CN108300926A - A kind of lightweight infusibility high-entropy alloy and preparation method thereof - Google Patents

A kind of lightweight infusibility high-entropy alloy and preparation method thereof Download PDF

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CN108300926A
CN108300926A CN201810146128.7A CN201810146128A CN108300926A CN 108300926 A CN108300926 A CN 108300926A CN 201810146128 A CN201810146128 A CN 201810146128A CN 108300926 A CN108300926 A CN 108300926A
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cleaning
lightweight
purity
infusibility
entropy alloy
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肖树龙
徐丽娟
周渊飞
陈玉勇
田竟
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Harbin Institute of Technology
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Harbin Institute of Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working

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Abstract

A kind of lightweight infusibility high-entropy alloy and preparation method thereof, it is related to technical field of high-entropy, provides a kind of more pivot lightweight infusibility high-entropy alloys and preparation method thereof.Present invention aim to address existing Ni based high-temperature alloys density is big, the problem of high temperature resistance difference.A kind of nominal formula of lightweight infusibility high-entropy alloy is TiaAlbCrcNbdVe.Preparation method：One, it cleans；Two, accurate weighing；Three, melting obtains as cast condition TiaAlbCrcNbdVeLightweight infusibility high-entropy alloy；Four, it is thermally treated resulting in lightweight infusibility high-entropy alloy.Advantage：One, the problems such as current high-entropy alloy preparation is difficult, and melting loss of elements is serious, and alloy degree of purity is not high, easy tos produce segregation is solved.Two, the lightweight infusibility high-entropy alloy ingredient obtained is uniform, and has low-density, high rigidity, higher yield strength and high-temperature behavior.Present invention is mainly used for prepare lightweight infusibility high-entropy alloy.

Description

A kind of lightweight infusibility high-entropy alloy and preparation method thereof
Technical field
The present invention relates to technical field of high-entropy, a kind of more pivot lightweight infusibility high-entropy alloys and its preparation side are provided Method.
Background technology
It shares more than 30 currently, the mankind have developed the practical alloy system used and plants, most of alloys are all with a kind of metal Based on element, obtained by adding different-alloy element.And TaiWan, China scholar Ye Junwei has broken the biography of alloy design before Overall view is read, it is proposed that new alloy design concept prepares more pivot high-entropy alloys or the high randomness alloy of more pivots.
Research finds that high-entropy alloy thermodynamically has higher entropy and atom is not easy to spread, to be easy have heat There is different characteristics, performance to be better than conventional alloys for stability high solid solution phase and nanostructure, different alloys.And high entropy Alloy be one can synthesize, can process, can analyze, applicable new alloy system, there is very high research value and very Big industrial development potentiality.
Aerospace industry continues to develop in recent years, wherein increasingly harsher requirement is proposed to high-temperature structural material, Aerospace industry needs the structural material that density is small, high-temperature comprehensive property is good, and the big (density of tradition Ni based high-temperature alloys density Generally 8.0g/cm3More than), and its temperature in use is restricted already close to material limits by itself fusing point, therefore develop a kind of The Materials with High Strength of lightweight high temperature resistance is extremely urgent.
Invention content
Present invention aim to address existing Ni based high-temperature alloys density is big, the problem of high temperature resistance difference, and provide one Kind lightweight infusibility high-entropy alloy,
A kind of lightweight infusibility high-entropy alloy, its nominal formula are TiaAlbCrcNbdVe, wherein 0.5≤a≤2.0,0.5 ≤ b≤2.0,0.5≤c≤2.0,0.5≤d≤2.0,0.5≤e≤2.0.
