CN107034410A - A kind of many pivot high-entropy alloys and preparation method thereof - Google Patents
A kind of many pivot high-entropy alloys and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of many pivot high-entropy alloys and preparation method thereof, the wherein composition of many pivot high-entropy alloys is FeaCobNicAldCue, wherein, a, b, c, d and e represent the corresponding mol ratio of each element, and 0.9≤a≤1.1,0.9≤b≤1.1,0.9≤c≤1.1,0.9≤d≤1.1,0.9≤e≤2.0 respectively.Many pivot high-entropy alloys have good plasticity, while higher intensity, excellent in mechanical performance can be obtained.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of many pivot high-entropy alloys and preparation method thereof.
Background technology
Nineteen ninety-five, TaiWan, China scholar Ye Junwei research groups break through conventional alloys design concept and propose that the high entropy of many pivots is closed
The concept of gold, is defined as high-entropy alloy to be made up of five kinds or more than five kinds essential elements, the molar fraction of every kind of element is in 5%-
Within the scope of 35%, then pass through alloy formed by the technique necessarily synthesized.Substantial amounts of experimental study shows that participant forms gold
The conventional alloys of compound or other complicated phases are different between category, and high-entropy alloy can produce high entropic effect and suppress intermetallic
The formation of thing, so as to promote element to be mixed to form the solid solution of simple phase structure（Mainly fcc（Face Center Cubic/
Face-Centered Cubic, face-centered cubic lattice）Or bcc（Stand Body-Centered Cubic Structure, body-centered
Prismatic crystal lattice）Structure）, the high-entropy alloy of some compositions can also nanocrystal even amorphous structure.It is high compared with conventional alloys
Entropy alloy is in addition to it can produce high entropic effect, the also slow effect of atoms permeating, distortion of lattice effect and cocktail effect.Institute
Conventional alloys are better than in some aspect of performances with, emerging high-entropy alloy, such as hardness, intensity, corrosion resistance, processing hardening,
High temperature resistance property of softening etc..It can be seen that, high-entropy alloy has great application prospect as a kind of material of innovation.
By vicennial exploratory development, the academic theory and practical application of many pivot high-entropy alloys have obtained hair energetically
Exhibition.At present, the research of many pivot high-entropy alloys relates generally to optimized alloy composition, phase formation mechenism, each pivot cellulose content pairing
The influence of payment organization structure, mechanical property, and different processing and influence of the Technology for Heating Processing to alloy structure and performance.Separately
Outside, performance, the practical application of researchers to improve alloy etc., is led more using a variety of different preparation method preparation/researchs
First high-entropy alloy, and influence of the research its preparation method to alloy, such as：Vacuum arc furnace melting, mechanical alloy, laser melting coating
Deng.
The performance of optimized alloy is the main purpose and meaning that scholars study alloy.Tool is found in the research reported
There is the high-entropy alloy system of high-ductility, its intensity is but very low, and the of a relatively high high-entropy alloy system of intensity, but its plasticity compares
It is poor.With more and more higher of the industry to alloy performance requirement, especially pair have both high intensity and alloy easy to process simultaneously
Application demand it is more extensive, with this, exploitation has high-ductility concurrently and many pivot high-entropy alloys of high intensity are extremely urgent.
The content of the invention
In view of the above-mentioned problems, the invention provides a kind of many pivot high-entropy alloys and preparation method thereof, obtained many pivots
High-entropy alloy is provided simultaneously with excellent intensity and plasticity.
The technical scheme that the present invention is provided is as follows：
A kind of many pivot high-entropy alloys, the composition of many pivot high-entropy alloys is FeaCobNicAldCue, wherein, a, b, c, d and e
Represent the corresponding mol ratio of each element respectively, and 0.9≤a≤1.1,0.9≤b≤1.1,0.9≤c≤1.1,
0.9 ≤ d ≤ 1.1、0.9 ≤ e ≤ 2.0。
It is further preferred that Fe, Co, Ni, Al and Cu raw material that many pivot high-entropy alloys are selected are that purity is big
In 99.99% granular/block stock.
