CN107034408B - A kind of high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity and preparation method thereof - Google Patents
A kind of high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity and preparation method thereof Download PDFInfo
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- CN107034408B CN107034408B CN201710298807.1A CN201710298807A CN107034408B CN 107034408 B CN107034408 B CN 107034408B CN 201710298807 A CN201710298807 A CN 201710298807A CN 107034408 B CN107034408 B CN 107034408B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 97
- 239000000956 alloy Substances 0.000 title claims abstract description 97
- 238000009826 distribution Methods 0.000 title claims abstract description 39
- 230000002902 bimodal effect Effects 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- 229910052742 iron Inorganic materials 0.000 claims abstract description 18
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000010949 copper Substances 0.000 claims description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000007596 consolidation process Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 230000004927 fusion Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000005551 mechanical alloying Methods 0.000 description 3
- 238000003701 mechanical milling Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007786 learning performance Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
High-entropy alloy the present invention relates to a kind of matched crystallite dimension bimodal distribution of high-strength tenacity and preparation method thereof, belongs to metal material and its preparing technical field.The atomic percent of each element component is in the high-entropy alloy of the present invention：Ni:30~35%, Co:10~30%, Fe:10~30%, Cu:12~19%, Al:1~8%, V:5~10%.Ni, Co, Fe, Cu, Al, V metal powder are fitted into ball grinder and the sealed cans in the glove box full of argon gas；Then the ball grinder of sealing is positioned on ball mill and carries out high-energy ball milling, obtain high-entropy alloy powder；Discharge plasma sintering is finally carried out to high-entropy alloy powder obtained by ball milling, the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity is made after consolidation.High-entropy alloy prepared by the present invention shows excellent comprehensive mechanical property, there is higher intensity and good plasticity simultaneously, and its preparation process is simple, cost is relatively low, and tissue, performance are stablized, therefore have broad application prospects in structural timber field.
Description
Technical field
High-entropy alloy the present invention relates to a kind of matched crystallite dimension bimodal distribution of high-strength tenacity and preparation method thereof belongs to
In metal material and its preparing technical field.
Background technology
Conventional alloys are typically based on one or two kinds of essential elements, by add one or more of a small amount of other elements come
The microscopic structure of alloy is adjusted, to reach certain specific performance requirement.It can be opened however, this design concept seriously limits
The quantity of the alloy system of hair, it is impossible to meet the increasingly increased production of people and scientific research demand.Until 2004, Taiwan's scholars leaf
Luxuriant et al. the thinking set for courageously breaching conventional alloys, takes the lead in proposing a kind of completely new alloy system, i.e. " more high entropys of pivot
Alloy " is referred to as " high-entropy alloy ".Such novel alloy includes at least five kinds of essential elements, and the atom hundred of each component
Divide ratio between 5% to 35%.More pivot characteristics of high-entropy alloy can inhibit the generation of the complicated phase such as intermetallic compound, favorably
In solid solution phase of the formation with simple crystal structure (such as FCC, BCC or HCP structure).Due to abnormal with high entropic effect, lattice
Change effect, sluggish diffusion effect and cocktail effect these typical features, high-entropy alloy typically exhibit excellent mechanics and
Physical property, such as high intensity, high rigidity, good thermal stability, corrosion-resistant, anti-oxidant and excellent magnetic property.Therefore,
High-entropy alloy is a kind of new structural material and functional material having a high potential.
The method of high-entropy alloy is prepared numerous, the application of fusion casting is then the most extensively.This method is in high vacuum argon
It under gas shielded environment, is heated by electrode discharge striking, alloying occurs after making high purity metal melting sources, after melting
Sample solidifies under the cooling effect of water cooled copper mould, that is, obtains high-entropy alloy.However, since smelting temperature is generally higher, and
Cooldown rate is limited when molten metal solidifies in copper mold, and therefore, the high-entropy alloy that this method is prepared usually has coarse
The microscopic structure of columnar dendrite or isometric dendrite, and its crystallite dimension is between tens microns to hundreds of microns.In consideration of it,
Though high-entropy alloy prepared by fusion casting shows excellent plasticity, intensity is generally relatively low.For example, prepared by fusion casting
The compression yield strength of CoNiFeCrCu alloys is only 230MPa, and its plastic strain then higher than 50.2% (X.F.Wang,
Y.Zhang,Y.Qiao,G.L.Chen,Intermetallics 15(2007)357-362).Since comprehensive mechanical property is universal
It is poor, thus high-entropy alloy prepared by fusion casting can not meet the needs of as structural timber.
