CN107142410A - CrMoNbTiZr high entropy alloy materials and preparation method thereof - Google Patents
CrMoNbTiZr 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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- C22C1/00—Making non-ferrous alloys
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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 CrMoNbTiZr, wherein, Cr:Mo:Nb:Ti:Zr mol ratio is followed successively by：1:1:1:1:1.Its preparation process is as follows：（1）Powder is prepared：According to equimolar than preparing each metal dust；（2）Powder is mixed：The powder prepared is mixed in V-type and is well mixed on powder machine；（3）Briquet：By mixed powder under forcing press cold-press moulding；（4）Molten alloy：Melting is carried out to the sample of briquet using vacuum non-consumable arc-melting furnace.It is mutually BCC solid solution phases and a small amount of Laves phases that CrMoNbTiZr high-entropy alloys prepared by the present invention, which are mainly constituted, while having the advantages that hardness is high and corrosion resistance is strong.The alloy has good application prospect in wear-resisting and anti-corrosion field.
Description
Technical field
The present invention relates to a kind of high-entropy alloy and preparation method thereof, specifically, it is related to a kind of wear-resisting, anti-corrosion
CrMoNbTiZr high-entropy alloys and preparation method thereof, belong to alloy material and its preparing technical field.
Background technology
Understanding of the traditional concept to alloy property is, alloy property can be improved by adding trace alloying element and
Improve, such as improve intensity, hardness, compression strength, corrosion resistance, heat endurance, but this method is not without shortcoming,
If addition can excessively cause the even brittle complicated phase of a large amount of weld metal zone brittle intermetallic things occur so that the mechanicalness of alloy
Can reduction.In addition, compound can excessively have adverse effect on to the research of alloy structure.Therefore, for a long time, scholar is opening
All it is using a kind of alloying element as pivot during sending out novel alloy and improving alloy（Generally more than 50%）, it is few using addition
Measure alloying element and improve the method for technique, so as to obtain excellent tissue and the alloy of performance.But with present industrial work
The high speed development of journey technology, the deficiency of homogenous material performance, which has become, restricts its difficulty further developed in engineering field
Topic.Therefore research staff, which increasingly tends to develop using new and high technology, prepares high performance new material, research and development intensity,
The properties such as toughness, hardness all excellent new materials, it has also become the Main way of Material Field development.High-entropy alloy is as near
Occur over year and a kind of fast-developing novel high-strength alloy, receive the highest attention of Material Field expert.TaiWan, China
Luxuriant etc. the development framework for taking the lead in jumping out conventional alloys of the leaf of Tsing-Hua University, multicomponent high-entropy alloy was proposed in 2004 first
Design philosophy, many pivot high-entropy alloys typically have 5 kinds or more than 5 kinds of essential element, and these essential elements are with equimolar
Than or approximate equimolar than configuration.The entropy of mixing of alloy is high, in process of setting, the analysis of brittlement phase in traditional multicomponent alloy
Go out suppressed, such as intermetallic compound；The single solid solution of BCC or FCC configuration is generally formed after solidification, is greatly reduced many
The fragility of first alloy.Many pivot high-entropy alloys have broken the conventional alloys design pattern using a kind of alloying element as base, can pass through
Alloying component optimization design, obtaining has the tissue such as microstructure simplification, nano-scaled precipitate, non crystalline structure, nanocrystal special
The excellent performance group of the high intensity, high rigidity, wear-resisting, corrosion-resistant, high temperature resistant creep, high temperature oxidation resisting, resistance to temper softening etc. of seeking peace
Alloy is closed, is widely used in high pressure resistant, corrosion-resistant pressure vessels for the chemical industry and engineering high-strength corrosion-resistant part.
The content of the invention
It is an object of the invention to develop the wear-and corrosion-resistant high-entropy alloy with excellent properties --- and CrMoNbTiZr is high
Entropy alloy, makes it meet requirement of the people to material wear-resistant anti-corrosion performance in modern industry so that high-entropy alloy is led in application
It is used widely in domain.
The present invention is to solve the technical scheme taken of above-mentioned technical problem：A kind of high entropy alloy material, composition is
CrMoNbTiZr, wherein, Cr:Mo:Nb:Ti:Zr mol ratio is followed successively by：1:1:1:1:1.
