CN107523740A - CuCrFeNiTi high entropy alloy materials and preparation method thereof - Google Patents
CuCrFeNiTi high entropy alloy materials and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The present invention relates to a kind of high entropy alloy material and its technology of preparing.High entropy alloy material composition is CuCrFeNiTi, wherein Cu:Cr:Fe:Ni:Ti mol ratio is followed successively by 1:1:1:1:1.Its preparation method is：First, it is ultrasonically treated：Priority acetone soln and absolute ethyl alcohol are cleaned by ultrasonic Cu materials, Cr materials, Fe materials, Ni materials, Ti materials；2nd, weighing：According to equimolar than weighing each material；3rd, melting：Melting, which is repeated, using the material of vacuum non-consumable electrode arc melting stove weighing prepares alloy 4 ~ 5 times.Compared with traditional alloy material, CuCrFeNiTi high-entropy alloys prepared by the present invention have simple face-centred cubic structure, body-centered cubic structure and Laves phases, higher hardness and stronger corrosion resistance are shown, can be applied to wear-resisting, corrosion-resistant pressure vessels for the chemical industry and engineering high-strength corrosion-resistant part.
Description
Technical field
The present invention relates to a kind of metal material and preparation method thereof, in particular to a kind of high rigidity, corrosion resistant
CuCrFeNiTi high-entropy alloys and preparation method thereof, belong to alloy material and its preparing technical field.
Background technology
Traditional alloy design concept is using one or two kind of element as matrix, adds a small amount of other elements, component alloy,
Such as magnesium alloy, aluminium alloy, stainless steel and block amorphous alloy.Traditional crystallographic theory is thought, adds excessive micro conjunction
Gold element can result in compound and other complex organization's structures between various metals so that and the mechanical performance of alloy reduces,
It is difficult to be applied in practical application.With the high speed development of present industrial engineering technology, the deficiency of homogenous material performance is
Through the bottleneck that it further develops in engineering field as restriction.Therefore research staff increasingly tends to use new and high technology
Exploitation prepares all excellent novel-section of properties such as high performance new material, research and development intensity, toughness, hardness, corrosion resistance
Material, it has also become the Main way of Material Field development.In the 1990s, TaiWan, China scholar Ye Junwei takes the lead in proposing one
The novel alloy design concept of kind, i.e. multi-principal elements alloy.So-called multi-principal elements alloy, i.e., by 5 kinds and more than 5 kinds essential element structures
Into, and every kind of essential element atomic percent is 5%~35% alloy.Due to alloy constituent element species more than and content all very
Height, its atomic arrangement entropy of mixing is very high, therefore this multi-principal elements alloy is otherwise known as more pivot high-entropy alloys.More high entropys of pivot
The conventional alloys that alloy has broken using a kind of alloying element as base design pattern, can be had by alloying component optimization design
Have the tissue signatures such as microstructure simplification, nano-scaled precipitate, non crystalline structure, nanocrystal and high intensity, high rigidity, it is wear-resisting,
The excellent combining properties alloy such as corrosion-resistant, high temperature resistant creep, high temperature oxidation resisting, resistance to temper softening, is widely used in resistance to height
Pressure, corrosion-resistant pressure vessels for the chemical industry and engineering high-strength corrosion-resistant part.Therefore, the research and development of more pivot high-entropy alloys to conventional metallurgical and
The lifting of steel industry is significant.Therefore, the CuCrFeNiTi high-entropy alloys that hardness is high, corrosion resistance is strong are developed also to have
There is very important meaning.
The content of the invention
It is an object of the invention to develop with all good high-entropy alloy of wearability and corrosion resistance --- CuCrFeNiTi
High-entropy alloy, it is set to meet that people are to material hardness, the requirement of corrosion resisting property in modern industry so that high-entropy alloy is being answered
It is used widely with field.
