CN109266945A - A kind of high tough high-entropy alloy and preparation method thereof - Google Patents

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

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CN109266945A
CN109266945A CN201811408539.5A CN201811408539A CN109266945A CN 109266945 A CN109266945 A CN 109266945A CN 201811408539 A CN201811408539 A CN 201811408539A CN 109266945 A CN109266945 A CN 109266945A
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entropy alloy
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CN109266945B (en
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陈祯
杨喜岗
张树哲
魏培
卢秉恒
张丽娟
邹亚桐
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National Institute Corp of Additive Manufacturing Xian
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Abstract

The invention discloses a kind of high tough high-entropy alloys and preparation method thereof, it is mixed by the above raw material of mass fraction, after deoxidation is dried to it, it is formed to obtain high tough high-entropy alloy using SLM technique, a kind of new non-high-strength and high-ductility multi-principal high-entropy alloy for waiting atomic ratios is obtained, it is different from existing high-entropy alloy.The molding that the irreplaceable new method for preparing alloy of conventional method, especially this method are easier to labyrinth is realized using 3D printing technique, can satisfy the demand of the fields such as Aeronautics and Astronautics complex component.The obtained tough high-entropy alloy density of height is 8.5-8.9g/cm3, tensile strength 800-830MPa, elongation after fracture 21-23%, selected alloy element is cheap, without some more expensive elements.

