CN109266945B - High-strength high-toughness high-entropy alloy and preparation method thereof - Google Patents

High-strength high-toughness high-entropy alloy and preparation method thereof Download PDF

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CN109266945B
CN109266945B CN201811408539.5A CN201811408539A CN109266945B CN 109266945 B CN109266945 B CN 109266945B CN 201811408539 A CN201811408539 A CN 201811408539A CN 109266945 B CN109266945 B CN 109266945B
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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 high-strength high-toughness high-entropy alloy and a preparation method thereof, wherein the high-strength high-toughness high-entropy alloy is obtained by mixing raw materials with mass fractions, drying and deoxidizing the mixture, and forming the mixture by adopting an S L M process, so that the high-strength high-toughness high-entropy alloy with a new non-equal atomic ratio is obtained, and the high-strength high-toughness high-entropy alloy is different from the existing high-entropy alloy3The tensile strength is 800-830MPa, the elongation after fracture is 21-23%, the selected alloying elements are low in price, and some expensive elements are not available.

Description

High-strength high-toughness high-entropy alloy and preparation method thereof
Technical Field
The invention belongs to the technical field of alloy materials, and particularly relates to a high-strength high-toughness high-entropy alloy and a preparation method thereof.
Background
With the rapid development of high-tech industries such as aerospace, advanced motor vehicles and the like and the continuous updating of material preparation technology, people put forward higher requirements on material performance, and the traditional material cannot meet the working condition requirements of complex active service. Therefore, researchers are continuously exploring and breaking through the range of chemical compositions of the alloy and searching for novel metal structural materials with excellent performance. The high-entropy alloy is a novel alloy material, and the alloy contains five or more main elements. The alloy has no obvious solute and solvent, is considered to be a super solid solution alloy, has extremely strong solid solution strengthening effect, and can obviously improve the strength and the toughness of the alloy. And the precipitation of a small amount of ordered phase and the appearance of nanocrystalline and amorphous phase can also play a further strengthening effect on the alloy. Therefore, the high-entropy alloy has excellent performances which cannot be compared with the traditional alloy, such as high strength and toughness, high hardness, high wear resistance, high thermal resistance, high resistivity, high-temperature oxidation resistance and high-temperature softening resistance. Therefore, the high-entropy alloy material can greatly expand the service range of the material and get general attention at home and abroad.
Disclosure of Invention
The invention aims to provide a high-strength high-toughness high-entropy alloy and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-strength, high-toughness and high-entropy alloy is prepared from the following raw materials in parts by mass: ni: 33% -39%, Cr: 16-24%, W: 7-15%, Fe: 25-35%, Ti: 1 to 7 percent.
Furthermore, the density of the material formed by adopting the high-strength high-toughness high-entropy alloy is 8.5-8.9g/cm3The tensile strength is 800-830MPa, and the elongation after fracture is 21-23%.
A preparation method of a high-strength, high-toughness and high-entropy alloy comprises the following steps:
step 1), taking the following raw materials in parts by mass: ni: 33% -39%, Cr: 16-24%, W: 7-15%, Fe: 25-35%, Ti: 1% -7%;
step 2), mixing the raw materials to prepare spherical alloy powder, and drying and deoxidizing;
and 3) forming the dried and deoxidized spherical alloy powder by adopting an S L M process under the protection of Ar gas and the environment with the oxygen content of less than 200ppm and the cavity pressure of 0-30mbar to obtain the high-strength high-toughness high-entropy alloy.
Furthermore, the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity is 15-53 mu m.
Further, mixing the simple substance powder of Ni, Cr, W, Fe and Ti with the purity of more than or equal to 99.9 percent according to the element content proportion, uniformly mixing, and ball-milling to prepare spherical alloy powder; or smelting Ni, Cr, W, Fe and Ti blocks with the purity of more than or equal to 99.9 percent according to the element content ratio to prepare bars, and preparing the bars into spherical alloy powder by using a gas atomization method or a rotating electrode method.
Further, the obtained spherical alloy powder was put into a drying oven to be dried and deoxidized, wherein the degree of vacuum was 1 × 10-2Pa, the temperature is 60-120 ℃, the time is 6-12 h, then the temperature is naturally cooled to the room temperature, and the vacuum packaging and the storage are carried out.