Present invention also offers a kind of many pivot method for preparing high-entropy alloy, including：
S1 weighs Fe, Co, Ni, Al and Cu former material of corresponding weight according to the mol ratio of each element in many pivot high-entropy alloys
Material, wherein, the mol ratio of each element be respectively 0.9≤a≤1.1,0.9≤b≤1.1,0.9≤c≤1.1,
0.9 ≤ d ≤ 1.1、0.9 ≤ e ≤ 2.0；
The raw material weighed up and titanium ingot are respectively put into the copper crucible in smelting furnace by S2 to carry out melting and obtains alloying component and be
FeaCobNicAldCueMany pivot high-entropy alloy ingot castings.
It is further preferred that the smelting furnace is vacuum arc melting furnace.
It is further preferred that specifically including in step s 2：
The raw material weighed up and titanium ingot are respectively put into the copper crucible in smelting furnace by S21 after smelting furnace is cleaned up；
S22 will extract vacuum with mechanical diffusion in smelting furnace, further further be vacuumized until vacuum with molecule diffusion pump
Value reaches that the first preset value stops；
High purity argon is filled with into smelting furnace by S23 until vacuum values reach that the second preset value stops in smelting furnace；
S24 opens magnetic stirrer, by titanium ingot melting one to twice；
S25 adds the raw material melt back weighed up repeatedly until uniform, completion melting.
In many pivot high-entropy alloys that the present invention is provided and preparation method thereof, following beneficial effect can be brought：
1）Many pivot high-entropy alloys have good plasticity, while higher intensity, excellent in mechanical performance can be obtained；
2）The preparation method technique is simple, and cost is relatively low, workable, is adapted to industrialized production.
Brief description of the drawings
Below by clearly understandable mode, preferred embodiment is described with reference to the drawings, to above-mentioned characteristic, technical characteristic,
Advantage and its implementation are further described.
Fig. 1 is the X-ray diffraction XRD spectra for many pivot high-entropy alloys that two examples are obtained；
The metallograph that Fig. 2 is many pivot high-entropy alloy FeCoNiAlCu in embodiment 1；
Fig. 3 is many pivot high-entropy alloy FeCoNiAlCu scanning electron microscope (SEM) photographs in embodiment 1；
Fig. 4 is many pivot high-entropy alloy FeCoNiAlCu in embodiment 21.5Metallograph；
Fig. 5 is many pivot high-entropy alloy FeCoNiAlCu in embodiment 21.5Scanning electron microscope (SEM) photograph；
Fig. 6 is the compressive stress strain curve figure for many pivot high-entropy alloys that two examples are obtained.
Embodiment
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, control is illustrated below
The embodiment of the present invention.It should be evident that drawings in the following description are only some embodiments of the present invention, for
For those of ordinary skill in the art, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing, and obtain other embodiments.
The invention provides a kind of many pivot high-entropy alloys, specifically, the composition of many pivot high-entropy alloys is
FeaCobNicAldCue, wherein, a, b, c, d and e represent the corresponding mol ratio of each element, and 0.9≤a≤1.1,0.9 respectively
≤ b ≤ 1.1、0.9 ≤ c ≤ 1.1、0.9 ≤ d ≤ 1.1、0.9 ≤ e ≤ 2.0.In one example, a=1.0,
B=1.0, c=1.0, d=1.0 and 1.0≤e≤1.5, that is, many pivot high-entropy alloys obtained are FeCoNiAlCu1-1.5。
In the method for preparing many pivot high-entropy alloys, including：
（1）Raw material pre-treatment, alloy raw material is placed in beaker, pours into the hydrochloric acid solution of low solubility, removes the oxidation on its surface
Layer, raw material is put into the beaker equipped with ethanol and beaker is placed in into cleaning in ultrasonic washer instrument again after layer to be oxidized removing completely
Certain time, such as 10 minutes；Then change ethanol and clean certain time again, such as 5 minutes, finally dried raw material with hair drier
Drying, in case melting is used.
（2）Dispensing, according to the mol ratio of many pivot high-entropy alloys, accurately weighed with electronic balance Fe, Co, Ni, Al and
Cu raw material（Purity is more than 99.99% granular/block stock）And mix.