Description

A kind of high tough high-entropy alloy and preparation method thereof
Technical field
The invention belongs to technical field of alloy material, and in particular to a kind of high tough high-entropy alloy and preparation method thereof.
Background technique
With the fast development of the high-tech industries such as aerospace, advance automotive, the continuous renewal of material preparation technology, More stringent requirements are proposed to material property by people, and traditional material has been unable to meet the duty requirements of active service complexity.For this purpose, grinding Study carefully the chemical composition ranges that personnel constantly explored and broke through alloy, finds the novel metal structural material haveing excellent performance.High entropy closes Gold is a kind of novel alloy material, and alloy contain there are five, five or more essential elements.The alloy does not have apparent solute With point of solvent, it is considered to be a kind of super solid solution alloy, such solid solution solid solution strengthening effect is extremely strong, can be significant Improve the intensity and toughness of alloy.And the precipitation and nanocrystalline and amorphous phase appearance of a small amount of ordered phase alloy can also be played into The effect that one step is strengthened.Therefore, the excellent properties that high-entropy alloy has some conventional alloys incomparable are such as high tough, high hard Degree, high abrasion, high thermal resistance, high resistivity, resistance to high temperature oxidation, softening resistant to high temperatures.Therefore, high entropy alloy material can substantially extend The military service range of material, has obtained common concern both domestic and external.
Summary of the invention
The purpose of the present invention is to provide a kind of high tough high-entropy alloy and preparation method thereof, the alloy tools of this method preparation There is excellent mechanical property, has reached the requirement of high-strength and high ductility alloy.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of high tough high-entropy alloy, is prepared: Ni:33%~39%, Cr:16 as mass fraction by following raw material ~24%, W:7~15%, Fe:25~35%, Ti:1%~7%.
Further, use the density of high tough high-entropy alloy forming material for 8.5-8.9g/cm3, tensile strength is 800-830MPa, elongation after fracture 21-23%.
A kind of preparation method of high tough high-entropy alloy, comprising the following steps:
Step 1) is taken following raw material: Ni:33%~39%, Cr:16~24%, W:7~15%, Fe:25 by mass fraction ~35%, Ti:1%~7%；
Step 2) is prepared as alloyed spherical powder after mixing the above raw material and deoxidation is dried；
Alloyed spherical powder after dry deoxidation is less than 200ppm, cavity pressure in Ar gas shield, oxygen content by step 3) It is formed to obtain high tough high-entropy alloy using SLM technique in the environment of 0-30mbar.
Further, alloyed spherical powder purity >=99.9%, granularity are 15~53 μm.
Further, the elemental powders of Ni, Cr, W, Fe and Ti element of purity >=99.9% are matched according to constituent content Than uniformly mixing, ball milling is prepared into alloyed spherical powder；Or by Ni, Cr, W, Fe and Ti block of purity >=99.9% according to Constituent content proportion melting is prepared into bar, then bar is prepared into alloyed spherical powder with aerosolization or rotary electrode method.
Further, alloyed spherical powder obtained is placed in drying box and deoxidation is dried, wherein vacuum degree be 1 × 10-2Pa, temperature are 60~120 DEG C, and the time is 6~12h, later cooled to room temperature, and Vacuum Package saves.
Further, alloy powder made from step 2) is placed in SLM metal 3D printer powder cylinder, intracavitary is indifferent gas Body protection, Control for Oxygen Content shape cavity pressure 0-30mbar within 200ppm；Be arranged 3D printer power be 250~ 350W, scanning speed are 1500~3500mm/s, and 0~90 ° of sweep span of rotation angle is 60~90 μm, and powdering amount is 30 μm, are sent Powder amount is 80 μm, and high tough high-entropy alloy can be obtained in completion.
Compared with prior art, the invention has the following beneficial technical effects:
A kind of high tough high-entropy alloy of the present invention, the height for taking the above raw material to be prepared as mass fraction is tough, and high entropy closes Gold, the density of forming material are 8.5-8.9g/cm3, tensile strength 800-830MPa, elongation after fracture 21-23%, institute The alloy element of selection is cheap, without some more expensive elements.
A kind of preparation method of high tough high-entropy alloy of the present invention, is mixed by the above raw material of mass fraction, to its into It goes after dry deoxidation, is formed to obtain high tough high-entropy alloy using SLM technique, obtain a kind of new non-height for waiting atomic ratios Strong high tenacity multi-principal high-entropy alloy is different from existing high-entropy alloy.
Further, the irreplaceable new method for preparing alloy of conventional method is realized using 3D printing technique, especially It is the molding that this method is easier to labyrinth, can satisfy the demand of the fields such as Aeronautics and Astronautics complex component.
Detailed description of the invention
Fig. 1 is embodiment NiCrWFeTi system alloy XRD spectrum.
Fig. 2 is NiCrWFeTi system alloy SEM organization chart.
Fig. 3 is the stress-strain curve diagram of NiCrWFeTi system high-entropy alloy.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawing:
A kind of high tough high-entropy alloy is prepared by following raw material by mass fraction ratio: Ni 33%~39%, Cr 16 ~24%, W 7~15%, Fe 25~35%, Ti 1%~7%, remaining is impurity.
A kind of high tough method for preparing high-entropy alloy, comprising the following steps:
Step 1) takes following raw material: Ni:33%~39%, Cr:16~24%, W:7~15%, Fe:25 by mass fraction ~35%, Ti:1%~7%, remaining is impurity；The above raw material is mixed with as alloyed spherical powder, alloyed spherical powder is pure Degree >=99.9%, granularity are 15~53 μm；
Specifically, the elemental powders of Ni, Cr, W, Fe, Ti element of purity >=99.9% are matched according to constituent content, Even mixing, ball milling are prepared into alloyed spherical powder；Ni, Cr, W, Fe, Ti block of purity >=99.9% are matched according to constituent content It is prepared into bar than melting, then bar is prepared into alloyed spherical powder with aerosolization or rotary electrode method；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 60~120 DEG C, and the time is 6~12h；Cooled to room temperature later obtains dry high-entropy alloy powder, Vacuum Package saves；Alloy molding is carried out to the alloy powder after dry deoxidation using selective laser fusing (SLM) forming technology High tough high-entropy alloy can be obtained in preparation.
Specifically prepared using following preparation process:
Alloy powder made from step 2) is placed in SLM metal 3D printer powder cylinder by step 3), and intracavitary is inert gas Protection, Control for Oxygen Content shape cavity pressure 0-30mbar within 200ppm；
Used inert gas is He, Ar or N2；
Step 4), the power that 3D printer is arranged are 250~350W, and scanning speed is 1500~3500mm/s, rotation angle 0 ~90 ° of sweep spans are 60~90 μm, and powdering amount is 30 μm, and powder sending quantity is 80 μm；After completing alloy preparation, after waiting 2h~4h It is sampled.