Further, the alloy powder prepared in the step 2) is placed in a powder cylinder of an S L M metal 3D printer, inert gas is used for protection in a cavity, the oxygen content is controlled within 200ppm, the pressure of a forming cavity is 0-30mbar, the power of the 3D printer is set to be 250-350W, the scanning speed is 1500-3500 mm/S, the scanning distance at a rotation angle of 0-90 degrees is 60-90 mu M, the powder laying amount is 30 mu M, and the powder feeding amount is 80 mu M, so that the high-strength-toughness high-entropy alloy can be obtained.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a high-strength-toughness high-entropy alloy which is prepared by taking the raw materials according to mass fraction, and the density of the formed material is 8.5-8.9g/cm3The tensile strength is 800-830MPa, the elongation after fracture is 21-23%, the selected alloying elements are low in price, and some expensive elements are not available.
The invention relates to a preparation method of a high-strength high-toughness high-entropy alloy, which comprises the steps of mixing raw materials with the mass fraction, drying and deoxidizing the mixture, and forming the mixture by adopting an S L M process to obtain the high-strength high-toughness high-entropy alloy, so that a novel high-strength high-toughness multi-principal-element high-entropy alloy with unequal atomic ratios is obtained, and the high-strength high-toughness high-entropy alloy is different from the existing high-entropy alloy.
Furthermore, a new method for preparing the alloy, which cannot be replaced by the conventional method, is realized by adopting a 3D printing technology, and particularly, the method is easier for forming a complex structure and can meet the requirements of complex components in the fields of aviation, aerospace and the like.
Drawings
FIG. 1 is an XRD spectrum of an alloy of the NiCrWFeTi system of the embodiment.
FIG. 2 is an SEM structure of NiCrWFeTi alloy.
FIG. 3 is a stress-strain diagram of NiCrWFeTi-based high entropy alloy.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
a high-strength, high-toughness and high-entropy alloy is prepared from the following raw materials in percentage by mass: 33-39% of Ni, 16-24% of Cr, 7-15% of W, 25-35% of Fe, 1-7% of Ti and the balance of impurities.
A preparation method of a high-strength, high-toughness and high-entropy alloy comprises the following steps:
step 1), taking the following raw materials in parts by mass: ni: 33% -39%, Cr: 16-24%, W: 7-15%, Fe: 25-35%, Ti: 1-7 percent of the total weight of the composition, and the balance of impurities; mixing the raw materials to prepare spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9%, and the granularity is 15-53 mu m;
specifically, elemental powder of Ni, Cr, W, Fe and Ti with the purity of more than or equal to 99.9 percent is mixed evenly according to the element content proportion and is ball-milled to prepare spherical alloy powder; smelting Ni, Cr, W, Fe and Ti blocks with the purity of more than or equal to 99.9 percent according to the element content ratio to prepare bars, and preparing spherical alloy powder from the bars by using a gas atomization or rotary electrode method;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa at the temperature of 60-120 ℃ for 6-12 h, naturally cooling to room temperature to obtain dry high-entropy alloy powder, carrying out vacuum packaging and storage, and carrying out alloy forming preparation on the dried and deoxidized alloy powder by adopting a selective laser melting (S L M) forming process to obtain the high-strength, high-toughness and high-entropy alloy.
The preparation method specifically adopts the following preparation process:
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of an S L M metal 3D printer, wherein the inert gas is used for protection in a cavity, the oxygen content is controlled within 200ppm, and the pressure of a forming cavity is 0-30 mbar;
the inert gas is He, Ar or N2；
Step 4), setting the power of the 3D printer to be 250-350W, the scanning speed to be 1500-3500 mm/s, the scanning interval to be 60-90 mu m at the rotation angle of 0-90 degrees, the powder spreading amount to be 30 mu m and the powder feeding amount to be 80 mu m; and after the alloy preparation is finished, sampling after 2-4 h.
