CN109112385A - CrCuNiFeTiMo high entropy alloy material and preparation method thereof - Google Patents
CrCuNiFeTiMo high entropy alloy material and preparation method thereof Download PDFInfo
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- CN109112385A CN109112385A CN201811085053.2A CN201811085053A CN109112385A CN 109112385 A CN109112385 A CN 109112385A CN 201811085053 A CN201811085053 A CN 201811085053A CN 109112385 A CN109112385 A CN 109112385A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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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 wear-resisting, anti-corrosion high entropy alloy material and its technologies of preparing.High entropy alloy material ingredient is CrCuNiFeTiMo, wherein the molar ratio of Cu:Cr:Fe:Ni:Ti:Mo is successively are as follows: 1:1:1:1:1:1.Its preparation process is as follows: (1) weighing: according to equimolar than weighing each metal material；(2) molten alloy: repeated melting 4 times using the material of non-consumable vacuum arc melting furnace weighing or more.CrCuNiFeTiMo high-entropy alloy prepared by the present invention mainly forms mutually as FCC phase and a small amount of Laves phase, has many advantages, such as wear-resisting and anti-corrosion, which has a good application prospect in wear-resisting and anti-corrosion field.
Description
Technical field
The present invention relates to a kind of high entropy alloy materials and preparation method thereof, specifically, being related to a kind of wear-resisting, anti-corrosion
CrCuNiFeTiMo high-entropy alloy and preparation method thereof belongs to alloy material and its preparation technical field.
Background technique
Traditional alloy is based on a kind of metallic element (content is generally more than 50%), by adding trace alloying element
To improve alloy property, such as raising intensity, hardness, compression strength, corrosion resistance, thermal stability.But addition is excessive
Alloying element type will appear more weld metal zone brittle intermetallic thing so that the mechanical performance of alloy reduces；In addition, compound
The research of alloy structure can excessively be had adverse effect on.Therefore, traditional alloy design concept is unfavorable for alloy to mostly main
First direction is developed.
TaiWan, China scholar professor Ye Junwei breaches the traditional concept of design of material, proposes the concept of high-entropy alloy, and
Defining high-entropy alloy has simple solid solution by what 5 kind or 5 kind or more elements of the atomic percent between 5% ~ 35% formed
The alloy of body phase.Multi-principal high-entropy alloy has broken the traditional alloy design mode using a kind of alloying element as base, can pass through conjunction
Golden optimizing components design, obtaining has the tissue signatures such as microstructure simplification, nano-scaled precipitate, non crystalline structure, nanocrystal
With the alloy of the combining properties of the excellents such as high intensity, high rigidity, wear-resisting, corrosion-resistant, high temperature resistant creep, resistance to high temperature oxidation,
It can be widely used for the high-strength corrosion-resistant part on high pressure resistant, corrosion-resistant pressure vessels for the chemical industry and ship.
Summary of the invention
It is an object of the invention to develop wear-resisting, anti-corrosion high-entropy alloy --- the CrCuNiFeTiMo with excellent properties
High-entropy alloy makes it meet requirement of the people to material wear-resistant and corrosion resisting property in modern industry, so that high-entropy alloy is being answered
It is used widely with field.
The technical solution that the present invention takes to solve above-mentioned technical problem are as follows: a kind of high entropy alloy material, ingredient are
CrCuNiFeTiMo, wherein the molar ratio of Cr:Cu:Ni:Fe:Ti:Mo is successively are as follows: 1:1:1:1:1:1.
The technical solution that the present invention takes to solve above-mentioned technical problem further include: a kind of ingredient is CrCuNiFeTiMo
High entropy alloy material preparation method, it is characterised in that be specifically realized by the following steps:
1) Cu, Cr, Fe, Ni, Ti and Mo material using purity not less than 99.5% are accurately claimed according to equimolar ratio
Amount proportion, the form using raw material is sheet, bulk or large grained in addition to powdered；
2) non-consumable arc furnace molten alloy is used, the material mixing of weighing is placed in peripheral melting pond, and will be pure
Titanium grain is placed in most intermediate melting pond, and placement closes fire door after finishing, and tightens sample room closing knob；
3) sample room is vacuumized, when vacuum degree reaches 5 × 10-3After Pa, purity >=99.99% argon gas is filled with until furnace pressure
Reach half of atmospheric pressure, and repeats this step 2 ~ 3 time；The purpose that repetition vacuumizes is gas washing, and charge and discharge argon gas to melt repeatedly
Air in furnace minimizes as far as possible；
4) charge and discharge argon gas reaches half of atmospheric pressure until furnace pressure after vacuum exhausts, and can start to carry out melting at this time；?