To high-entropy alloy is enable to be provided simultaneously with higher intensity and good plasticity, that is, show high strong plasticity
Match, a kind of feasible effective method is exactly the microscopic structure by adjusting high-entropy alloy, and it is double to make it have suitable crystallite dimension
Peak is distributed.This is because：In deformation process, fine grained region in bimodal distribution tissue is since crystallite dimension is tiny, grain boundary area
It is larger, the effect of significant intercrystalline strengthening can be generated, so as to improve the intensity of alloy；In addition, larger-size crystalline substance in coarse grain zone
Grain has work hardening capacity, tunable deformation, so as to which alloy be made to show certain plasticity.Up to the present, although having
Researcher has been prepared bimodal with crystallite dimension by mechanical alloying (MA) with reference to discharge plasma sintering (SPS) technology
The high-entropy alloy of distribution, but since coarse grain zone and fine grained region proportion be improper in high-entropy alloy microscopic structure and coarse-grain
The problems such as area's average grain size is smaller, therefore these high-entropy alloys with bimodal distribution reported remain strong modeling
Property matching it is undesirable the problem of.Such as CoCrFeNiAl alloys prepared by " MA+SPS " method, due to its bimodal point
Crystallite dimension ＜ 50nm in fine grained region in the microscopic structure of cloth, and coarse grain zone crystallite dimension is~200nm, therefore the high-entropy alloy table
Reveal poor strength plastic's matching, compression yield strength is~1250MPa, and plastic strain be only 11.16% (W.Ji,
Z.Fu,W.Wang,H.Wang,J.Zhang,Y.Wang,F.Zhang,Journal of Alloys and Compounds,589
(2014)61-66)。
Invention content
Obdurability the purpose of the present invention is to solve high-entropy alloy in the prior art matches the problem of poor, provides one
High-entropy alloy of the kind matched crystallite dimension bimodal distribution of high-strength tenacity and preparation method thereof.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity, including：Nickel, cobalt, iron, copper, aluminium and vanadium；
The atomic percent of each component is：Ni:30~35%, Co:10~30%, Fe:10~30%, Cu:12~19%, Al:1~
8%, V:5~10%.
In the high-entropy alloy, the atomic percent preferred value of each component is：Ni:30%, Co:20%, Fe:20%, Cu:
14~18%, Al:2~6%, V:10%, and each component atomic percent summation is 100%.
A kind of preparation method of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity, is as follows：
Step 1: by atomic percent summation be 100% Ni, Co, Fe, Cu, Al, V metal powder and account for the gold
The toluene for belonging to powder gross mass 8~10% is added in the ball grinder equipped with abrading-ball, then the sealed cans in the glove box full of argon gas,
The ball grinder sealed；
Step 2: the ball grinder for the sealing that step 1 is obtained, which is packed on ball mill, carries out high-energy ball milling, obtain high entropy and close
Bronze end；
Step 3: discharge plasma sintering, sintering temperature are carried out to high-entropy alloy powder obtained by step 2：1000~1050
DEG C, heating rate：75~100 DEG C/min, apply pressure：30~50MPa, soaking time：It is tough to obtain the height by 5~10min
The high-entropy alloy of the matched crystallite dimension bimodal distribution of property.
The abrading-ball being packed into ball grinder described in step 1 is that ball material mass ratio is 10~15:1 stainless steel ball.
The rotational speed of ball-mill of high-energy ball milling described in step 2 is 300~350rpm, and total Ball-milling Time is 54~70h.
Process During High Energy Ball Milling described in step 2 is divided into two stages, and first stage ball milling duration is no less than 50h, treats first
After the completion of stage, into ball grinder, injection accounts for the absolute ethyl alcohol of tank volume 1/2 in the glove box full of argon gas, then by ball
Grinding jar body is placed on ball mill carries out second stage ball milling again.
During discharge plasma sintering described in step 3, the vacuum degree ＜ 15Pa in agglomerating plant cavity.
Grain size≤45 μm of Ni, Co, Fe, Cu, Al, V metal powder described in step 1, and purity >=99.5%.
Advantageous effect
(1) the present invention provides a kind of high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity, i.e., described height
There is the visibly different two kinds of regions of crystal particle scale in the microscopic structure of entropy alloy：Coarse grain zone and fine grained region, wherein, coarse grain zone
Occupied area percentage is 10~26%, and average grain size is 300~1000nm；Fine grained region occupied area percentage is 74
~90%, average grain size is 50~200nm.