The present invention also includes to solve the technical scheme that above-mentioned technical problem is taken：A kind of composition is CrMoNbTiZr's
The preparation method of high entropy alloy material, it is characterised in that be specifically realized by the following steps：
First, using metallurgical raw material Cr, Mo, Nb, Ti and Zr metal dust of purity more than 99.5%, carried out according to equimolar ratio
It is accurate to weigh proportioning, it is mixed uniform；
2nd, using pressure-like machine by the powder briquet of mixing, prepare alloy for melt and use；
3rd, using vacuum non-consumable electrode electric arc furnace molten alloy, block sample is placed in the melting groove of periphery first,
And pure titanium grain is placed in most middle melting groove, placement closes fire door after finishing, and tightens four, sample room closing knob；
4th, sample room is vacuumized, when vacuum reaches 5 × 10-3After Pa, be filled with purity for 99.99% argon gas until stove internal pressure
Power reaches half of atmospheric pressure, and repeats this step 2 ~ 3 time；The purpose that repetition is vacuumized is gas washing, and charge and discharge argon gas causes repeatedly
Air in smelting furnace, which is tried one's best, to be minimized；
5th, charge and discharge argon gas reaches half of atmospheric pressure until furnace pressure after vacuum is exhausted, and just can now proceed by melting；
First by the pure titanium grain melting one time in melting pond before melting sample, the oxygen that will be remained as far as possible in stove is depleted；
6th, in order that raw material is preferably well mixed in fusion process, after each molten alloy fusing, the electric arc retention time is 90
~ 120s, is overturn after after alloy block cooling, is so repeated 4 times the above；
7th, after melting is completed, according to the size shape of required product, the aluminium alloy repeated after melting can be cast in mould
Interior, then cooling is obtained.
The principle and beneficial effect of the present invention is：
1. the invention provides a kind of CrMoNbTiZr high-entropy alloys, the high-entropy alloy by simple structure solid solution phase and
A small amount of laves phase compositions, alloy structure is uniform, with higher hardness and excellent decay resistance, the alloy it is micro-
Hardness is up to 689HV.Have broad application prospects；
2. the invention provides a kind of preparation method of CrMoNbTiZr high-entropy alloys, carried out using high vacuum alloy electric arc melting
Prepare, preparation method is simple and reliable.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of the CrMoNbTiZr high-entropy alloys prepared in embodiment.
Fig. 2 is the scanning electron microscopy tissue of the CrMoNbTiZr high-entropy alloys prepared in embodiment.
Embodiment
Illustrate the preparation method and processing performance of the present invention by particular specific embodiment below, those skilled in the art can
Advantages of the present invention and effect are comprehensively understood by content disclosed in the present specification.
1st, CrMoNbTiZr high-entropy alloys composition design.
Present embodiment is a kind of CrMoNbTiZr high-entropy alloys being made up of five kinds of elements of Cr, Mo, Nb, Ti and Zr, its
In, Cr:Mo:Nb:Ti:Zr mol ratio is followed successively by：1:1:1:1:1.
2nd, the preparation of CrMoNbTiZr high-entropy alloys.
The preparation of high-entropy alloy is a step of most critical, and preparation process is as follows：
1）Raw material prepares：The alloy smelting raw material that the present invention is used is high-purity（Purity is more than 99.5%）Cr, Mo, Nb, Ti and Zr
Element, all dusty materials of raw material used；
2）Weigh with powder：Accurate weighing and proportioning is carried out according to molar ratio, and the dusty material after weighing is blended in one
Rise, mixed using V-type and at the uniform velocity mix 10h on powder machine；
3）Briquet：By the powder mixed on cold press with 200MPa pressure cold-press moulding, the dwell time is about 90-
120s；
4）Melting high-entropy alloy：1. vacuum non-consumable electrode electric arc furnace molten alloy is used, first block sample is placed on
In peripheral four melting grooves, and pure titanium grain is placed in most middle melting groove, placement closes fire door after finishing, and tightens sample
The closing knob of product room four；2. sample room is vacuumized, when vacuum reaches 5 × 10-3After Pa, purity is filled with for 99.99% argon gas
Until furnace pressure reaches half of atmospheric pressure, and repetition this step 2 ~ 3 time；The purpose that repetition is vacuumized is gas washing, fills repeatedly
Argon gas is put so that the air in smelting furnace is tried one's best and is minimized；3. charge and discharge argon gas reaches half until furnace pressure after vacuum is exhausted
Individual atmospheric pressure, just can now proceed by melting；First by the pure titanium grain melting one time in melting pond before melting sample, as far as possible
The oxygen remained in stove is depleted；4. in order that raw material is preferably well mixed in fusion process, each molten alloy melts
After change, the electric arc retention time, in 90 ~ 120s, is overturn after after alloy block cooling, is so repeated 4 times the above；5. melting is completed
Afterwards, non-consumable vacuum arc melting furnace is opened after alloy cools to room temperature with the furnace and takes out sample, finally give an ellipsoid
The CrMoNbTiZr high-entropy alloy ingot castings of shape.
3rd, the institutional framework and performance of CrMoNbTiZr high-entropy alloys.