A kind of preparation method of lightweight infusibility high-entropy alloy, is specifically realized by the following steps：
One, it cleans：With high-purity stud, titanium niobium clast, pure niobium sheet, High Pure Chromium, high-purity Al ingots, high-purity V pieces and titanium vanadium clast Then it is cleaned by ultrasonic in alcohol using mechanical means to raw material scale removal for raw material, is dried up, after obtaining cleaning High-purity V after high-purity Al ingots, cleaning after High Pure Chromium, cleaning after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning Titanium vanadium clast after piece and cleaning；
Two, weighing：It is Ti according to nominal formulaaAlbCrcNbdVeTitanium niobium after high-purity stud, cleaning after accurate weighing cleaning After clast, cleaning after pure niobium sheet, cleaning after High Pure Chromium, cleaning after high-purity Al ingots, cleaning high-purity V pieces and cleaning after titanium vanadium clast, Nominal formula is TiaAlbCrcNbdVeIn 0.5≤a≤2.0,0.5≤b≤2.0,0.5≤c≤2.0,0.5≤d≤2.0,0.5 ≤e≤2.0；
Three, melting：1., will High Pure Chromium after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning after cleaning, Titanium vanadium clast is put into dryer preheating 15min~25min, preheating after high-purity V pieces and cleaning after high-purity Al ingots, cleaning after cleaning Temperature is 50~100 DEG C, then that titanium vanadium after high-purity V pieces after High Pure Chromium, cleaning after titanium niobium clast, cleaning after cleaning and cleaning is broken Bits mixing, obtains mixture；2., high-purity stud after cleaning is put into the copper earthenware of water jacketed copper crucible vacuum induction melting furnace vertically In crucible, mixture is then poured into the surrounding in stud, then is successively placed on high-purity Al ingots after pure niobium sheet after cleaning and cleaning mixed It closes on material, fastens the fire door of water jacketed copper crucible vacuum induction melting furnace；3., in the stove of water jacketed copper crucible vacuum induction melting furnace It is vacuumized, is evacuated to 5 × 10-2Pa is hereinafter, be then charged with argon gas, until pressure is 800Pa；4., repeat step 3. Then operation 1~3 time is 60kW~70W with the speed of 5kW/min~10kW/min load power to power, until water-cooled copper earthenware Raw material all melts in crucible vacuum induction melting furnace, and continues to keep the temperature 15min~25min in the case where power is 60kW~70W, then It is 80kW~90kW with speed load power to the power of 10kW/min~20kW/min, and is protected in the case where power is 80kW~90kW Warm 3min~7min closes power and cools to room temperature with the furnace, obtains as cast condition TiaAlbCrcNbdVeLightweight infusibility high-entropy alloy；
Four, it is heat-treated：By as cast condition TiaAlbCrcNbdVeLightweight infusibility high-entropy alloy is equal at being 1000~1200 DEG C in temperature Annealing 12h~48h is homogenized, lightweight infusibility high-entropy alloy is obtained.
Advantage of the present invention：One, the present invention uses water jacketed copper crucible vacuum induction melting method, and this method solve current high entropys Alloy prepares difficult, and melting loss of elements is serious, and alloy degree of purity is not high, the problems such as easy ting produce segregation.Two, the present invention obtains light Characteristic with infusibility high-entropy alloy while matter infusibility high-entropy alloy is with low-density, the alloying component obtained by this method Uniformly, the microscopic structure of alloy is intergranular there are the equiax crystal of small second phase, and alloy density is 5.0~6.0g/cm3, hardness For 555HV~840HV, Compressive Mechanical Properties are at room temperature：σ0.2For 1400MPa~1920MPa, Compressive Mechanical Properties under high temperature For：At 750 DEG C, σ0.2=900MPa~1250MPa；At 850 DEG C, σ0.2=500MPa~950MPa；At 950 DEG C, σ0.2= 100MPa~290MPa.Therefore the obtained lightweight infusibility high-entropy alloy ingredient of the present invention is uniform, and with low-density, high rigidity, Higher yield strength and high-temperature behavior.
Description of the drawings
Fig. 1 is X ray diffracting spectrum, and 1# indicates Ti in figure1.5The X-ray diffractogram of AlCrNbV lightweight infusibility high-entropy alloys It composes, 2# indicates Ti in figure2The X ray diffracting spectrum of AlCrNbV lightweight infusibility high-entropy alloys, in figure ● indicate BBC；
Fig. 2 is Ti1.5The SEM of AlCrNbV lightweight infusibility high-entropy alloys schemes；
Fig. 3 is Ti2The SEM of AlCrNbV lightweight infusibility high-entropy alloys schemes；
Fig. 4 is Ti1.5The mechanical property figure of AlCrNbV lightweight infusibility high-entropy alloys；
Fig. 5 is Ti2The mechanical property figure of AlCrNbV lightweight infusibility high-entropy alloys.
Specific implementation mode
Specific implementation mode one：Present embodiment is a kind of lightweight infusibility high-entropy alloy, its nominal formula is TiaAlbCrcNbdVe, wherein 0.5≤a≤2.0,0.5≤b≤2.0,0.5≤c≤2.0,0.5≤d≤2.0,0.5≤e≤2.0.