(2) a kind of high-entropy alloy proposed by the present invention shows high strong plasticity matching, i.e., has higher intensity simultaneously
And good plasticity, yield strength are 1200~1750MPa, plastic strain is 9~38%, the excellent resultant force of the alloy
Learning performance makes it have broad application prospects in structural timber field.
(3) the present invention provides a kind of preparation sides of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity
Method, this method is simple for process, and cost is relatively low, is easy to realize in production, and the tissue of obtained high-entropy alloy, performance are steady
It is fixed.
Description of the drawings
Attached drawing 1 exists for the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity prepared by the embodiment of the present invention 1
Bright field image (TEM-BF) photo under transmission electron microscope；
Attached drawing 2 exists for the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity prepared by the embodiment of the present invention 2
Bright field image (TEM-BF) photo under transmission electron microscope；
The high-entropy alloy for the matched crystallite dimension bimodal distribution of high-strength tenacity that attached drawing 3 is prepared for the embodiment of the present invention 2
The crystallite dimension statistical distribution result of coarse grain zone and fine grained region in microscopic structure；
Attached drawing 4 exists for the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity prepared by the embodiment of the present invention 3
Bright field image (TEM-BF) photo under transmission electron microscope；
The high entropy for the matched crystallite dimension bimodal distribution of high-strength tenacity that attached drawing 5 is prepared for the embodiment of the present invention 1,2,3 closes
The room temperature quasistatic compression load-deformation curve of gold.
Specific embodiment
Present disclosure is described further with reference to embodiment, but not limited to this.
Embodiment 1：
The high-entropy alloy of the matched crystallite dimension bimodal distribution of a kind of high-strength tenacity of the present embodiment, according to each component
Atomic percent is calculated as：Ni32Co25Fe15Cu18Al2V8。
The preparation method of the high-entropy alloy of the above-mentioned matched crystallite dimension bimodal distribution of high-strength tenacity, concrete operation step is such as
Under：
(1) using commercially available purity >=99.5%, grain size≤45 μm Ni, Co, Fe, Cu, Al, V metal powder as raw material,
According to atomic percent Ni：32%th, Co：25%th, Fe：15%th, Cu：18%th, Al：2%th, V：8% accurate weighing goes out gross mass
The metal powder raw material of 50g, and be loaded into the ball grinder of dried and clean, in addition to this, also respectively according to ball material mass ratio
10:1 and mass fraction 9% toluene (the density of 500g stainless steels abrading-ball and 5ml is added into ball grinder again：0.866g/cm3),
Sealed cans are then carried out in the glove box full of argon gas；
(2) ball grinder sealed in step (1) is fitted into QM-3SP4 type planetary ball mills, then 300rpm's
Ball milling 70h in total under running speed acquires high-entropy alloy powder, and above-mentioned mechanical milling process actually carries out in two stages：
The first stage ball milling of a length of 66h when carrying out first, after treating the stage, the can opening in the glove box full of argon gas, and to
Injection accounts for the absolute ethyl alcohol of tank volume 1/2 in ball grinder, and then sealed cans, ball grinder then be again placed in carrying out on ball mill
The second stage ball milling of Shi Changwei 4h；
(3) high-entropy alloy powder obtained by step (2) is fitted into graphite jig, according to sintering temperature：1000 DEG C, heating speed
Rate：75 DEG C/min, apply pressure：50MPa, soaking time：The technological parameter of 10min carries out discharge plasma sintering, final to obtain
To the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity.
It is characterized as below to what the high-entropy alloy that the present embodiment is prepared carried out：
Fig. 1 is bright field image (TEM-BF) photo of high-entropy alloy manufactured in the present embodiment under transmission electron microscope.Fig. 1 shows：
In the microscopic structure of prepared high-entropy alloy, it is implicitly present in the visibly different two kinds of regions of crystal particle scale：Coarse grain zone and
Fine grained region.By the curve 1 in Fig. 5 it is found that under the conditions of room temperature quasistatic compression, the surrender of high-entropy alloy manufactured in the present embodiment
Intensity is 1219MPa, and plastic strain ＞ 35%, this shows that the intensity of high-entropy alloy manufactured in the present embodiment is higher and plasticity is excellent
Different, i.e., its comprehensive mechanical property is good.
