subjected to wrinkle processing, roll of the workpiece Jing Guo gear-like
Rolling, workpiece torsional deformation, and first time deformation processing is obtained without drafts workpiece;Workpiece carries out cold rolling after going out roll, will
The workpiece straightening of distortion is tried by nanocrystalline (Ultra-fine Grained) high-entropy alloy that control wrinkle-cold rolling pass obtains different distortion amount
Sample.
Sample after wrinkle are primary is as shown in Figure 3.
It is as shown in Figure 2 that shown this tests used gear roll.It is shone by the sample transmission Electronic Speculum of 50% cold roling reduction
Piece is as shown in the figure.It is primary by wrinkle, sample transmission electromicroscopic photograph twice is as shown in the figure
By the sample of cold rolling and wrinkle twice, yield strength has reached 984 MPa, and tensile strength has reached 1231MPa,
Inside forms the Ultra-fine Grained and deformation twin of nanoscale.
Embodiment 2
With 1 difference of embodiment with Al0.45CoCrFeNi be substrate carry out and sample without homogenization heat at
Reason, other steps are identical.
Its material engineering stress-strain diagram after 2 wrinkle-cold rollings is as shown in fig. 7, by 700 DEG C of heat treatments 1
Tiny nanometer crystal microstructure is formd after hour, microscopic structure is as shown in figure 8, its yield strength is respectively reached with tensile strength
1280 MPa and 1411 MPa.
Claims (4)
1. the preparation method of a kind of nanometer of Ultra-fine Grained high-entropy alloy, the nanometer Ultra-fine Grained high-entropy alloy is single-phase face-centered cubic knot
Structure, ingredient AlxCoCrFeNi represents the molar ratio of each element Al, Co, Cr, Fe, Ni as x:1:1:1:1;Wherein, x=0.1 ~
0.45;It is characterized by: by alloy smelting raw material A l, Co, Cr, Fe and Ni element of use according to molar ratio x:1:1:1:1 into
Row accurate weighing matches and purifies oxidation on metal surface object;The raw material prepared is placed on to the water-cooled copper of II type vacuum arc furnace ignition of WK-
In slot in mould melting pond ,-applying argon gas is vacuumized, melting electric current is 250 ~ 320 amperes, and the time is 30-60 seconds, is filled to alloy
After dividing fusing, alloy block is overturn, alloy pig is put into the slot of water cooled copper mould later, adjusts melting electric current in 250 ~ 320 peaces
Training opens after alloy melting is uniform and inhales casting inlet valve, carries out suction casting using vacuum in pumping, takes out after alloy mold is cooling,
Obtain high-entropy alloy;
The preparation method sequentially includes the following steps:
(1) alloy smelting raw material A l, Co, Cr, Fe and Ni element of use is subjected to accurate weighing according to molar ratio x:1:1:1:1
It matches and purifies oxidation on metal surface object;
(2) raw material prepared is placed in the slot in the water cooled copper mould melting pond of II type vacuum arc furnace ignition of WK-, vacuumizes-argon filling
Gas, melting electric current are 250 ~ 320 amperes, and the time is 30-60 seconds, and after alloy sufficiently melts, alloy block is overturn, and will be closed later
Ingot is put into the slot of water cooled copper mould, and adjusting melting electric current is 250 ~ 320 amperes, after alloy melting is uniform, is opened to inhale to cast and be inhaled
Air valve carries out suction casting using vacuum in pumping, is taken out after alloy mold is cooling to get high-entropy alloy is arrived;
(3) the high-entropy alloy ingot casting for inhaling casting is heat-treated 5 hours uniform equiax crystal groups of acquisition ingredient in 1100 DEG C of homogenization
It knits;
(4) alloy for crossing Homogenization Treatments carries out the cold rolling pretreatment of 50% drafts in CR-140 type milling train;
(5) sample after cold rolling is subjected to wrinkle processing, roll rolling of the workpiece Jing Guo gear-like, workpiece torsional deformation, and do not had
There is drafts workpiece to obtain first time deformation processing;Workpiece carries out cold rolling after going out roll, by the workpiece straightening of distortion, passes through wrinkle
1 ~ 2 passage-is cold rolled to 70% processing and obtains sample.
2. the preparation method of according to claim 1 nanometer of Ultra-fine Grained high-entropy alloy, it is characterised in that: the high-entropy alloy
Al, Co, Cr, Fe and Ni raw materials for metallurgy purity that substrate uses are not less than 99.9 %.
3. the preparation method of according to claim 1 nanometer of Ultra-fine Grained high-entropy alloy, it is characterised in that: in step (3)
Heat treatment carries out in TL-1700 vacuum heat treatment furnace.
4. the preparation method of according to claim 1 nanometer of Ultra-fine Grained high-entropy alloy, it is characterised in that: the gear-like
Roll are as follows: diameter is 148 mm, and the diameter of circular groove gear is 4.2mm, and the spacing between circular groove is 2.3mm, roll linear velocity energy
It adjusts.
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CN108998714B (en) * | 2018-06-07 | 2020-04-24 | 东南大学 | Design and preparation method of biphase intermediate entropy alloy |
CN110629059B (en) * | 2018-06-25 | 2021-02-23 | 南京理工大学 | Heterogeneous high-entropy alloy material and preparation method thereof |
CN110144476A (en) * | 2019-06-04 | 2019-08-20 | 中北大学 | A kind of preparation method of aluminium cobalt ferrochrome nickel high-entropy alloy |
CN111394636B (en) * | 2020-03-24 | 2021-06-15 | 太原理工大学 | High-strength high-plasticity high-entropy alloy with martensite phase transformation and preparation method thereof |
CN111961893B (en) * | 2020-07-20 | 2022-02-11 | 东南大学 | High-strength high-plasticity high-entropy alloy and preparation method thereof |
CN112893468A (en) * | 2021-02-08 | 2021-06-04 | 太原理工大学 | Method for improving strength of Fe-Mn-Cr-Ni high-entropy alloy through corrugated rolling and plain rolling process |
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