It is as far as possible that oxygen remaining in furnace is depleted first by pure the melting of titanium grain one time in melting pond before melting sample；
5) in order to which raw material is better mixed uniformly in fusion process, after each molten alloy fusing, the electric arc retention time is 120
~ 150s is overturn after alloy block is cooling, is so repeated 4 times above；
6) melting 4 times or more stopping meltings later can pour the aluminium alloy after repetition melting according to the size shape of required product
Casting is then cooling to obtain alloy material of the present invention in mold.
The principle of the present invention and beneficial effect are:
1. the high-entropy alloy is by FCC phase and on a small quantity the present invention provides a kind of wear-resisting, anti-corrosion CrCuNiFeTiMo high-entropy alloy
Laves phase composition, alloy structure is uniform, have excellent wear-resisting, corrosion resisting property；It has broad application prospects.
2. the present invention provides a kind of preparation methods of wear-resisting, anti-corrosion CrCuNiFeTiMo high-entropy alloy, using non-consumable
Prepared by vacuum arc melting furnace smelting process, preparation method is simple and reliable, and the high-entropy alloy even tissue of acquisition is stablized.
Detailed description of the invention
Fig. 1 is the metallographic structure of the CrCuNiFeTiMo high-entropy alloy prepared in embodiment.
Specific embodiment:
Illustrate preparation method and processing performance of the invention by particular specific embodiment below, those skilled in the art can be by this
The revealed content of specification comprehensively understands advantages of the present invention and effect.
The design of 1.CrCuNiFeTiMo high-entropy alloy ingredient.
Present embodiment is a kind of CrCuNiFeTiMo high entropy conjunction being made of six kinds of elements of Cr, Cu, Ni, Fe, Ti and Mo
Gold, wherein the molar ratio of Cr:Cu:Ni:Fe:Ti:Mo is followed successively by 1:1:1:1:1:1.
The preparation of 2.CrCuNiFeTiMo high-entropy alloy.
The preparation of high-entropy alloy is a step of most critical, and preparation process is as follows:
1) raw material preparation: the alloy smelting raw material that the present invention uses is high-purity (purity is not less than 99.5%) Cr, Cu, Ni, Fe, Ti
With Mo element, the form of raw material raw material used is sheet, bulk or large grained in addition to powdered.
2) weighing: accurate weighing and proportioning Cr, Cu, Ni, Fe, Ti and Mo material is carried out according to equimolar ratio, for melting
Prepare alloy use.
3) melting prepares high-entropy alloy: 1. using non-consumable arc furnace molten alloy, the material of weighing is mixed first
Conjunction is placed in peripheral melting pond, and pure titanium grain is placed in most intermediate melting pond, and placement closes fire door after finishing, and is twisted
Close knob in tight sample room；2. being vacuumized to sample room, when vacuum degree reaches 5 × 10-3After Pa, it is filled with the argon of purity >=99.99%
Gas reaches half of atmospheric pressure until furnace pressure, and repeats this step 2 ~ 3 time；The purpose that repetition vacuumizes is gas washing, repeatedly
Charge and discharge argon gas minimizes the air in smelting furnace as far as possible；3. charge and discharge argon gas reaches until furnace pressure after vacuum exhausts
Half of atmospheric pressure can start to carry out melting at this time；First by pure the melting of titanium grain one time in melting pond before melting sample, to the greatest extent
It measures oxygen remaining in furnace is depleted；4. in order to which raw material is better mixed uniformly in fusion process, each molten alloy
After fusing, the electric arc retention time in 120 ~ 150s, is overturn after alloy block is cooling, is so repeated 4 times above；5. melting 4
The secondary above stopping melting later, opens non-consumable vacuum arc melting furnace after alloy cools to room temperature with the furnace and takes out sample, most
The CrCuNiFeTiMo high-entropy alloy ingot casting an of ellipsoid is obtained eventually；It also can be after melting completion, according to required product
Size shape can cast in the aluminium alloy after repetition melting in mold, then cooling to obtain alloy material of the present invention.
The institutional framework and performance of 3.CrCuNiFeTiMo high-entropy alloy.
1) X-ray diffraction (XRD) test and crystal species analysis
The ingot casting of acquisition is cut into 10mm × 10mm × 2mm size Rectangular samples using wire cutting, then successively by sample
It is successively carefully ground using the abrasive paper for metallograph of 800#, 1200#, 1500# and 2000#, reuses polishing machine and polished.X
X ray diffraction material phase analysis carries out on 2500 X-ray diffractometer of Rigaku Rigaku D/Max.Equipment and technology specification: make
Use Cu as radiation source, graphite monochromator operates voltage 40kV, electric current 250mA, rotation target.8 °/min of sweep speed, selection are spread out
Elevation range is 2 θ=5-90 °.Experimental data is analyzed using 6.0 software of MDI-Jade, determines object phase, as the result is shown the master of alloy
Form is mutually FCC phase and Laves phase.