Embodiment 2
The high-entropy alloy of the matched crystallite dimension bimodal distribution of a kind of high-strength tenacity of the present embodiment, according to each component
Atomic percent is calculated as：Ni30Co20Fe20Cu16Al4V10。
The preparation method of the high-entropy alloy of the above-mentioned matched crystallite dimension bimodal distribution of high-strength tenacity, concrete operation step is such as
Under：
(1) using commercially available purity >=99.5%, grain size≤45 μm Ni, Co, Fe, Cu, Al, V metal powder as raw material,
According to atomic percent Ni：30%th, Co：20%th, Fe：20%th, Cu：16%th, Al：4%th, V：10% accurate weighing goes out gross mass
The metal powder raw material of 50g, and be loaded into the ball grinder of dried and clean, in addition to this, also respectively according to ball material mass ratio
10:1 and mass fraction 9% toluene (the density of 500g stainless steels abrading-ball and 5ml is added into ball grinder again：0.866g/cm3),
Sealed cans are then carried out in the glove box full of argon gas；
(2) ball grinder sealed in step (1) is fitted into QM-3SP4 type planetary ball mills, then 300rpm's
Ball milling 70h in total under running speed acquires high-entropy alloy powder, and above-mentioned mechanical milling process actually carries out in two stages：
The first stage ball milling of a length of 66h when carrying out first, after treating the stage, the can opening in the glove box full of argon gas, and to
Injection accounts for the absolute ethyl alcohol of tank volume 1/2 in ball grinder, and then sealed cans, ball grinder then be again placed in carrying out on ball mill
The second stage ball milling of Shi Changwei 4h.
(3) high-entropy alloy powder obtained by step (2) is fitted into graphite jig, according to sintering temperature：1000 DEG C, heating speed
Rate：100 DEG C/min, apply pressure：50MPa, soaking time：The technological parameter of 6min carries out discharge plasma sintering, final to obtain
To the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity.
It is characterized as below to what the high-entropy alloy that the present embodiment is prepared carried out：
Fig. 2 is bright field image (TEM-BF) photo of high-entropy alloy manufactured in the present embodiment under transmission electron microscope.Fig. 2 is confirmed：
In the microscopic structure of prepared high-entropy alloy, it is implicitly present in the visibly different two kinds of regions of crystal particle scale：Coarse grain zone and
Fine grained region.Wherein coarse grain zone proportion is 18.13%, and fine grained region proportion is 81.87%.Fig. 3 is prepared for the present embodiment
High-entropy alloy microscopic structure in the crystallite dimension statistical distribution result of coarse grain zone and fine grained region.It can by Fig. 3 (a) and Fig. 3 (b)
, the average grain size of coarse grain zone is 542 ± 232nm in high-entropy alloy manufactured in the present embodiment, and the average crystalline substance of fine grained region
Particle size is 97 ± 44nm, this further proves that gained high-entropy alloy has crystallite dimension bimodal distribution.By the curve 2 in Fig. 5
It is found that under the conditions of room temperature quasistatic compression, the yield strength of high-entropy alloy manufactured in the present embodiment is 1504MPa, and be broken
It is 16.9% to strain, this shows that the high-entropy alloy had not only had high intensity but also showed good plasticity, i.e. its strong plasticity matching
It is higher.
Embodiment 3
The high-entropy alloy of the matched crystallite dimension bimodal distribution of a kind of high-strength tenacity of the present embodiment, according to each component
Atomic percent is calculated as：Ni33Co15Fe25Cu14Al6V7。
The preparation method of the high-entropy alloy of the above-mentioned matched crystallite dimension bimodal distribution of high-strength tenacity, concrete operation step is such as
Under：
(1) using commercially available purity >=99.5%, grain size≤45 μm Ni, Co, Fe, Cu, Al, V metal powder as raw material,
According to atomic percent Ni：33%th, Co：15%th, Fe：25%th, Cu：14%th, Al：6%th, V：7% accurate weighing goes out gross mass
The metal powder raw material of 50g, and be loaded into the ball grinder of dried and clean, in addition to this, also respectively according to ball material mass ratio
15:1 and mass fraction 9% toluene (the density of 750g stainless steels abrading-ball and 5ml is added into ball grinder again：0.866g/cm3),
Sealed cans are then carried out in the glove box full of argon gas；
(2) ball grinder sealed in step (1) is fitted into QM-3SP4 type planetary ball mills, then 350rpm's
Ball milling 54h in total under running speed acquires high-entropy alloy powder, and above-mentioned mechanical milling process actually carries out in two stages：
The first stage ball milling of a length of 50h when carrying out first, after treating the stage, the can opening in the glove box full of argon gas, and to
Injection accounts for the absolute ethyl alcohol of tank volume 1/2 in ball grinder, and then sealed cans, ball grinder then be again placed in carrying out on ball mill
The second stage ball milling of Shi Changwei 4h；
(3) high-entropy alloy powder obtained by step (2) is fitted into graphite jig, according to sintering temperature：1050 DEG C, heating speed
Rate：100 DEG C/min, apply pressure：30MPa, soaking time：The technological parameter of 8min carries out discharge plasma sintering, final to obtain
To the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity.
