CN109487099A - A kind of CrVTaHfZrTi high-entropy alloy and preparation method thereof - Google Patents
A kind of CrVTaHfZrTi high-entropy alloy and preparation method thereof Download PDFInfo
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- CN109487099A CN109487099A CN201910042845.XA CN201910042845A CN109487099A CN 109487099 A CN109487099 A CN 109487099A CN 201910042845 A CN201910042845 A CN 201910042845A CN 109487099 A CN109487099 A CN 109487099A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
Abstract
The present invention relates to a kind of CrVTaHfZrTi high-entropy alloys and preparation method thereof.The ingredient of high-entropy alloy is CrVTaHfZrTi, and the molar ratio of Cr:V:Ta:Hf:Zr:Ti is followed successively by 1:1:1:1:1:1.Its preparation process is as follows: 1) being ultrasonically treated: spare after material ultrasonic treatment；2) accurate weighing: equimolar weighing material accurate in scale is pressed；3) divide crucible blowing: titanium and the material of weighing are placed in crucible；4) it cleans repeatedly: vacuumizing backlash argon gas iterative cycles clean vacuum chambers；5) multiple melting molten alloy: is carried out to material using non-consumable vacuum arc melting technique.CrVTaHfZrTi high-entropy alloy prepared by the present invention is made of the solid solution of BCC+FCC, and structure is simple, has good corrosion resistance and wearability.The alloy compensates for the deficiency of conventional alloys, can be used for corrosion-resistant and wear-resisting working condition.
Description
Technical field
The present invention relates to technical field of new material preparation, and in particular to a kind of wear-resisting, corrosion resistant CrVTaHfZrTi high entropy
Alloy and preparation method thereof.
Background technique
High-entropy alloy (High Entropy Alloy) is a kind of new alloy design concept proposed the 1990s,
Also known as high randomness alloy.It is a kind of alloy with the characteristics of Determination of multiple metal elements equimolar ratio or nearly equimolar ratio, is dashed forward
The development framework for having broken the conventional alloys based on a kind or 2 kinds of metallic elements, has thermodynamics, dynamics, structure and performance side
The four big high-entropy alloy effects that face sums up, i.e. high entropy effect, sluggish diffusion effect, distortion of lattice effect and cocktail effect.
Due to in high entropy effect thermodynamically, sluggish diffusion effect kinetically, the distortion of lattice effect in structure, performance
Cocktail effect, be easy to get structure is simple, thermal stability is high solid solution phase and nanostructure even non crystalline structure, have
The characteristics such as high-intensitive, wear-resisting, corrosion-resistant, high rigidity, resistance to temper softening.For example, can significantly be applied to production obdurability, resistance to
Mill, corrosion resistant mold and parts；Manufacture the resistant material of chemical plant, ships etc.；By various process for treating surface, it is made
High entropy alloy coating improves substrate performance.The application of high-entropy alloy is the high function of incision, high added value specific alloy Material Field
Good opportunity.Therefore, high performance high-entropy alloy is designed and prepared to have very important significance.
Summary of the invention
The present invention provide it is a kind of with corrosion-resistant and wear-resisting high-entropy alloy and preparation method thereof, with meet it is corrosion-resistant,
Application under wear-resisting working condition.
The present invention in order to solve the above problem used by technical solution are as follows: a kind of CrVTaHfZrTi high-entropy alloy, feature
It is, the group of the high-entropy alloy is divided into CrVTaHfZrTi, wherein the mol ratio of each element is 1:1:1:1:1:1；It uses
Mass percentage content, that is, purity of the materials such as Cr, V, Ta, Hf, Zr, Ti is 99.5% or more；Cr, V of use, Ta, Hf,
The materials such as Zr, Ti are sheet or large grained material.
A kind of preparation method of CrVTaHfZrTi high-entropy alloy, comprising the following steps:
1), mass percentage is set in 99.5% or more sheet or Cr, V, Ta, Hf, Zr, Ti material of large grained
It is spare after being ultrasonically treated respectively in container；
2) Cr, V, Ta, Hf, Zr, Ti material obtained in accurate weighing step 1, are carried out in equimolar ratio；
3) it, takes processed a small amount of Ti material in step 1 to be put into the intermediate crucible of water cooled copper mould, then step 2 is claimed
The material taken is placed in the several melting kettles in periphery of water cooled copper mould, in each crucible from low to high according to the fusing point of material
Principle is sequentially placed from bottom to top；
4), by the vacuum chamber inside smelting furnace to 5.0 × 10-3MPa is then charged with argon gas to 0.05MPa；Lay equal stress on
Multiple this step 2~3 time；The purpose that repetition vacuumizes is gas washing, and charge and discharge argon gas subtracts the air in smelting furnace as far as possible repeatedly
To minimum, to achieve the purpose that clean vacuum chambers；
5), first to melting after individually placed Ti material striking, it can consume, reduce remnant oxygen in smelting furnace, then
Successively Cr, V, Ta, Hf, Zr, Ti material in the other crucibles of melting to melting；By the alloy cast ingot obtained after melting by same
Method melting 3~5 times again, overturn sample after each melting, after furnace cooling, CrVTaHfZrTi high-entropy alloy is made.