（3）Molten alloy, first removes foreign matter in stove, and cleaned the copper crucible in smelting furnace and its inwall with absolute ethyl alcohol
Totally, recirculating cooling water system is then opened, load weighted mixed material and titanium ingot are then respectively put into the copper crucible in stove
In, fasten fire door.Body of heater is extracted into low vacuum to certain value with mechanical diffusion, such as 10 Pa（Handkerchief）, then spread using molecule
Pumping takes high vacuum to the first preset value, such as 2.5 × 10-3 Pa；Corresponding valve is then shut off, charging valve is opened, started
High purity argon is passed through into stove, treats that the atmospheric pressure in stove gos up to about the second preset value, during such as 0.5 Pa, closing is filled
Air valve stops logical argon gas.Then start melting, electrode is down to from striking at crucible 1-2 mm, then electrode lifting to suitably
Position, then slowly high current is to 230 ~ 280 A progress meltings, while opening magnetic stirrer, before melting sample first
By titanium ingot melting one to twice, oxygen content in stove is further reduced；Each alloy sample is overturn into melting repeatedly repeatedly again, such as 4
It is secondary to uniform, and each smelting time of alloy is 3 min to 4 min.After melting terminates, power supply is closed, alloy cooling is treated about
After 10 min, vent valve is opened, that opens that vacuum melting furnace door can obtain button shape has many of high-ductility and high intensity concurrently
Pivot high-entropy alloy ingot casting.
High vacuum arc-melting furnace used in following examples is limited for Chinese Academy of Sciences's Shenyang scientific instrument share
The DHL-300 type high vacuum arc-melting furnaces of company's production.
To much the Mechanics Performance Testing of pivot high-entropy alloy and the characterization information of institutional framework are as follows：
(1) material phase analysis：Material phase analysis is carried out using German Bruker D-8fucus types X-ray diffractometer, operating voltage is 40
KV, sweep speed 4s/ are walked, 0.02 ° of step-length, 20 ° -100 ° of diffraction angular region.
(2) microstructure：Using MeF3 types metallographic microscope and the F SEM of Japan FEI Quanta 200
Carry out microstructure observation.
(3) room temperature compression performance is tested：Room temperature compression test, test sample are carried out using MTS types electronic universal tester
Cuboid is made and high wide according to pertinent regulations in metal material room temperature compression test method (GB/T7314-2005) national standard
Than being defined as 2:1, the specification of test sample of the invention is the mm of the mm of 3 mm × 3 × 6, strain rate 1 × 10-4。
The purity of Fe, Co, Ni, Al and Cu raw material described in following examples are 99.99%.
Embodiment 1
The composition of many pivot high-entropy alloys is FeCoNiAlCu, i.e. a=1.0, b=1.0, c=1.0, d=1.0, e=1, specific steps
It is as follows：
Step 1：Alloy raw material is placed in beaker, the hydrochloric acid solution of low solubility is poured into, the oxide layer on its surface is removed, it is to be oxidized
Raw material is put into the beaker equipped with ethanol and beaker is placed in into cleaning 10 minutes in ultrasonic washer instrument again after layer removing completely, so
Ethanol is changed afterwards to clean again 5 minutes, and finally raw material are dried with hair drier and dried up, in case melting is used.
Step 2：According to the mol ratio of many pivot high-entropy alloys, Fe, Co, Ni, Al and Cu are accurately weighed with electronic balance
Raw material are simultaneously mixed.
Step 3：Foreign matter in stove is first removed, and is scrubbed the copper crucible and its inwall in smelting furnace with absolute ethyl alcohol,
Then recirculating cooling water system is opened, then load weighted mixed material and titanium ingot are respectively put into the copper crucible in stove, is closed
Tight fire door.Body of heater is extracted into low vacuum to 10 Pa with mechanical diffusion, then high vacuum is extracted to 2.5 using molecule diffusion pump
×10-3 Pa；Corresponding valve is then shut off, charging valve is opened, starts to be passed through high purity argon into stove, treat big in stove
When atmospheric pressure is gone up to about 0.5 Pa, close charge valve and stop logical argon gas.Then start melting, electrode is down to from crucible
Striking at 1-2 mm, then electrode lifting to suitable position, then slowly high current carries out melting to 230 ~ 280 A, together
Shi Kaiqi magnetic stirrers, it is further to reduce oxygen content in stove first by titanium ingot melting one to twice before melting sample, then will
Each alloy sample overturns melting 4 times to uniform repeatedly, and each smelting time of alloy is 3 min to 4 min.Melting terminates
Afterwards, power supply is closed, after alloy cools down about 10 min, vent valve is opened, button shape can be obtained by opening vacuum melting furnace door
The many pivot high-entropy alloy ingot castings for having high-ductility and high intensity concurrently.