Embodiment 1:
Step 1) takes following material: Ni:33, Cr:20, W:14, Fe:28, Ti:5 by mass fraction, and the above material is matched Alloyed spherical powder is made and is prepared as, >=99.9%, granularity is 15 μm to purity；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 60 DEG C, time 7h, and cooled to room temperature, Vacuum Package save later；
Alloy powder made from step 2) is placed in 3D printer powder cylinder by step 3), and cavity is vacuumized as 98ppm, Intracavitary is Ar gas shield, and wherein cavity oxygen content is 760ppm, forms chamber pressure 17mba, operating pressure 3.8bar, blowing speed Spend 950r/min；
Step 4), be arranged 3D printer power be 250W, scanning speed 1500mm/s, 30 ° of rotation angle, sweep span It is 80 μm, powdering amount is 30 μm, and powder sending quantity is 80 μm, and starting device carries out alloy preparation later,
After the completion of step 5), alloy preparation, high tough high-entropy alloy is obtained after waiting 2h.
Embodiment 2:
Following material: Ni:33, Cr:20, W:14, Fe:28, Ti:5 is taken by mass fraction, the above material is prepared and prepared For alloyed spherical powder, >=99.9%, granularity is 20 μm to purity；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 70 DEG C, time 6h, and cooled to room temperature, Vacuum Package save later；
Alloy powder made from step 2) is placed in 3D printer powder cylinder by step 3), and cavity is vacuumized as 100ppm, Intracavitary is He gas shield, and wherein cavity oxygen content is 755ppm, forms chamber pressure 17mba, operating pressure 3.9bar, blowing speed Spend 1020r/min；
Step 4), be arranged 3D printer power be 250W, scanning speed 1500mm/s, 30 ° of rotation angle, sweep span It is 80 μm, powdering amount is 30 μm, and powder sending quantity is 80 μm, and starting device carries out alloy preparation later,
After the completion of step 5), alloy preparation, high tough high-entropy alloy is obtained after waiting 2h.
Embodiment 3:
Following material: Ni:35, Cr:18, W:12, Fe:32, Ti:3 is taken by mass fraction, the above material is prepared and prepared For alloyed spherical powder, >=99.9%, granularity is 25 μm to purity；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 80 DEG C, time 8h, and cooled to room temperature, Vacuum Package save later；
Alloy powder made from step 2) is placed in 3D printer powder cylinder by step 3), and cavity is vacuumized as 97ppm, Intracavitary is Ar gas shield, and wherein cavity oxygen content is 750ppm, forms chamber pressure 19mba, operating pressure 3.8bar, blowing speed Spend 950r/min；
Step 4), be arranged 3D printer power be 250W, scanning speed 1500mm/s, 30 ° of rotation angle, sweep span It is 80 μm, powdering amount is 30 μm, and powder sending quantity is 80 μm, and starting device carries out alloy preparation later,
After the completion of step 5), alloy preparation, high tough high-entropy alloy is obtained after waiting 2h.
Embodiment 4
Following material: Ni:36, Cr:22, W:11, Fe:27, Ti:4 is taken by mass fraction, the above material is prepared and prepared For alloyed spherical powder, >=99.9%, granularity is 30 μm to purity；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 90 DEG C, time 9h, and cooled to room temperature, Vacuum Package save later；
Alloy powder made from step 2) is placed in 3D printer powder cylinder by step 3), and cavity is vacuumized as 96ppm, Intracavitary is He gas shield, and wherein cavity oxygen content is 745ppm, forms chamber pressure 18mba, operating pressure 3.9bar, blowing speed Spend 960r/min；
Step 4), be arranged 3D printer power be 250W, scanning speed 1500mm/s, 30 ° of rotation angle, sweep span It is 80 μm, powdering amount is 30 μm, and powder sending quantity is 80 μm, and starting device carries out alloy preparation later,
After the completion of step 5), alloy preparation, high tough high-entropy alloy is obtained after waiting 2h.
Embodiment 5
Step 1) takes following material: Ni:37, Cr:20, W:7, Fe:35, Ti:1 by mass fraction, and the above material is prepared And it is prepared as alloyed spherical powder, >=99.9%, granularity is 35 μm to purity；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 100 DEG C, time 10h, and cooled to room temperature, Vacuum Package save later；
Alloy powder made from step 2) is placed in 3D printer powder cylinder by step 3), and cavity is vacuumized as 95ppm, Intracavitary is Ar gas shield, and wherein cavity oxygen content is 740ppm, forms chamber pressure 17mba, operating pressure 3.8bar, blowing speed Spend 980r/min；
Step 4), be arranged 3D printer power be 250W, scanning speed 1500mm/s, 30 ° of rotation angle, sweep span It is 80 μm, powdering amount is 30 μm, and powder sending quantity is 80 μm, and starting device carries out alloy preparation later,
After the completion of step 5), alloy preparation, high tough high-entropy alloy is obtained after waiting 2h.
Embodiment 6
Step 1) takes following material: Ni:38, Cr:16, W:10, Fe:29, Ti:7 by mass fraction, and the above material is matched Alloyed spherical powder is made and is prepared as, >=99.9%, granularity is 45 μm to purity；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 110 DEG C, time 11h, and cooled to room temperature, Vacuum Package save later；
Alloy powder made from step 2) is placed in 3D printer powder cylinder by step 3), and cavity is vacuumized as 94ppm, Intracavitary is Ar gas shield, and wherein cavity oxygen content is 760ppm, forms chamber pressure 18mba, operating pressure 3.8bar, blowing speed Spend 1000r/min；
Step 4), be arranged 3D printer power be 250W, scanning speed 1500mm/s, 30 ° of rotation angle, sweep span It is 80 μm, powdering amount is 30 μm, and powder sending quantity is 80 μm, and starting device carries out alloy preparation later,
After the completion of step 5), alloy preparation, high tough high-entropy alloy is obtained after waiting 2h.
Embodiment 7
Step 1) takes following material: Ni:39, Cr:17, W:8, Fe:30, Ti:6 by mass fraction, and the above material is prepared And it is prepared as alloyed spherical powder, >=99.9%, granularity is 53 μm to purity；
Alloy powder made from step 1) is placed in drying box deoxidation is dried by step 2), wherein vacuum degree be 1 × 10-2Pa, temperature are 120 DEG C, time 12h, and cooled to room temperature, Vacuum Package save later；
Alloy powder made from step 2) is placed in 3D printer powder cylinder by step 3), and cavity is vacuumized as 93ppm, Intracavitary is N2Gas shield, wherein cavity oxygen content is 740ppm, forms chamber pressure 19mba, operating pressure 4.0bar, blowing speed Spend 1050r/min；
Step 4), be arranged 3D printer power be 250W, scanning speed 1500mm/s, 30 ° of rotation angle, sweep span It is 90 μm, powdering amount is 50 μm, and powder sending quantity is 80 μm, and starting device carries out alloy preparation later,
After the completion of step 5), alloy preparation, high tough high-entropy alloy is obtained after waiting 2h.
A kind of preparation method of high tough high-entropy alloy provided by the invention, the high entropy obtained under different technology conditions Alloy cube matherial, its performance data is as shown in table 1 and Fig. 1 to Fig. 3 after tested:
The properties of the tough high-entropy alloy of height produced by the present invention of table 1
What said above is only the result that the present invention is preferably implemented, it is noted that for those skilled in the art, Without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to guarantor of the invention Protect range.