Further, the method for the ultrasonic treatment in step 1) are as follows: after addition acetone floods material in container, ultrasound is clear
Wash 15~20min, the greasy dirt and impurity of the attachment of removal metal surface；Then again by Cr, V, Ta, Hf, Zr, Ti after removal impurity
Material is respectively placed in the container that dehydrated alcohol is added, and is cleaned by ultrasonic 15~20min, is subsequently placed in low temperature drying in baking oven, obtains
Cr, V, Ta, Hf, Zr, Ti material after to ultrasonic treatment.
Further, melting, smelting technology are as follows: voltage are carried out using non-consumable vacuum arc melting technique in step 5)
30~50V, electric current 200~300A, each melting 90-120s.
Compared with present technology, the present invention has the advantages that
1. the present invention provides a kind of VTiTaHfZr high-entropy alloy, the high-entropy alloy is mainly consolidated by simple BCC+FCC
Solution phase composition, alloy structure are uniform.
2. the component element density of high-entropy alloy of the invention is larger, prepared by non-consumable vacuum arc melting technique
Obdurability, corrosion-resistant and wear-resisting high entropy alloy material, make up the deficiency of conventional alloys, meet the following obdurability, it is corrosion-resistant and
Wear-resistant material application demand.The alloy has good corrosion resistance, wearability, has broad application prospects.
3. in the present invention, control melting vacuum degree, melting electric current and melting number, are prepared when alloy melting
VTiTaHfZr high-entropy alloy；Hf, Zr, Ta (refractory metal) improve Impact Toughness of Alloy advantageous.
Detailed description of the invention
Fig. 1 is that X ray diffracting spectrum Fig. 2 of the CrVTaHfZrTi high-entropy alloy prepared in embodiment is to make in embodiment
The scanning electron microscopy tissue of standby CrVTaHfZrTi high-entropy alloy
Specific embodiment
Illustrate preparation method and processing performance of the invention by particular specific embodiment below, those skilled in the art can
Other advantages and effect of the invention are comprehensively understood by content disclosed in the present specification.
The design of 1.CrVTaHfZrTi high-entropy alloy ingredient.
A kind of CrVTaHfZrTi high-entropy alloy of present embodiment is made of six kinds of elements of Cr, V, Ta, Hf, Zr and Ti,
In, the molar ratio of Cr:V:Ta:Hf:Zr:Ti is successively are as follows: 1:1:1:1:1:1；The materials such as Cr, V, Ta, Hf, Zr, Ti of use
Mass percentage content, that is, purity is 99.5% or more.
The preparation of 2.CrVTaHfZrTi high-entropy alloy.
The preparation of high-entropy alloy is a step of most critical, and preparation process is as follows.
1) it is ultrasonically treated: after addition acetone floods material in container, being cleaned by ultrasonic 15~20min, remove metal surface
The greasy dirt and impurity of attachment；Cr, V, Ta, Hf, Zr, Ti material after removal impurity are then respectively placed in addition dehydrated alcohol again
Container in, be cleaned by ultrasonic 15~20min, be subsequently placed in low temperature drying in baking oven, Cr, V, Ta, Hf after being ultrasonically treated,
Zr, Ti material；
2) weighing stock: according to equimolar ratio accurately weigh Cr, V after the ultrasonic treatment that step 1) obtains,
Ta, Hf, Zr, Ti materials for later use；
3) divide crucible blowing: processed a small amount of Ti material in step 1) being taken to be put into the intermediate crucible of water cooled copper mould, then
The weighed material of step 2) is placed in the several melting kettles in periphery of water cooled copper mould, according to the fusing point of material in each crucible
Principle from low to high is sequentially placed from bottom to top；
4) it cleans repeatedly: lock sealing smelting furnace vacuum chamber after material is put in crucible well, first by the vacuum inside smelting furnace
Room is evacuated to 5.0 × 10-3MPa is then charged with argon gas to 0.05MPa；And this step 2~3 time are repeated, with clean vacuum chambers；
5) it molten alloy: first to melting after individually placed Ti material striking, consumes, the residual oxygen in reduction smelting furnace
Gas, then successively Cr, V, Ta, Hf, Zr, Ti material in the other crucibles of melting to melting；In order to make raw material more in fusion process
It is uniformly mixed well, after each molten alloy fusing, the electric arc retention time in 90~120s, is turned over after alloy block is cooling
Turn, is so repeated 4 times above；Stop melting after melting 4 times or more, it is true that non-consumable is opened after alloy cools to room temperature with the furnace
Empty arc-melting furnace takes out sample, finally obtains the CrVTaHfZrTi high-entropy alloy ingot casting an of ellipsoid.