It is characterized as below to what the high-entropy alloy that the present embodiment is prepared carried out：
Fig. 4 is bright field image (TEM-BF) photo of high-entropy alloy manufactured in the present embodiment under transmission electron microscope.Fig. 4 is confirmed：
In the microscopic structure of prepared high-entropy alloy, it is implicitly present in the visibly different two kinds of regions of crystal particle scale：Coarse grain zone and
Fine grained region.By the curve 3 in Fig. 5 it is found that under the conditions of room temperature quasistatic compression, the surrender of high-entropy alloy manufactured in the present embodiment
Intensity is 1721MPa, and breaking strain is 9.0%, this shows that the high-entropy alloy has high intensity and suitable plasticity.
Claims (7)
1. a kind of preparation method of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity, it is characterised in that：Specifically
Step is as follows：
Step 1: by atomic percent summation be 100% Ni, Co, Fe, Cu, Al, V metal powder and account for the metal powder
The toluene of last gross mass 8~10% is added in the ball grinder equipped with abrading-ball, and then the sealed cans in the glove box full of argon gas, obtain
The ball grinder of sealing；
Step 2: the ball grinder for the sealing that step 1 is obtained, which is packed on ball mill, carries out high-energy ball milling, high-entropy alloy powder is obtained
End；
Step 3: discharge plasma sintering, sintering temperature are carried out to high-entropy alloy powder obtained by step 2：1000~1050 DEG C,
Heating rate：75~100 DEG C/min, apply pressure：30~50MPa, soaking time：5~10min obtains the high-strength tenacity
The high-entropy alloy of matched crystallite dimension bimodal distribution；
The nickel, cobalt, iron, copper, aluminium and vanadium atomic percent be：Ni:30~35%, Co:10~30%, Fe:10~30%,
Cu:12~19%, Al:1~8%, V:5~10%.
2. a kind of preparation side of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity as described in claim 1
Method, it is characterised in that：The atomic percent of the high-entropy alloy each component is：Ni:30%, Co:20%, Fe:20%, Cu:14
~18%, Al:2~6%, V:10%, and each component atomic percent summation is 100%.
3. a kind of preparation side of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity as described in claim 1
Method, it is characterised in that：The abrading-ball being packed into ball grinder described in step 1 is that ball material mass ratio is 10~15:1 stainless steel ball.
4. a kind of preparation side of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity as described in claim 1
Method, it is characterised in that：The rotational speed of ball-mill of high-energy ball milling described in step 2 is 300~350rpm, total Ball-milling Time for 54~
70h。
5. a kind of preparation of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity as described in claim 1 or 4
Method, it is characterised in that：Process During High Energy Ball Milling described in step 2 is divided into two stages, and first stage ball milling duration is no less than
50h, after the completion for the treatment of the first stage, into ball grinder, injection accounts for the anhydrous second of tank volume 1/2 in the glove box full of argon gas
Ball milling tank body is then placed on ball mill and carries out second stage ball milling again by alcohol.
6. a kind of preparation side of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity as described in claim 1
Method, it is characterised in that：During discharge plasma sintering described in step 3, the vacuum degree ＜ 15Pa in agglomerating plant cavity.
7. a kind of preparation side of the high-entropy alloy of the matched crystallite dimension bimodal distribution of high-strength tenacity as described in claim 1
Method, it is characterised in that：Grain size≤45 μm of Ni, Co, Fe, Cu, Al, V metal powder described in step 1, and purity >=99.5%.
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| CN110257686B (en) * | 2019-07-10 | 2021-05-18 | 江苏理工学院 | FeCuNiCoVAlB high-entropy alloy material and preparation method thereof |
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