1）X-ray diffraction（XRD）Test and crystal species analysis
The ingot casting of acquisition cuts into the square sample of 5mm × 5mm × 4mm sizes using wire cutting, then successively by sample successively
Carefully ground using 800#, 1200#, 1500# and 2000# abrasive paper for metallograph, reuse polishing machine and be polished.X-ray
Diffraction phase analysis are carried out on the X-ray diffractometers of Rigaku Rigaku D/Max 2500.Equipment and technology specification：Use Cu
It is used as radiation source, graphite monochromator, operating voltage 40kV, electric current 250mA, rotation target.8 °/min of sweep speed, selects the angle of diffraction
Scope is 2 θ=5-90 °.Using the software analysis experimental datas of MDI-Jade 6.0, thing phase is determined.As shown in Figure 1
The XRD test results of CrMoNbTiZr high-entropy alloys show that the main composition of CrMoNbTiZr high-entropy alloys is mutually body-centered cubic knot
Structure solid solution phase and a small amount of Laves phases.And Laves phases among these are mainly CrTi2、Mo3Nb intermetallic compounds.
2）Microscopic examination
The ingot casting of acquisition cuts into the square sample of 5mm × 5mm × 4mm sizes using wire cutting, then successively by sample successively
Carefully ground using 800#, 1200#, 1500# and 2000# abrasive paper for metallograph, reuse polishing machine and be polished.With scanning
Electron microscope observation sample tissue pattern.The cellular crystal tissue that CrMoNbTiZr high-entropy alloys are generated as shown in Figure 2.
3）Microsclerometry and analysis
The ingot casting of acquisition cuts into the square sample of 5mm × 5mm × 4mm sizes using wire cutting, then successively by sample successively
Carefully ground using 800#, 1200#, 1500# and 2000# abrasive paper for metallograph, reuse polishing machine and be polished.Using
The hardness of HZr-1000 type microhardness testers test samples, the test force of the microhardness testers is 9.807N (1kgf), loading
15s.Sample chooses 7 diverse locations and measures its microhardness, removes maximum hardness value and lowest hardness value, takes remaining hardness number
Mean values as sample microhardness value, finally give the alloy microhardness value be 689HV.
4）The decay resistance of alloy
The ingot casting of acquisition cuts into the square sample of 5mm × 5mm × 4mm sizes using wire cutting, then successively by sample successively
Carefully ground using 800#, 1200#, 1500# and 2000# abrasive paper for metallograph, reuse polishing machine and be polished.Will grinding
Polished sample is put into alcohol and 30min is cleaned with ultrasonic washing instrument, and dries weighing, afterwards by sample full immersion respectively
Concentration is 5%, 15%, 30% HNO3In solution and 3.5% NaCl solution, keep taking out after 6h, 12h, 24h, 48h, 96h,
Specimen surface state and weight change before and after analysis corrosion.
As seen from Table 1, mass change very little of the alloy in different corrosive liquids, and the surface of alloy is several without change, table
CrMoNbTiZr high-entropy alloys prepared by bright the application have excellent decay resistance.
CrMoNbTiZr high-entropy alloys are in 3.5% NaCl solution and 5%, 15%, 30% HNO3 solution in the example of table 1
Soak the mass change after 96h
| Etchant solution | 3.5%NaCl | 5%HNO3 | 15%HNO3 | 30%HNO3 |
| Quality/g before corrosion | 0.7359 | 0.6776 | 0.7663 | 0.7219 |
| Quality/g after corrosion | 0.7360 | 0.6786 | 0.7668 | 0.7210 |
| Mass change/g | 0.0001 | 0.0010 | 0.0005 | -0.0009 |
Claims (3)
1. a kind of high entropy alloy material, it is characterised in that：The high-entropy alloy composition is CrMoNbTiZr, wherein, Cr:Mo:Nb:
Ti:Zr mol ratio is followed successively by：1:1:1:1:1.
2. a kind of preparation method of high-entropy alloy, it is characterised in that the composition high-entropy alloy is prepared by the following method, the party
What method was specifically realized by the following steps：
First, using Cr, Mo, Nb, Ti and Zr metal dust, carry out accurate weigh according to equimolar ratio and match, be mixed
Uniformly；
2nd, using pressure-like machine by the powder briquet of mixing, prepare alloy for melt and use；
3rd, using vacuum non-consumable electrode electric arc furnace molten alloy, block sample is placed in the melting groove of periphery first,
And pure titanium grain is placed in most middle melting groove, placement closes fire door after finishing, and tightens four, sample room closing knob；
4th, sample room is vacuumized, when vacuum reaches 5 × 10-3After Pa, be filled with purity for 99.99% argon gas until furnace pressure
Half of atmospheric pressure is reached, and repeats this step 2 ~ 3 time；The purpose that repetition is vacuumized is gas washing, and charge and discharge argon gas to melt repeatedly
Air in furnace, which is tried one's best, to be minimized；
5th, charge and discharge argon gas reaches half of atmospheric pressure until furnace pressure after vacuum is exhausted, and just can now proceed by melting；
First by the pure titanium grain melting one time in melting pond before melting sample, the oxygen that will be remained as far as possible in stove is depleted；
6th, in order that raw material is preferably well mixed in fusion process, after each molten alloy fusing, the electric arc retention time is 90
~ 120s, is overturn after after alloy block cooling, is so repeated 4 times the above；
7th, after melting is completed, according to the size shape of required product, the aluminium alloy repeated after melting can be cast in mould
Interior, then cooling is obtained.