The institutional framework and performance of 3.CrVTaHfZrTi high-entropy alloy.
1) X-ray diffractometer (XRD) test and crystal species analysis.
The ingot casting of acquisition is cut into 10mm × 10mm × 4mm size square sample using wire cutting, then by sample according to
The secondary abrasive paper for metallograph using 600#, 800#, 1000# and 1500# is polished, and is reused diamond polishing cream and is polished.X-ray
Diffraction phase analysis carries out on Rigaku Rigaku D/Max 2500X x ray diffractometer x.Equipment and technology specification: Cu is used
As radiation source, graphite monochromator operates voltage 40kCRV, electric current 250mA, rotation target.8 °/min of sweep speed selects diffraction
Angular region is 2 θ=5-90 °.Experimental data is analyzed using MDI-Jade6.0 software, determines object phase.
As shown in Figure 1, the XRD test result of CrVTaHfZrTi high-entropy alloy shows that alloy is mainly tied by simple BCC
The solid solution phase of structure and FCC configuration composition, has preferable obdurability and corrosion resistance.
2) microscopic examination.
The ingot casting of acquisition is cut into 10mm × 10mm × 4mm size square sample using wire cutting, then by sample according to
The secondary abrasive paper for metallograph using 600#, 800#, 1000# and 1500# is polished, and is reused diamond polishing cream and is polished.With scanning
The tissue topography of electron microscope observation sample.As shown in Figure 2, the crystal grain that CrVTaHfZrTi high-entropy alloy generates is dendrite group
Knit form.
3) performance detection.
A, it is rectangular that ingot casting microsclerometry and analysis: is cut into 5mm × 5mm × 4mm size using wire cutting machine
Sample successively uses sample the abrasive paper for metallograph of 600#, 800#, 1000# and 1500# to grind, reuse diamond polishing cream into
Row polishing.Using the hardness of HZr-1000 type microhardness testers test sample, the test force of the microhardness testers is 9.807N
(1kgf) loads 15s.Sample chooses 7 different locations and measures its microhardness, removes maximum hardness value and lowest hardness value,
Take the mean values of remaining hardness number as the microhardness value of sample, the microhardness value for finally obtaining the alloy is
471.0HV。
B, the ingot casting of acquisition the corrosion resistance of alloy: is cut into 10mm × 10mm × 3mm size using wire cutting
Square sample, then successively sample is successively used the abrasive paper for metallograph of 800#, 1200#, 1500# and 2000# carefully grind, it reuses
Polishing machine is polished.The good sample of grinding and polishing is put into alcohol and cleans 30min, and dry title with ultrasonic washing instrument
Amount, by sample, the full concentration that immerses is to protect in 5%, 15%, 30% HNO3 solution and 3.5% NaCl solution respectively later
Hold 6h, 12h, for 24 hours, take out after 48h, 96h, analysis corrosion front and back specimen surface state and weight change.Alloy exists as the result is shown
Mass change very little in different corrosive liquids, and there are few changes on the surface of alloy, show the CrVTaHfZrTi high of the application preparation
Entropy alloy has excellent corrosion resistance.
Claims (6)
1. a kind of CrVTaHfZrTi high-entropy alloy, which is characterized in that mole of Cr:V:Ta:Hf:Zr:Ti in the high-entropy alloy
Than what is be specifically realized by the following steps for 1:1:1:1:1:1, preparation method:
1) mass percentage, is placed in appearance in 99.5% or more sheet or Cr, V, Ta, Hf, Zr, Ti material of large grained
It is spare after being ultrasonically treated respectively in device；
2) Cr, V, Ta, Hf, Zr, Ti material obtained in accurate weighing step 1, are carried out in equimolar ratio；
3) processed a small amount of Ti material in step 1, is taken to be put into the intermediate crucible of water cooled copper mould, then step 2 is weighed
Material is placed in the several melting kettles in periphery of water cooled copper mould, the principle in each crucible according to the fusing point of material from low to high
It is sequentially placed from bottom to top；
4), by the vacuum chamber inside smelting furnace to 5.0 × 10-3MPa is then charged with argon gas to 0.05MPa；And repeat this
Step 2 ~ 3 time；The purpose that repetition vacuumizes is gas washing, and charge and discharge argon gas reduces to the air in smelting furnace as far as possible most repeatedly
It is small, to achieve the purpose that clean vacuum chambers；
5), first to melting after individually placed Ti material striking, it can consume, reduce remnant oxygen in smelting furnace, then successively
To Cr, V, Ta, Hf, Zr, Ti material of melting in the other crucibles of melting；In the same way by the alloy cast ingot obtained after melting
Melting 3 ~ 5 times again overturn sample after each melting, after furnace cooling, CrVTaHfZrTi high-entropy alloy is made.