The present invention is for the technical scheme taken of solution above-mentioned technical problem：A kind of high entropy alloy material, composition are
CuCrFeNiTi, wherein, Cu:Cr:Fe:Ni:Ti mol ratio is followed successively by 1:1:1:1:1.The Cu materials that the high-entropy alloy uses
The purity of material, Cr materials, Fe materials, Ni materials and Ti materials is not less than 99.7%, and the form using raw material is except powder
Sheet, bulk or large grained outside shape.
The present invention also includes to solve the technical scheme that above-mentioned technical problem is taken：A kind of composition is CuCrFeNiTi
High entropy alloy material preparation method, it is characterised in that be specifically realized by the following steps：
First, it is ultrasonically treated：Cu materials, Cr materials, Fe materials, Ni materials and Ti materials are placed in container, add acetone
Solution, 15~30min of cleaning in sonicator is placed on, pours into ethanol after concussion again and repeat identical step once, so
After be placed in 45 DEG C of drying bakers and carry out drying 5~6 hours, Cu materials, Cr materials, Fe materials after obtained supersound process,
Ni materials and Ti materials.
2nd, weighing：Each material after the supersound process obtained according to equimolar than carrying out weighing step 1；
3rd, melting：Using vacuum non-consumable electrode arc melting stove molten alloy, at the ultrasound for 1. weighing step 2
Material after reason is placed sequentially in peripheral water jacketed copper crucible from the bottom up by the principle of fusing point from low to high, and by pure titanium grain
It is placed in most middle water jacketed copper crucible, placement closes fire door after finishing, and tightens sample room closing knob.2. to sample
Room vacuumizes, when vacuum reaches 5 × 10-3After Pa, be re-filled with purity for 99.99% argon gas until furnace pressure reaches half
Atmospheric pressure, and repeat this step 2~3 time；The purpose that repetition vacuumizes is gas washing, and charge and discharge argon gas causes in smelting furnace repeatedly
Air as far as possible be minimized；Charge and discharge argon gas reaches half of atmospheric pressure until furnace pressure after 3. vacuum exhausts, now just
Melting can be proceeded by；First by the pure titanium grain in melting pond under the conditions of melting electric current is 70A~120A before melting sample
Melting 2~3 times, each smelting time are 120s or so, it is therefore an objective to as far as possible that the oxygen remained in stove is depleted；4. molten
Cu materials, Cr materials, Fe materials after the supersound process that refining electric current is weighed in melting step two under the conditions of being 70A~120A,
Ni materials and Ti materials 120s or so, overturn after alloy block cooling, repeat this operation 4~5 times, furnace cooling, obtain
CuCrFeNiTi high-entropy alloys.
The beneficial effects of the present invention are：
1. compared with conventional crystal material, CuCrFeNiTi high-entropy alloys of the invention by simple face-centred cubic structure,
The solid solution of body-centered cubic structure and laves phase compositions, not occurring the complicated phase such as intermetallic compound, alloy structure is uniform, and
High hardness and strong corrosion resistance are shown, the microhardness of the high-entropy alloy is 586.4HV.Application prospect is wider
It is wealthy.
2. the invention provides a kind of preparation method of CuCrFeNiTi high-entropy alloys, melted using high vacuum alloy electric arc
Prepared by refining, preparation method is simple and reliable.
Brief description of the drawings
Fig. 1 is the CuCrFeNiTi high-entropy alloy XRD spectrums of the present invention；
Fig. 2 is CuCrFeNiTi high-entropy alloys SEM (SEM) photo of the present invention；
Fig. 3 is the CuCrFeNiTi high-entropy alloys of the present invention in 0.5M H2SO4Solution and 3.5%NaCl
Polarization curve in solution.
Embodiment
Illustrate the preparation method and processing performance of the present invention, those skilled in the art by particular specific embodiment below
Advantages of the present invention and effect can comprehensively be understood by content disclosed in the present specification.
1st, CuCrFeNiTi high-entropy alloys composition design.