A kind of microscopic structure of lightweight infusibility high-entropy alloy described in present embodiment be intergranular there are small second phase etc. Axialite, alloy density are 5.0~6.0g/cm3, hardness is 555HV~840HV, and Compressive Mechanical Properties are at room temperature：σ0.2For 1400MPa~1920MPa, Compressive Mechanical Properties are under high temperature：At 750 DEG C, σ0.2=900MPa~1250MPa；At 850 DEG C, σ0.2=500MPa~950MPa；At 950 DEG C, σ0.2=100MPa~290MPa.
Specific implementation mode two：The difference of present embodiment and specific implementation mode one is：The high entropy of lightweight infusibility The nominal formula of alloy is Ti1.5AlCrNbV.Other are same as the specific embodiment one.
Specific implementation mode three：Present embodiment and the difference of one of specific implementation mode one or two are：The lightweight The nominal formula of infusibility high-entropy alloy is Ti2AlCrNbV.Other are the same as one or two specific embodiments.
Specific implementation mode four：Present embodiment is a kind of preparation method of lightweight infusibility high-entropy alloy, specifically press with What lower step was completed：
One, it cleans：With high-purity stud, titanium niobium clast, pure niobium sheet, High Pure Chromium, high-purity Al ingots, high-purity V pieces and titanium vanadium clast Then it is cleaned by ultrasonic in alcohol using mechanical means to raw material scale removal for raw material, is dried up, after obtaining cleaning High-purity V after high-purity Al ingots, cleaning after High Pure Chromium, cleaning after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning Titanium vanadium clast after piece and cleaning；
Two, weighing：It is Ti according to nominal formulaaAlbCrcNbdVeTitanium niobium after high-purity stud, cleaning after accurate weighing cleaning After clast, cleaning after pure niobium sheet, cleaning after High Pure Chromium, cleaning after high-purity Al ingots, cleaning high-purity V pieces and cleaning after titanium vanadium clast, Nominal formula is TiaAlbCrcNbdVeIn 0.5≤a≤2.0,0.5≤b≤2.0,0.5≤c≤2.0,0.5≤d≤2.0,0.5 ≤e≤2.0；
Three, melting：1., will High Pure Chromium after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning after cleaning, Titanium vanadium clast is put into dryer preheating 15min~25min, preheating after high-purity V pieces and cleaning after high-purity Al ingots, cleaning after cleaning Temperature is 50~100 DEG C, then that titanium vanadium after high-purity V pieces after High Pure Chromium, cleaning after titanium niobium clast, cleaning after cleaning and cleaning is broken Bits mixing, obtains mixture；2., high-purity stud after cleaning is put into the copper earthenware of water jacketed copper crucible vacuum induction melting furnace vertically In crucible, mixture is then poured into the surrounding in stud, then is successively placed on high-purity Al ingots after pure niobium sheet after cleaning and cleaning mixed It closes on material, fastens the fire door of water jacketed copper crucible vacuum induction melting furnace；3., in the stove of water jacketed copper crucible vacuum induction melting furnace It is vacuumized, is evacuated to 5 × 10-2Pa is hereinafter, be then charged with argon gas, until pressure is 800Pa；4., repeat step 3. Then operation 1~3 time is 60kW~70W with the speed of 5kW/min~10kW/min load power to power, until water-cooled copper earthenware Raw material all melts in crucible vacuum induction melting furnace, and continues to keep the temperature 15min~25min in the case where power is 60kW~70W, then It is 80kW~90kW with speed load power to the power of 10kW/min~20kW/min, and is protected in the case where power is 80kW~90kW Warm 3min~7min closes power and cools to room temperature with the furnace, obtains as cast condition TiaAlbCrcNbdVeLightweight infusibility high-entropy alloy；
Four, it is heat-treated：By as cast condition TiaAlbCrcNbdVeLightweight infusibility high-entropy alloy is equal at being 1000~1200 DEG C in temperature Annealing 12h~48h is homogenized, lightweight infusibility high-entropy alloy is obtained.
The purity of high-purity stud, pure niobium sheet, High Pure Chromium, high-purity Al ingots and high-purity V pieces described in the present embodiment step 1 Not less than 99.9wt.%.