Cut using wire cutting machine in gained FeCoNiAlCu alloy cast ingots, cut several pieces size for 3 mm × 3
The mm of mm × 6 sample, respectively as metallographic specimen, XRD（X-Ray Diffraction, X-ray diffraction）Sample and compression are tried
Sample.Then metallographic specimen is inlayed, polished, is polished, is corroded, XRD samples and compression sample are carried out slightly with 240# sand paper
Mill, is cleaned by ultrasonic to XRD samples and compression sample with absolute ethyl alcohol, obtains FeCoNiAlCu high-entropy alloys to be tested afterwards
Sample, afterwards：
Material phase analysis, its X-ray diffraction are carried out to the FeCoNiAlCu high-entropy alloys XRD samples（XRD）Spectrogram such as Fig. 1 institutes
Show, it is known that FeCoNiAlCu high-entropy alloys are by face-centered cubic（Fcc in diagram）And body-centered cubic（Bcc in diagram）Solid solution phase group
Into.
To the FeCoNiAlCu high-entropy alloys metallographic specimen carry out Analysis on Microstructure, its metallograph as shown in Fig. 2
ESEM（SEM）As shown in Figure 3, it is known that, alloy is typical dendrite tissue.
To the FeCoNiAlCu high-entropy alloys compression sample carry out room temperature Compressive Mechanical Properties test, its compression stress-
Strain curve is as shown in Figure 6, it is known that the room temperature compression yield strength of FeCoNiAlCu high-entropy alloys is 882 MPa, compression strength
For 1481 MPa, compression strain is 18.9%.
Embodiment 2
The composition of many pivot high-entropy alloys is FeCoNiAlCu1.5, i.e. a=1.0, b=1.0, c=1.0, d=1.0, e=1.5, specifically
Step is as follows：
Step 1：Alloy raw material is placed in beaker, the hydrochloric acid solution of low solubility is poured into, the oxide layer on its surface is removed, it is to be oxidized
Raw material is put into the beaker equipped with ethanol and beaker is placed in into cleaning 10 minutes in ultrasonic washer instrument again after layer removing completely, so
Ethanol is changed afterwards to clean again 5 minutes, and finally raw material are dried with hair drier and dried up, in case melting is used.
Step 2：According to the mol ratio of many pivot high-entropy alloys, Fe, Co, Ni, Al and Cu are accurately weighed with electronic balance
Raw material are simultaneously mixed.
Step 3：Foreign matter in stove is first removed, and is scrubbed the copper crucible and its inwall in smelting furnace with absolute ethyl alcohol,
Then recirculating cooling water system is opened, then load weighted mixed material and titanium ingot are respectively put into the copper crucible in stove, is closed
Tight fire door.Body of heater is extracted into low vacuum to 10 Pa with mechanical diffusion, then high vacuum is extracted to 2.5 using molecule diffusion pump
×10-3 Pa；Corresponding valve is then shut off, charging valve is opened, starts to be passed through high purity argon into stove, treat big in stove
When atmospheric pressure is gone up to about 0.5 Pa, close charge valve and stop logical argon gas.Then start melting, electrode is down to from crucible
Striking at 1-2 mm, then electrode lifting to suitable position, then slowly high current carries out melting to 230 ~ 280 A, together
Shi Kaiqi magnetic stirrers, it is further to reduce oxygen content in stove first by titanium ingot melting one to twice before melting sample, then will
Each alloy sample overturns melting 4 times to uniform repeatedly, and each smelting time of alloy is 3 min to 4 min.Melting terminates
Afterwards, power supply is closed, after alloy cools down about 10 min, vent valve is opened, button shape can be obtained by opening vacuum melting furnace door
The many pivot high-entropy alloy ingot castings for having high-ductility and high intensity concurrently.