A kind of CuCrFeNiTi high-entropy alloys in present embodiment are made up of five kinds of elements of Cu, Cr, Fe, Ni and Ti
, wherein, Cu:Cr:Fe:Ni:Ti mol ratio is followed successively by 1:1:1:1:1.
2nd, CuCrFeNiTi high entropy alloy materials select.
The purity of Cu materials, Cr materials, Fe materials, Ni materials and Ti materials that the high-entropy alloy uses is not less than
99.7%, the form using raw material is sheet, bulk or large grained in addition to powdered.
3rd, CuCrFeNiTi method for preparing high-entropy alloy.
A kind of preparation method of CuCrFeNiTi high-entropy alloys of present embodiment, preparation process are as follows：
(1) it is ultrasonically treated：Cu materials, Cr materials, Fe materials, Ni materials and Ti materials are placed in container, add acetone
Solution, 15~30min of cleaning in sonicator is placed on, pours into absolute ethyl alcohol after concussion again and repeat identical step 1
It is secondary, it is subsequently placed in 45 DEG C of drying bakers and carries out drying 5~6 hours, Cu materials, Cr materials, Fe after obtained supersound process
Material, Ni materials and Ti materials.
(2) weighing：Cu materials, Cr materials, Fe after the supersound process obtained according to equimolar than carrying out weighing step 1
Material, Ni materials and Ti materials；
(3) melting：Using vacuum non-consumable electrode electric arc furnace molten alloy, after the supersound process for 1. weighing step 2
Material is placed sequentially in peripheral water jacketed copper crucible from the bottom up by the principle of fusing point from low to high, and pure titanium grain is placed on
In most middle water jacketed copper crucible, placement closes fire door after finishing, and tightens sample room closing knob.2. sample room is taken out very
Sky, when vacuum reaches 5 × 10-3After Pa, be re-filled with purity for 99.99% argon gas until furnace pressure reaches half of air
Pressure, and repeat this step 2~3 time；Charge and discharge argon gas reaches half of atmospheric pressure until furnace pressure after 3. vacuum exhausts, now
Melting can be proceeded by；By the pure titanium grain in melting pond in melting electric current it is first 70A~120A conditions before melting sample
Lower melting 2~3 times, each smelting time are 120s or so；4. the melting step two under the conditions of melting electric current is 70A~120A
Cu materials, Cr materials, Fe materials, Ni materials and Ti materials 120s after the supersound process of weighing or so, after alloy block cooling
Overturn, to make raw material be sufficiently mixed uniformly, repeat this operation 4~5 times, opened after alloy cools to room temperature with the furnace
Non-consumable vacuum arc melting furnace takes out sample, obtains CuCrFeNiTi high-entropy alloy ingot castings.
4th, the institutional framework of CuCrFeNiTi high-entropy alloys and performance evaluation
(1) CuCrFeNiTi high-entropy alloys SEM microstructures and XRD analysis
The high-entropy alloy ingot casting of acquisition is cut into 5mm × 5mm × 10mm cuboid sample using wire cutting, will be obtained
The sample obtained is carried out with varigrained sand paper 180#, 360#, 600#, 800#, 1000#, 1200#, 1500# and 2000# successively
Grinding, reuses diamond paste and is polished in polishing machine, the sample after being polished, reuse X-ray diffractometer
(XRD) crystal species analysis is carried out to the sample after polishing, Cu is as radiation source, graphite monochromator, operating voltage 40kV, electric current
250mA, rotation target.8 °/min of sweep speed, selection diffraction angular region are 2 θ=5-90 °.Utilize the softwares point of MDI-Jade 6.0
Experimental data is analysed, determines thing phase.Microstructure observation and composition point are carried out to the sample after polishing using SEM
Analysis EDS is analyzed, and is mainly imaged using backscattered electron.