Present embodiment uses water jacketed copper crucible vacuum induction melting method, and this method solve the preparation of current high-entropy alloy is tired Difficulty, melting loss of elements is serious, and alloy degree of purity is not high, the problems such as easy ting produce segregation.
Spy with infusibility high-entropy alloy while the lightweight infusibility high-entropy alloy that present embodiment obtains is with low-density Property, the alloying component obtained by this method is uniform, and the microscopic structure of alloy is that there are the equiax crystal of small second phase for intergranular, closes Golden density is 5.0~6.0g/cm3, hardness is 555HV~840HV, and Compressive Mechanical Properties are at room temperature：σ0.2For 1400MPa~ 1920MPa, Compressive Mechanical Properties are under high temperature：At 750 DEG C, σ0.2=900MPa~1250MPa；At 850 DEG C, σ0.2=500MPa ~950MPa；At 950 DEG C, σ0.2=100MPa~290MPa.Therefore the lightweight infusibility high-entropy alloy ingredient that the present invention obtains is equal It is even, and there is low-density, high rigidity, higher yield strength and high-temperature behavior.
Specific implementation mode five：The difference of present embodiment and specific implementation mode four is：Name described in step 2 Adopted chemical formula is TiaAlbCrcNbdVeMiddle a=1.5, b=1, c=1, d=1, e=1.Other are identical as specific implementation mode four.
Specific implementation mode six：The difference of present embodiment and specific implementation mode four or five is：Described in step 2 Nominal formula be TiaAlbCrcNbdVeMiddle a=2, b=1, c=1, d=1, e=1.Other and specific implementation mode four or five It is identical.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific implementation modes Contract sample can also realize the purpose of invention.
Using following verification experimental verifications effect of the present invention
Embodiment 1：A kind of preparation method of lightweight infusibility high-entropy alloy, is specifically realized by the following steps：
One, it cleans：With high-purity stud, titanium niobium clast, pure niobium sheet, High Pure Chromium, high-purity Al ingots, high-purity V pieces and titanium vanadium clast Then it is cleaned by ultrasonic in alcohol using mechanical means to raw material scale removal for raw material, is dried up, after obtaining cleaning High-purity V after high-purity Al ingots, cleaning after High Pure Chromium, cleaning after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning Titanium vanadium clast after piece and cleaning；High-purity stud, pure niobium sheet, High Pure Chromium, high-purity Al ingots and high-purity V pieces described in step 1 it is pure Degree is not less than 99.9wt.%；
Two, weighing：It is Ti according to nominal formula1.5Titanium niobium after high-purity stud, cleaning after the cleaning of AlCrNbV accurate weighings After clast, cleaning after pure niobium sheet, cleaning after High Pure Chromium, cleaning after high-purity Al ingots, cleaning high-purity V pieces and cleaning after titanium vanadium clast；
Three, melting：1., will High Pure Chromium after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning after cleaning, Titanium vanadium clast is put into dryer and preheats 20min after high-purity V pieces and cleaning after high-purity Al ingots, cleaning after cleaning, and preheating temperature is 80 DEG C, then titanium vanadium clast after high-purity V pieces after High Pure Chromium, cleaning after titanium niobium clast, cleaning after cleaning and cleaning is mixed, is obtained Mixture；2., high-purity stud after cleaning is put into vertically in the copper crucible of water jacketed copper crucible vacuum induction melting furnace, then will Mixture pours into the surrounding in stud, then high-purity Al ingots after pure niobium sheet after cleaning and cleaning are placed on mixture successively, fastens The fire door of water jacketed copper crucible vacuum induction melting furnace；3., to being vacuumized in the stove of water jacketed copper crucible vacuum induction melting furnace, It is evacuated to 5 × 10-2Pa is hereinafter, be then charged with argon gas, until pressure is 800Pa；4., repeat step and 3. operate 2 times, then It is 60kW with speed load power to the power of 5kW/min, until raw material all melts in water jacketed copper crucible vacuum induction melting furnace, And continue to keep the temperature 20min in the case where power is 60kW, it is then 80kW with the speed of 10kW/min load power to power, and in work( Rate is that 5min is kept the temperature under 80kW, closes power and cools to room temperature with the furnace, obtains as cast condition Ti2AlCrNbV lightweight infusibility high-entropy alloys；
Four, it is heat-treated：By as cast condition Ti2Homogenizing annealing at AlCrNbV lightweight infusibility high-entropy alloys are 1200 DEG C in temperature 12h obtains lightweight infusibility high-entropy alloy.