3. the preparation method of high entropy alloy material according to claim 2, it is characterised in that Cr, Mo described in step,
The purity of the metal dusts such as Nb, Ti and Zr is more than 99.5%.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108220741A (en) * | 2018-02-14 | 2018-06-29 | 哈尔滨工业大学 | A kind of bio-medical high-entropy alloy and preparation method thereof |
| CN108220740A (en) * | 2018-01-15 | 2018-06-29 | 湘潭大学 | A kind of wear-resisting, anti-corrosion high entropy alloy material and preparation method thereof |
| CN108441744A (en) * | 2018-02-06 | 2018-08-24 | 湘潭大学 | A kind of self-lubricating antifriction wear resistant alloy material and preparation method thereof |
| CN109161776A (en) * | 2018-10-10 | 2019-01-08 | 湘潭大学 | A kind of porous high-entropy alloy of pre-alloyed CrMoNbTiZr and preparation method thereof |
| CN109252199A (en) * | 2018-11-23 | 2019-01-22 | 西安工业大学 | A kind of high entropy alloy material of surface ceramic deposition and preparation method thereof |
| CN110358964A (en) * | 2019-07-24 | 2019-10-22 | 中国科学院金属研究所 | One kind is towards nuclear power MoVNbTiCrxHigh-entropy alloy and preparation method thereof |
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| CN115505813A (en) * | 2022-09-20 | 2022-12-23 | 中国科学院兰州化学物理研究所 | B-doped high-entropy alloy wear-resistant material with multistage precipitation strengthening function and preparation method and application thereof |
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| CN108220741A (en) * | 2018-02-14 | 2018-06-29 | 哈尔滨工业大学 | A kind of bio-medical high-entropy alloy and preparation method thereof |
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| CN109252199A (en) * | 2018-11-23 | 2019-01-22 | 西安工业大学 | A kind of high entropy alloy material of surface ceramic deposition and preparation method thereof |
| WO2020118802A1 (en) * | 2018-12-10 | 2020-06-18 | 北京理工大学 | Lightweight high-entropy alloy having high strength and high plasticity and preparation method therefor |
| CN110358964B (en) * | 2019-07-24 | 2021-11-05 | 中国科学院金属研究所 | MoVNbTiCr for nuclear powerxHigh-entropy alloy and preparation method thereof |
| CN110358964A (en) * | 2019-07-24 | 2019-10-22 | 中国科学院金属研究所 | One kind is towards nuclear power MoVNbTiCrxHigh-entropy alloy and preparation method thereof |
| CN111058076A (en) * | 2019-12-30 | 2020-04-24 | 安徽工业大学 | Zr-based high-entropy alloy material and method for synthesizing porous spherical structure on surface of Zr-based high-entropy alloy |
| CN111058076B (en) * | 2019-12-30 | 2020-11-20 | 安徽工业大学 | Zr-based high-entropy alloy material and method for synthesizing porous spherical structure on surface of Zr-based high-entropy alloy |
| CN111850372A (en) * | 2020-06-23 | 2020-10-30 | 湘潭大学 | A series of FeCoCrNiW (VC)XPreparation of high-entropy alloy and precipitation strengthening process thereof |
| CN112553517A (en) * | 2020-12-04 | 2021-03-26 | 湘潭大学 | Preparation method and process of wear-resistant CrMoNiTaHfW high-entropy alloy |
| CN112553517B (en) * | 2020-12-04 | 2022-06-21 | 湘潭大学 | Preparation method and process of wear-resistant CrMoNiTaHfW high-entropy alloy |
| CN115505813A (en) * | 2022-09-20 | 2022-12-23 | 中国科学院兰州化学物理研究所 | B-doped high-entropy alloy wear-resistant material with multistage precipitation strengthening function and preparation method and application thereof |
| CN115505813B (en) * | 2022-09-20 | 2023-05-23 | 中国科学院兰州化学物理研究所 | B-doped high-entropy alloy wear-resistant material with multistage precipitation strengthening function, and preparation method and application thereof |
| CN116024480A (en) * | 2023-01-10 | 2023-04-28 | 昆明理工大学 | High-entropy alloy material and preparation method thereof |
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