Claims (8)

1. a kind of high tough high-entropy alloy, which is characterized in that be prepared as mass fraction by following raw material: Ni:33%~ 39%, Cr:16~24%, W:7~15%, Fe:25~35%, Ti:1%~7%.
2. a kind of high tough high-entropy alloy according to claim 1, which is characterized in that high tough high-entropy alloy forming material Density be 8.5-8.9g/cm3, tensile strength 800-830MPa, elongation after fracture 21-23%.
3. a kind of preparation method of high tough high-entropy alloy, which comprises the following steps:
Step 1) is taken following raw material by mass fraction: Ni:33%~39%, Cr:16~24%, W:7~15%, Fe:25~ 35%, Ti:1%~7%；
Step 2) is prepared as alloyed spherical powder after mixing the above raw material and deoxidation is dried；
Alloyed spherical powder after dry deoxidation is less than 200ppm, cavity pressure 0- in Ar gas shield, oxygen content by step 3) It is formed to obtain high tough high-entropy alloy using SLM technique in the environment of 30mbar.
4. a kind of high tough method for preparing high-entropy alloy according to claim 3, which is characterized in that alloyed spherical powder is pure Degree >=99.9%, granularity are 15~53 μm.
5. a kind of high tough method for preparing high-entropy alloy according to claim 3, which is characterized in that by purity >=99.9% The elemental powders of Ni, Cr, W, Fe and Ti element matched according to constituent content, uniformly mix, ball milling is prepared into spherical alloy powder End；Or Ni, Cr, W, Fe and Ti block of purity >=99.9% are prepared into bar according to constituent content proportion melting, then will Bar is prepared into alloyed spherical powder with aerosolization or rotary electrode method.
6. a kind of high tough method for preparing high-entropy alloy according to claim 3, which is characterized in that by spherical conjunction obtained Bronze end is placed in drying box and deoxidation is dried, and wherein vacuum degree is 1 × 10-2Pa, temperature be 60~120 DEG C, the time be 6~ 12h, cooled to room temperature, Vacuum Package save later.
7. a kind of high tough method for preparing high-entropy alloy according to claim 3, which is characterized in that
Alloy powder made from step 2) is placed in SLM metal 3D printer powder cylinder, intracavitary is inert gas shielding, oxygen content Control shapes cavity pressure 0-30mbar within 200ppm；The power that 3D printer is arranged is 250~350W, and scanning speed is 1500~3500mm/s, 0~90 ° of sweep span of rotation angle are 60~90 μm, and powdering amount is 30 μm, and powder sending quantity is 80 μm, are completed High tough high-entropy alloy can be obtained.
8. a kind of high tough method for preparing high-entropy alloy according to claim 3, which is characterized in that high tough high-entropy alloy The density of forming material is 8.5-8.9g/cm3, tensile strength 800-830MPa, elongation after fracture 21-23%.
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CN114799206A (en) * 2022-03-28 2022-07-29 北京科技大学 Preparation method and application of high-entropy alloy material for catalytic electrode multi-level structure

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