The as cast condition Ti that 1 step 3 of embodiment is obtained2AlCrNbV lightweight infusibility high-entropy alloys use wire cutting, if cutting The sample of dry 10mm × 10mm × 5mm is respectively intended to observe under X-ray analysis test, scanning electron microscope microcosmic Tissue and micro-hardness testing.The sample that wire cutting obtains will be passed through into 200#, 320#, 600#, 1000#, 1500#, 2000# water Dry sanding paper carries out grind away, obtains the sample after having ground, the sample washes of absolute alcohol after having ground, and then carries out drainage survey Density is tried, test result is as shown in table 1 with result of calculation.
Table 1
Alloying component Calculate density Test density
Ti1.5AlCrNbV 5.62g/cm3 5.65g/cm3
Then sample washes of absolute alcohol after having ground carries out X-ray analysis test, XRD spectra such as Fig. 1 institutes Show, Fig. 1 is X ray diffracting spectrum, and 1# indicates Ti in figure1.5The X ray diffracting spectrum of AlCrNbV lightweight infusibility high-entropy alloys, figure Middle 2# indicates Ti2The X ray diffracting spectrum of AlCrNbV lightweight infusibility high-entropy alloys, in figure ● indicate BBC；The 1#XRD from Fig. 1 As can be seen that the structure for the lightweight infusibility high-entropy alloy that embodiment 1 obtains is body-centered cubic structure (BCC) on curve, meet height The characteristics of entropy alloy；For high-entropy alloy, simple solid solution phase is that composition design person is desired, based on solid solution phase Alloy can have certain intensity can also keep certain plasticity and toughness.
Sample washes of absolute alcohol after having ground, then carries out hardness test, and test result is as shown in table 2.
Table 2
Hardness It measures for the first time Second of measurement Third time measures 4th measurement Average value
Ti1.5AlCrNbV 620HV 617HV 625HV 620HV 620.5HV
Sample after having ground is mechanically polished, then uses washes of absolute alcohol, then under a scanning electron microscope Observation, as shown in Fig. 2, Fig. 2 is Ti1.5The SEM of AlCrNbV lightweight infusibility high-entropy alloys schemes；Embodiment 1 obtains as shown in Figure 2 Lightweight infusibility high-entropy alloy is typical equiax crystal, and there are the second small phase precipitation near crystal boundary, the shape of the second phase is in Strip.With increasing for Ti elements, the volume fraction of the second phase continuously decreases in alloy.
Wire cutting is used to the lightweight infusibility high-entropy alloy that embodiment 1 obtains, cuts the sample of several 6 × 9mm of Φ, it will The sample that wire cutting obtains will pass through 200#, 320#, 600#, 1000#, 1500#, 2000# silicon carbide paper and carry out grind away, will grind Sample washes of absolute alcohol afterwards carries out compression performance at being successively then 25 DEG C, 750 DEG C, 850 DEG C and 950 DEG C in temperature Test, test results are shown in figure 4, and Fig. 4 is Ti1.5The mechanical property figure of AlCrNbV lightweight infusibility high-entropy alloys；It can from Fig. 4 To find out, the compressive strength of alloy has reached 1500MPa or more at room temperature, and the compression that the increases of Ti elements reduces alloy is strong Degree, but improve the plasticity of alloy.The compressive strength of alloy can all decline with the rising of temperature at high temperature, but mould Property is obviously improved.Ti1.5AlCrNbV high-entropy alloys its yield strength at 750 DEG C is 1100MPa, and elongation percentage is 5%；At 850 DEG C, its yield strength is 667MPa, and plasticity is more than 50%.