Fig. 1 show the XRD spectrum of CuCrFeNiTi high-entropy alloys, it can be seen that the high entropys of CuCrFeNiTi close
The main composition of gold is mutually body-centered cubic structure solid solution phase (BCC) and face-centred cubic structure solid solution phase (FCC), from XRD
Analyzed in spectrum, CuCrFeNiTi high-entropy alloys do not form numerous intermetallic compound, and this is mainly mixed by its height
Close what entropy characteristic determined.Fig. 2 show CuCrFeNiTi high-entropy alloy backscattered electron images, as can be seen from the figure the conjunction
Payment organization is by dendrite (black region C and gray area B in such as Fig. 2) and branch intergranular (white portion A in such as Fig. 2) tissue
Composition.
(2) the microsclerometry of CuCrFeNiTi high-entropy alloys and analysis
By the sample after above-mentioned polishing, its hardness is tested using HZr-1000 type microhardness testers, the microhardness testers
Test force is 9.807N (1kgf), loads 15s.Sample chooses 9 diverse locations and measures its microhardness, removes maximum hardness
Value and lowest hardness value, take the mean values of remaining hardness number to finally give the alloy as the microhardness value of the sample
Microhardness value is 586.4HV.
(3) the test and analysis of the corrosion resisting property of CuCrFeNiTi high-entropy alloys
The high-entropy alloy ingot casting of acquisition is cut into 5mm × 5mm × 6mm and 5mm × 5mm × 10mm's using wire cutting
Cuboid sample, by the sample of acquisition successively with varigrained sand paper 180#, 360#, 600#, 800#, 1000#, 1200#,
1500# and 2000# are ground, and are reused diamond paste and are polished in polishing machine, the sample after being polished.Will
Sample after polishing is placed in a reservoir, adds absolute ethyl alcohol, is placed on 15~30min of cleaning in sonicator, then
It is placed in 50 DEG C of drying bakers and carries out drying 3 hours, then weighed, it is 0.5MH that sample is invaded to concentration respectively afterwards2SO4With
3.5wt%NaCl solution 10 days, the front and rear weight change of analysis corrosion, table 1 are invaded bubble for CuCrFeNiTi high-entropy alloys and existed
0.5MH2SO4With the 3.5wt%NaCl solution mass change of 10 days.Using model CS2350 electrochemical workstation to polishing
Sample afterwards carries out electrochemistry test, studies the high-entropy alloy in 0.5MH2SO4Corrosion in solution and 3.5wt%NaCl solution
Behavior, Fig. 3 are CuCrFeNiTi high-entropy alloys in 0.5MH2SO4Potentiodynamic polarization in solution and 3.5wt%NaCl solution is bent
Line.
CuCrFeNiTi high-entropy alloys are in 0.5MH as can be seen from Table 12SO4Corrode in solution and 3.5wt%NaCl solution
Front and rear mass change very little, and several no changes in surface of alloy.From figure 3, it can be seen that the alloy is in 0.5MH2SO4Solution and
Corrosion potential in 3.5wt%NaCl solution is more or less the same, but the alloy is in 0.5MH2SO4Corrosion electric current density ratio in solution
Big two orders of magnitude of corrosion electric current density in 3.5wt%NaCl solution, therefore, the alloy is in 3.5wt%NaCl solution
In corrosive nature ratio in 0.5MH2SO4Corrosive nature in solution will get well, and this is consistent with the result of table 1.Show the application
The CuCrFeNiTi high-entropy alloys of preparation have excellent decay resistance.
The CuCrFeNiTi high-entropy alloys of table 1 invade bubble in 0.5MH2SO4With the 3.5wt%NaCl solution mass change of 10 days
Claims (3)
- A kind of 1. high entropy alloy material, it is characterised in that：The high-entropy alloy composition is CuCrFeNiTi, wherein, Cu:Cr:Fe: Ni:Ti mol ratio is followed successively by 1:1:1:1:1.
- A kind of 2. preparation method of high-entropy alloy, it is characterised in that Cu materials, Cr materials, Fe materials described in claim 1, The purity of Ni materials and Ti materials is not less than 99.7%.