2) microscopic examination
The ingot casting of acquisition is cut into 5mm × 5mm × 4mm size square sample using wire cutting, then sample is successively used
The abrasive paper for metallograph of 800#, 1200#, 1500# and 2000# are carefully ground, and are reused polishing machine and are polished.Fig. 1 is shown
The arborescent structure of CrCuNiFeTiMo high-entropy alloy.
3) microsclerometry and analysis
Ingot casting is cut into 5mm × 5mm × 4mm size square sample using wire cutting machine, then sample is successively used
The abrasive paper for metallograph of 800#, 1200#, 1500# and 2000# are carefully ground, and are reused polishing machine and are polished.Using HZr-
The hardness of 1000 type microhardness testers test samples, the test force of the microhardness testers are 9.807N (1kgf), load 15s.Examination
Sample chooses 7 different locations and measures its microhardness, removes maximum hardness value and lowest hardness value, takes being averaged for remaining hardness number
Microhardness value of the numerical value as sample, the microhardness value for finally obtaining the alloy is 625.8HV.
4) corrosion resistance measurement and analysis
The ingot casting of acquisition is cut into 10mm × 10mm × 2mm size square sample using wire cutting, then is successively used
The abrasive paper for metallograph of 800#, 1200#, 1500# and 2000# carefully grind sample, are polished after ground with polishing machine,
Sample after polishing is put into alcohol and cleans 30min with ultrasonic washing instrument, then is cleaned with deionized water, is subsequently placed in 50 DEG C of bakings
Drying 3 hours is carried out in dry case, then is weighed, and it is 0.5MH that sample is invaded to concentration respectively later2SO4And 3.5wt%NaCl
Solution 10 days, specimen surface state and weight change before and after analysis corrosion.Utilize CS350 Series Electrochemical work station and correlator
Device carries out electrochemistry test to the sample after polishing, studies the high-entropy alloy in 0.5MH2SO4Solution and 3.5wt%NaCl solution
In corrosion row.CrCuNiFeTiMo high-entropy alloy is in 0.5MH2SO4The matter of corrosion front and back in solution and 3.5wt%NaCl solution
Amount varies less, and there are few changes on the surface of alloy；The alloy is in 0.5MH2SO4Corrosion in solution and 3.5wt%NaCl solution
Current potential is not much different, but the alloy is in 0.5MH2SO4Corrosion electric current density is than the corrosion in 3.5wt%NaCl solution in solution
Big two orders of magnitude of current density, therefore, corrosive nature ratio of the alloy in 3.5wt%NaCl solution is in 0.5MH2SO4It is molten
Corrosive nature in liquid will be got well, and illustrate that this alloy has excellent corrosion resistance.
Claims (3)
1. a kind of high entropy alloy material, it is characterised in that: the high-entropy alloy ingredient is CuCrFeNiTiMo, wherein Cu:Cr:
The molar ratio of Fe:Ni:Ti:Mo is followed successively by 1:1:1:1:1:1, and phase composition is FCC phase and a small amount of Laves phase；It is described
The preparation method of CuCrFeNiTiMo high entropy alloy material, it is characterised in that be specifically realized by the following steps:
1) six kinds of metal materials of Cr, Cu, Ni, Fe, Ti and Mo are used, accurate weigh is carried out according to equimolar ratio and matches, supply
Melting prepares alloy use；
2) non-consumable arc furnace molten alloy is used, the material mixing of weighing is placed in peripheral melting pond, and will be pure
Titanium grain is placed in most intermediate melting pond, and placement closes fire door after finishing, and tightens sample room closing knob；
3) sample room is vacuumized, when vacuum degree reaches 5 × 10-3After Pa, purity >=99.99% argon gas is filled with until furnace pressure
Reach half of atmospheric pressure, and repeats this step 2 ~ 3 time；The purpose that repetition vacuumizes is gas washing, and charge and discharge argon gas to melt repeatedly
Air in furnace minimizes as far as possible；
4) charge and discharge argon gas reaches half of atmospheric pressure until furnace pressure after vacuum exhausts, and can start to carry out melting at this time；?
It is as far as possible that oxygen remaining in furnace is depleted first by pure the melting of titanium grain one time in melting pond before melting sample；
5) in order to which raw material is better mixed uniformly in fusion process, after each molten alloy fusing, the electric arc retention time is 120
~ 150s is overturn after alloy block is cooling, is so repeated 4 times above；
6) melting 4 times or more stopping meltings later can pour the aluminium alloy after repetition melting according to the size shape of required product
Casting is then cooling to obtain in mold.
2. high entropy alloy material according to claim 1, it is characterised in that Cu, Cr, Fe, Ni, Ti described in step 1) and
The purity of Mo material is not less than 99.5%.
3. high entropy alloy material according to claim 1, it is characterised in that Cu, Cr, Fe, Ni, Ti described in step 1) and
The form of Mo material is sheet, bulk or large grained in addition to powdered.
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Cited By (1)
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| 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 |
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Application publication date: 20190101 |