Embodiment 2：A kind of preparation method of lightweight infusibility high-entropy alloy, is specifically realized by the following steps：
One, it cleans：With high-purity stud, titanium niobium clast, pure niobium sheet, High Pure Chromium, high-purity Al ingots, high-purity V pieces and titanium vanadium clast Then it is cleaned by ultrasonic in alcohol using mechanical means to raw material scale removal for raw material, is dried up, after obtaining cleaning High-purity V after high-purity Al ingots, cleaning after High Pure Chromium, cleaning after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning Titanium vanadium clast after piece and cleaning；High-purity stud, pure niobium sheet, High Pure Chromium, high-purity Al ingots and high-purity V pieces described in step 1 it is pure Degree is not less than 99.9wt.%；
Two, weighing：It is Ti according to nominal formula2Titanium niobium is broken after high-purity stud, cleaning after the cleaning of AlCrNbV accurate weighings Titanium vanadium clast after high-purity V pieces and cleaning after high-purity Al ingots, cleaning after High Pure Chromium, cleaning after pure niobium sheet, cleaning after bits, cleaning；
Three, melting：1., will High Pure Chromium after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning after cleaning, Titanium vanadium clast is put into dryer and preheats 20min after high-purity V pieces and cleaning after high-purity Al ingots, cleaning after cleaning, and preheating temperature is 50~100 DEG C, then titanium vanadium clast after high-purity V pieces after High Pure Chromium, cleaning after titanium niobium clast, cleaning after cleaning and cleaning is mixed It closes, obtains mixture；2., high-purity stud after cleaning is put into the copper crucible of water jacketed copper crucible vacuum induction melting furnace vertically It is interior, mixture is then poured into the surrounding in stud, then high-purity Al ingots after pure niobium sheet after cleaning and cleaning are placed on mixing successively On material, the fire door of water jacketed copper crucible vacuum induction melting furnace is fastened；3., in the stove of water jacketed copper crucible vacuum induction melting furnace into Row vacuumizes, and is evacuated to 5 × 10-2Pa is hereinafter, be then charged with argon gas, until pressure is 800Pa；4., repeat step 3. grasp Make 2 times, is then 70W with the speed of 10kW/min load power to power, until former in water jacketed copper crucible vacuum induction melting furnace Material all fusings, and continue to keep the temperature 20min in the case where power is 70W, then it is with the speed of 20kW/min load power to power 90kW, and 5min is kept the temperature in the case where power is 90kW, it closes power and cools to room temperature with the furnace, obtain as cast condition Ti2AlCrNbV lightweights are difficult Molten high-entropy alloy；
Four, it is heat-treated：By as cast condition Ti2Homogenizing annealing at AlCrNbV lightweight infusibility high-entropy alloys are 1200 DEG C in temperature 12h obtains lightweight infusibility high-entropy alloy.
The as cast condition Ti that 2 step 3 of embodiment is obtained2AlCrNbV lightweight infusibility high-entropy alloys use wire cutting, if cutting The sample of dry 10mm × 10mm × 5mm is respectively intended to observe under X-ray analysis test, scanning electron microscope microcosmic Tissue and micro-hardness testing.The sample that wire cutting obtains will be passed through into 200#, 320#, 600#, 1000#, 1500#, 2000# water Dry sanding paper carries out grind away, obtains the sample after having ground, the sample washes of absolute alcohol after having ground, and then carries out drainage survey Density is tried, test result is as shown in table 3 with result of calculation.
Table 3
Alloying component Calculate density Test density
Ti2AlCrNbV 5.52g/cm3 5.56g/cm3
Then sample washes of absolute alcohol after having ground carries out X-ray analysis test, XRD spectra such as Fig. 1 institutes Show, Fig. 1 is X ray diffracting spectrum, and 1# indicates Ti in figure1.5The X ray diffracting spectrum of AlCrNbV lightweight infusibility high-entropy alloys, figure Middle 2# indicates Ti2The X ray diffracting spectrum of AlCrNbV lightweight infusibility high-entropy alloys, in figure ● indicate BBC；The 2#XRD from Fig. 1 As can be seen that the structure for the lightweight infusibility high-entropy alloy that embodiment 2 obtains is body-centered cubic structure (BCC) on curve, meet height The characteristics of entropy alloy；For high-entropy alloy, simple solid solution phase is that composition design person is desired, based on solid solution phase Alloy can have certain intensity can also keep certain plasticity and toughness.
Sample washes of absolute alcohol after having ground, then carries out hardness test, and test result is as shown in table 4.