Using wire cutting machine in gained FeCoNiAlCu1.5Alloy cast ingot is cut, cut several pieces size for 3 mm ×
The mm of 3 mm × 6 sample, respectively as metallographic specimen, XRD samples and compression sample.Then metallographic specimen is inlayed, ground
Light, polishing, corrosion, with 240# sand paper to XRD samples and compression sample roughly grind, afterwards with absolute ethyl alcohol to XRD samples with
Compression sample is cleaned by ultrasonic, and obtains FeCoNiAlCu1.5High-entropy alloy sample to be tested, afterwards：
To the FeCoNiAlCu1.5High-entropy alloy XRD samples carry out material phase analysis, and its X-ray diffraction spectrogram is as shown in figure 1, can
Know FeCoNiAlCu1.5High-entropy alloy is by face-centered cubic（Fcc in diagram）And body-centered cubic（Bcc in diagram）Solid solution phase is constituted.
To the FeCoNiAlCu1.5High-entropy alloy metallographic specimen carries out Analysis on Microstructure, its metallograph such as Fig. 4 institutes
Show, ESEM is as shown in Figure 5, it is known that, alloy is typical dendrite tissue.
To the FeCoNiAlCu1.5High-entropy alloy compression sample carries out room temperature Compressive Mechanical Properties test, and it compresses should
Force-strain curve is as shown in Figure 6, it is known that FeCoNiAlCu1.5The room temperature compression yield strength of high-entropy alloy is 689 MPa, resistance to compression
Intensity is 1302 MPa, and compression strain is 36.1%.
It should be noted that above-described embodiment can independent assortment as needed.Described above is only the preferred of the present invention
Embodiment, it is noted that for those skilled in the art, is not departing from the premise of the principle of the invention
Under, some improvements and modifications can also be made, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of many pivot high-entropy alloys, it is characterised in that the composition of many pivot high-entropy alloys is FeaCobNicAldCue,
Wherein, a, b, c, d and e represent the corresponding mol ratio of each element respectively, and 0.9≤a≤1.1,0.9≤b≤1.1,
0.9 ≤ c ≤ 1.1、0.9 ≤ d ≤ 1.1、0.9 ≤ e ≤ 2.0。
2. many pivot high-entropy alloys as claimed in claim 1, it is characterised in that the Fe of many pivot high-entropy alloys selections,
Co, Ni, Al and Cu raw material are granular/block stock that purity is more than 99.99%.
3. a kind of many pivot method for preparing high-entropy alloy, it is characterised in that the preparation method includes：
S1 weighs Fe, Co, Ni, Al and Cu former material of corresponding weight according to the mol ratio of each element in many pivot high-entropy alloys
Material, wherein, the mol ratio of each element be respectively 0.9≤a≤1.1,0.9≤b≤1.1,0.9≤c≤1.1,
0.9 ≤ d ≤ 1.1、0.9 ≤ e ≤ 2.0；
The raw material weighed up and titanium ingot are respectively put into the copper crucible in smelting furnace by S2 to carry out melting and obtains alloying component and be
FeaCobNicAldCueMany pivot high-entropy alloy ingot castings.
4. many pivot method for preparing high-entropy alloy as claimed in claim 3, it is characterised in that the smelting furnace is vacuum arc
Smelting furnace.
5. many pivot method for preparing high-entropy alloy as claimed in claim 4, it is characterised in that specifically include in step s 2：
The raw material weighed up and titanium ingot are respectively put into the copper crucible in smelting furnace by S21 after smelting furnace is cleaned up；
S22 will extract vacuum with mechanical diffusion in smelting furnace, further further be vacuumized until vacuum with molecule diffusion pump
Value reaches that the first preset value stops；
High purity argon is filled with into smelting furnace by S23 until vacuum values reach that the second preset value stops in smelting furnace；
S24 opens magnetic stirrer, by titanium ingot melting one to twice；
S25 adds the raw material melt back weighed up repeatedly until uniform, completion melting.
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| CN110373595A (en) * | 2019-08-06 | 2019-10-25 | 西安工业大学 | A kind of high entropy high temperature alloy of high-performance and preparation method thereof |
| CN111809096A (en) * | 2020-06-23 | 2020-10-23 | 江苏理工学院 | CuNiTi series high-entropy alloy and preparation method thereof |
| CN111809096B (en) * | 2020-06-23 | 2021-12-21 | 江苏理工学院 | CuNiTi series high-entropy alloy and preparation method thereof |
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