- A kind of 3. preparation method of high-entropy alloy, it is characterised in that Cu materials, Cr materials, Fe materials described in claim 1, The form of Ni materials and Ti materials is sheet, bulk or large grained in addition to powdered.
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Cited By (11)
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| CN108130470A (en) * | 2018-01-15 | 2018-06-08 | 湘潭大学 | A kind of MoNbTaZrHf high-entropy alloys and preparation method thereof |
| CN108179345A (en) * | 2018-01-31 | 2018-06-19 | 湘潭大学 | A kind of wear-resisting, anti-corrosion CrVNiHfNb high-entropy alloys and preparation method thereof |
| CN108277418A (en) * | 2018-04-13 | 2018-07-13 | 湘潭大学 | MoNbTaTiHf high entropy alloy materials and preparation method thereof |
| CN108336062A (en) * | 2018-01-30 | 2018-07-27 | 上海电机学院 | A kind of Cu interconnecting integrated circuits high-entropy alloy diffusion impervious layer and preparation method thereof |
| CN109112385A (en) * | 2018-09-18 | 2019-01-01 | 湘潭大学 | CrCuNiFeTiMo high entropy alloy material and preparation method thereof |
| CN110629059A (en) * | 2018-06-25 | 2019-12-31 | 南京理工大学 | Heterogeneous high-entropy alloy material and preparation method thereof |
| CN111331280A (en) * | 2020-03-05 | 2020-06-26 | 西安理工大学 | High-entropy alloy preform and TA2/0Cr18Ni9 fusion welding method |
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| CN111809096A (en) * | 2020-06-23 | 2020-10-23 | 江苏理工学院 | CuNiTi series high-entropy alloy and preparation method thereof |
| CN114990413A (en) * | 2022-05-27 | 2022-09-02 | 中国科学院赣江创新研究院 | Corrosion-resistant FeCrNiCuTi high-entropy alloy and preparation method thereof |
| CN115852229A (en) * | 2022-12-20 | 2023-03-28 | 中国科学院赣江创新研究院 | Acid corrosion resistant rare earth high-entropy alloy and preparation method thereof |
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| CN108130470A (en) * | 2018-01-15 | 2018-06-08 | 湘潭大学 | A kind of MoNbTaZrHf high-entropy alloys and preparation method thereof |
| CN108336062A (en) * | 2018-01-30 | 2018-07-27 | 上海电机学院 | A kind of Cu interconnecting integrated circuits high-entropy alloy diffusion impervious layer and preparation method thereof |
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| CN109112385A (en) * | 2018-09-18 | 2019-01-01 | 湘潭大学 | CrCuNiFeTiMo high entropy alloy material and preparation method thereof |
| CN111331280B (en) * | 2020-03-05 | 2022-01-07 | 西安理工大学 | High-entropy alloy preform and TA2/0Cr18Ni9 fusion welding method |
| CN111331280A (en) * | 2020-03-05 | 2020-06-26 | 西安理工大学 | High-entropy alloy preform and TA2/0Cr18Ni9 fusion welding method |
| CN111690863A (en) * | 2020-06-17 | 2020-09-22 | 江苏理工学院 | High-hardness Cr-Cu-Fe-Ni-V high-entropy alloy and preparation method thereof |
| CN111690863B (en) * | 2020-06-17 | 2021-09-28 | 江苏理工学院 | High-hardness Cr-Cu-Fe-Ni-V high-entropy alloy 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 |
| CN114990413A (en) * | 2022-05-27 | 2022-09-02 | 中国科学院赣江创新研究院 | Corrosion-resistant FeCrNiCuTi high-entropy alloy and preparation method thereof |
| CN115852229A (en) * | 2022-12-20 | 2023-03-28 | 中国科学院赣江创新研究院 | Acid corrosion resistant rare earth high-entropy alloy and preparation method thereof |
| CN115852229B (en) * | 2022-12-20 | 2024-06-04 | 中国科学院赣江创新研究院 | Acid corrosion resistant rare earth high-entropy alloy and preparation method thereof |
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