Table 4
Hardness It measures for the first time Second of measurement Third time measures 4th measurement Average value
Ti2AlCrNbV 557HV 550HV 557HV 555HV 554.75HV
Sample after having ground is mechanically polished, then uses washes of absolute alcohol, then under a scanning electron microscope Observation, as shown in figure 3, Fig. 3 is Ti2The SEM of AlCrNbV lightweight infusibility high-entropy alloys schemes；Embodiment 2 obtains as shown in Figure 3 Lightweight infusibility high-entropy alloy is typical equiax crystal, and there are the second small phase precipitation near crystal boundary, the shape of the second phase is in Strip.With increasing for Ti elements, the volume fraction of the second phase continuously decreases in alloy.
Wire cutting is used to the lightweight infusibility high-entropy alloy that embodiment 2 obtains, cuts the sample of several 6 × 9mm of Φ, it will The sample that wire cutting obtains will pass through 200#, 320#, 600#, 1000#, 1500#, 2000# silicon carbide paper and carry out grind away, will grind Sample washes of absolute alcohol afterwards carries out compression performance at being successively then 25 DEG C, 750 DEG C, 850 DEG C and 950 DEG C in temperature Test, test results are shown in figure 5, and Fig. 5 is Ti2The mechanical property figure of AlCrNbV lightweight infusibility high-entropy alloys；It can from Fig. 5 To find out, the compressive strength of alloy has reached 1500MPa or more at room temperature, and the compression that the increases of Ti elements reduces alloy is strong Degree, but improve the plasticity of alloy.The compressive strength of alloy can all decline with the rising of temperature at high temperature, but mould Property is obviously improved.Ti2AlCrNbV high-entropy alloys its yield strength at 750 DEG C is 1060MPa, and elongation percentage is 15%；At 850 DEG C, its yield strength is 675MPa, and plasticity is more than 50%.Fig. 4 and Fig. 5 is compared it is found that under high temperature Ti1.5AlCrNbV lightweight infusibility high-entropy alloys and Ti2The yield strength of AlCrNbV lightweight infusibility high-entropy alloys does not have apparent area Not, in 850 DEG C or more Ti2The yield strength ratio Ti of AlCrNbV lightweight infusibility high-entropy alloys1.5The high entropy of AlCrNbV lightweight infusibilities closes Gold is slightly higher.

Claims (6)

1. a kind of lightweight infusibility high-entropy alloy, it is characterised in that a kind of nominal formula of lightweight infusibility high-entropy alloy is TiaAlbCrcNbdVe, wherein 0.5≤a≤2.0,0.5≤b≤2.0,0.5≤c≤2.0,0.5≤d≤2.0,0.5≤e≤2.0.
2. a kind of lightweight infusibility high-entropy alloy according to claim 1, it is characterised in that the lightweight infusibility high-entropy alloy Nominal formula be Ti1.5AlCrNbV。
3. a kind of lightweight infusibility high-entropy alloy according to claim 1, it is characterised in that the lightweight infusibility high-entropy alloy Nominal formula be Ti2AlCrNbV。
4. a kind of preparation method of lightweight infusibility high-entropy alloy as described in claim 1, it is characterised in that a kind of lightweight infusibility The preparation method of high-entropy alloy is completed according to the following steps：
One, it cleans：It is original with high-purity stud, titanium niobium clast, pure niobium sheet, High Pure Chromium, high-purity Al ingots, high-purity V pieces and titanium vanadium clast Material, using mechanical means to raw material scale removal, is then cleaned by ultrasonic in alcohol, is dried up, high-purity after being cleaned After stud, cleaning after titanium niobium clast, cleaning after pure niobium sheet, cleaning after High Pure Chromium, cleaning after high-purity Al ingots, cleaning high-purity V pieces and Titanium vanadium clast after cleaning；
Two, weighing：It is Ti according to nominal formulaaAlbCrcNbdVeTitanium niobium is broken after high-purity stud, cleaning after accurate weighing cleaning Titanium vanadium clast, name after high-purity V pieces and cleaning after high-purity Al ingots, cleaning after High Pure Chromium, cleaning after pure niobium sheet, cleaning after bits, cleaning Adopted chemical formula is TiaAlbCrcNbdVeIn 0.5≤a≤2.0,0.5≤b≤2.0,0.5≤c≤2.0,0.5≤d≤2.0,0.5≤ e≤2.0；