2. a kind of preparation method of CrVTaHfZrTi high-entropy alloy, it is characterised in that be specifically realized by the following steps:
1) mass percentage, is placed in appearance in 99.5% or more sheet or Cr, V, Ta, Hf, Zr, Ti material of large grained
It is spare after being ultrasonically treated respectively in device；
2) Cr, V, Ta, Hf, Zr, Ti material obtained in accurate weighing step 1, are carried out in equimolar ratio；
3) processed a small amount of Ti material in step 1, is taken to be put into the intermediate crucible of water cooled copper mould, then step 2 is weighed
Material is placed in the several melting kettles in periphery of water cooled copper mould, the principle in each crucible according to the fusing point of material from low to high
It is sequentially placed from bottom to top；
4), by the vacuum chamber inside smelting furnace to 5.0 × 10-3MPa is then charged with argon gas to 0.05MPa；And repeat this
Step 2 ~ 3 time；The purpose that repetition vacuumizes is gas washing, and charge and discharge argon gas reduces to the air in smelting furnace as far as possible most repeatedly
It is small, to achieve the purpose that clean vacuum chambers；
5), first to melting after individually placed Ti material striking, it can consume, reduce remnant oxygen in smelting furnace, then successively
To Cr, V, Ta, Hf, Zr, Ti material of melting in the other crucibles of melting；In the same way by the alloy cast ingot obtained after melting
Melting 3 ~ 5 times again overturn sample after each melting, after furnace cooling, CrVTaHfZrTi high-entropy alloy is made.
3. a kind of CrVTaHfZrTi high-entropy alloy according to claim 1, it is characterised in that: ultrasonic treatment in step 1)
Method are as follows: be added in container after acetone floods material, be cleaned by ultrasonic 15 ~ 20min, the greasy dirt of removal metal surface attachment and
Impurity；Then Cr, V, Ta, Hf, Zr, Ti material after removal impurity are respectively placed in the container that dehydrated alcohol is added again, surpassed
Sound cleans 15 ~ 20 min, is subsequently placed in low temperature drying in baking oven, obtains stand-by Cr, V, Ta, Hf, Zr, Ti material.
4. a kind of CrVTaHfZrTi high-entropy alloy according to claim 1, it is characterised in that: non-consumable is true in step 5)
Empty electric arc melting technique are as follows: 30 ~ 50 V of voltage, electric current 200 ~ 300 A, each melting 90-120 s.
5. a kind of preparation method of CrVTaHfZrTi high-entropy alloy according to claim 2, it is characterised in that: step 1)
The method of middle ultrasonic treatment are as follows: after addition acetone floods material in container, be cleaned by ultrasonic 15 ~ 20min, removal metal surface is attached
Greasy dirt and impurity；Then Cr, V, Ta, Hf, Zr, Ti material after removal impurity are respectively placed in again, dehydrated alcohol is added
In container, it is cleaned by ultrasonic 15 ~ 20 min, is subsequently placed in low temperature drying in baking oven, obtains stand-by Cr, V, Ta, Hf, Zr, Ti material
Material.
6. a kind of CrVTaHfZrTi high-entropy alloy according to claim 2, it is characterised in that: non-consumable is true in step 5)
Empty electric arc melting technique are as follows: 30 ~ 50 V of voltage, electric current 200 ~ 300 A, each melting 90-120 s.
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Cited By (3)
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| CN112553517A (en) * | 2020-12-04 | 2021-03-26 | 湘潭大学 | Preparation method and process of wear-resistant CrMoNiTaHfW high-entropy alloy |
| CN112553488A (en) * | 2020-12-16 | 2021-03-26 | 湘潭大学 | CrAlNbTiVZr high-entropy alloy material and preparation method thereof |
| CN117165945A (en) * | 2023-07-25 | 2023-12-05 | 中国船舶集团有限公司第七一九研究所 | Laves phase enhanced eutectic high-entropy alloy wear-resistant superhydrophobic surface and preparation method thereof |
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| CN117165945B (en) * | 2023-07-25 | 2024-03-12 | 中国船舶集团有限公司第七一九研究所 | Laves phase enhanced eutectic high-entropy alloy wear-resistant superhydrophobic surface and preparation method thereof |
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Application publication date: 20190319 |