Three, melting：1., will High Pure Chromium, cleaning after pure niobium sheet, cleaning after titanium niobium clast, cleaning after high-purity stud, cleaning after cleaning Titanium vanadium clast is put into dryer preheating 15min~25min, preheating temperature after high-purity V pieces and cleaning after high-purity Al ingots, cleaning afterwards It is 50~100 DEG C, then mixes titanium vanadium clast after high-purity V pieces after High Pure Chromium, cleaning after titanium niobium clast, cleaning after cleaning and cleaning It closes, obtains mixture；2., high-purity stud after cleaning is put into the copper crucible of water jacketed copper crucible vacuum induction melting furnace vertically It is interior, mixture is then poured into the surrounding in stud, then high-purity Al ingots after pure niobium sheet after cleaning and cleaning are placed on mixing successively On material, the fire door of water jacketed copper crucible vacuum induction melting furnace is fastened；3., in the stove of water jacketed copper crucible vacuum induction melting furnace into Row vacuumizes, and is evacuated to 5 × 10-2Pa is hereinafter, be then charged with argon gas, until pressure is 800Pa；4., repeat step 3. grasp Make 1~3 time, is then 60kW~70W with the speed of 5kW/min~10kW/min load power to power, until water jacketed copper crucible In vacuum induction melting furnace raw material all melt, and continue power be 60kW~70W under keep the temperature 15min~25min, then with It is 80kW~90kW that the speed of 10kW/min~20kW/min, which loads power to power, and is kept the temperature in the case where power is 80kW~90kW 3min~7min closes power and cools to room temperature with the furnace, obtains as cast condition TiaAlbCrcNbdVeLightweight infusibility high-entropy alloy；
Four, it is heat-treated：By as cast condition TiaAlbCrcNbdVeLightweight infusibility high-entropy alloy homogenizes at being 1000~1200 DEG C in temperature Anneal 12h~48h, obtains lightweight infusibility high-entropy alloy.
5. a kind of preparation method of lightweight infusibility high-entropy alloy according to claim 4, it is characterised in that institute in step 2 The nominal formula stated is TiaAlbCrcNbdVeMiddle a=1.5, b=1, c=1, d=1, e=1.
6. a kind of preparation method of lightweight infusibility high-entropy alloy according to claim 4, it is characterised in that institute in step 2 The nominal formula stated is TiaAlbCrcNbdVeMiddle a=2, b=1, c=1, d=1, e=1.
CN201810146128.7A 2018-02-12 2018-02-12 A kind of lightweight infusibility high-entropy alloy and preparation method thereof Pending CN108300926A (en)

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CN110669977A (en) * 2018-10-22 2020-01-10 南京航空航天大学 Light super-tough high-strength NbTiVAlxZry as-cast high-entropy alloy
TWI693290B (en) * 2019-11-27 2020-05-11 國立中央大學 Ti-RICH MEDIUM ENTROPY ALLOY
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CN113621863A (en) * 2021-07-21 2021-11-09 中国科学院金属研究所 Submicron precipitated phase ZrTiNbTaSn refractory high-entropy alloy and preparation method thereof
CN114350989A (en) * 2021-12-01 2022-04-15 江苏大学 Refractory Al-Cr-Ti-V-Nb light high-entropy alloy and preparation method thereof
CN115094291A (en) * 2022-06-24 2022-09-23 大连理工大学 Ti-V-Al-Cr-M series light high-strength high-entropy alloy and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110669977A (en) * 2018-10-22 2020-01-10 南京航空航天大学 Light super-tough high-strength NbTiVAlxZry as-cast high-entropy alloy
TWI693290B (en) * 2019-11-27 2020-05-11 國立中央大學 Ti-RICH MEDIUM ENTROPY ALLOY
CN112899525A (en) * 2021-01-18 2021-06-04 中国航发北京航空材料研究院 Titanium-based multi-principal-element alloy
CN113621863A (en) * 2021-07-21 2021-11-09 中国科学院金属研究所 Submicron precipitated phase ZrTiNbTaSn refractory high-entropy alloy and preparation method thereof
CN113621863B (en) * 2021-07-21 2022-06-03 中国科学院金属研究所 Submicron precipitated phase ZrTiNbTaSn refractory high-entropy alloy and preparation method thereof
CN114350989A (en) * 2021-12-01 2022-04-15 江苏大学 Refractory Al-Cr-Ti-V-Nb light high-entropy alloy and preparation method thereof
CN115094291A (en) * 2022-06-24 2022-09-23 大连理工大学 Ti-V-Al-Cr-M series light high-strength high-entropy alloy and preparation method thereof

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