Figure BDA0001877955770000041
Example 1:
step 1), taking the following materials in parts by mass: ni: 33, Cr: 20, W: 14, Fe: 28, Ti: 5, preparing the materials into spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity of the spherical alloy powder is 15 mu m;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, the temperature is 60 ℃, the time is 7 hours, then the natural cooling is carried out to the room temperature, and the vacuum packaging and the storage are carried out;
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of a 3D printer, vacuumizing a cavity to 98ppm, and protecting Ar gas in the cavity, wherein the oxygen content of the cavity is 760ppm, the pressure of a forming chamber is 17mba, the working pressure is 3.8bar, and the blowing speed is 950 r/min;
step 4), setting the power of the 3D printer to be 250W, the scanning speed to be 1500mm/s, the rotation angle to be 30 degrees, the scanning interval to be 80 mu m, the powder laying amount to be 30 mu m and the powder feeding amount to be 80 mu m, then starting the equipment to prepare the alloy,
and 5) after the alloy preparation is finished, waiting for 2h to obtain the high-strength high-toughness high-entropy alloy.
Example 2:
taking the following materials in parts by mass: ni: 33, Cr: 20, W: 14, Fe: 28, Ti: 5, preparing the materials into spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity of the spherical alloy powder is 20 mu m;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, the temperature is 70 ℃, the time is 6 hours, then the natural cooling is carried out to the room temperature, and the vacuum packaging and the storage are carried out;
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of a 3D printer, vacuumizing a cavity to 100ppm, and protecting the cavity with He gas, wherein the oxygen content of the cavity is 755ppm, the pressure of a forming chamber is 17mba, the working pressure is 3.9bar, and the blowing speed is 1020 r/min;
step 4), setting the power of the 3D printer to be 250W, the scanning speed to be 1500mm/s, the rotation angle to be 30 degrees, the scanning interval to be 80 mu m, the powder laying amount to be 30 mu m and the powder feeding amount to be 80 mu m, then starting the equipment to prepare the alloy,
and 5) after the alloy preparation is finished, waiting for 2h to obtain the high-strength high-toughness high-entropy alloy.
Example 3:
taking the following materials in parts by mass: ni: 35, Cr: 18, W: 12, Fe: 32, Ti: 3, preparing the materials into spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity of the spherical alloy powder is 25 mu m;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, the temperature is 80 ℃, the time is 8 hours, then the mixture is naturally cooled to the room temperature, and the vacuum packaging and the storage are carried out;
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of a 3D printer, vacuumizing a cavity to 97ppm, and protecting Ar gas in the cavity, wherein the oxygen content of the cavity is 750ppm, the pressure of a forming chamber is 19mba, the working pressure is 3.8bar, and the blowing speed is 950 r/min;
step 4), setting the power of the 3D printer to be 250W, the scanning speed to be 1500mm/s, the rotation angle to be 30 degrees, the scanning interval to be 80 mu m, the powder laying amount to be 30 mu m and the powder feeding amount to be 80 mu m, then starting the equipment to prepare the alloy,
and 5) after the alloy preparation is finished, waiting for 2h to obtain the high-strength high-toughness high-entropy alloy.
Example 4
Taking the following materials in parts by mass: ni: 36, Cr: 22, W: 11, Fe: 27, Ti: 4, preparing the materials into spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity of the spherical alloy powder is 30 mu m;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, the temperature is 90 ℃, the time is 9 hours, then the mixture is naturally cooled to the room temperature, and the vacuum packaging and the storage are carried out;
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of a 3D printer, vacuumizing a cavity to 96ppm, and protecting the cavity with He gas, wherein the oxygen content of the cavity is 745ppm, the pressure of a forming chamber is 18mba, the working pressure is 3.9bar, and the blowing speed is 960 r/min;
step 4), setting the power of the 3D printer to be 250W, the scanning speed to be 1500mm/s, the rotation angle to be 30 degrees, the scanning interval to be 80 mu m, the powder laying amount to be 30 mu m and the powder feeding amount to be 80 mu m, then starting the equipment to prepare the alloy,
and 5) after the alloy preparation is finished, waiting for 2h to obtain the high-strength high-toughness high-entropy alloy.
Example 5
Step 1), taking the following materials in parts by mass: ni: 37, Cr: 20, W: 7, Fe: 35, Ti: 1, preparing the materials into spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity of the spherical alloy powder is 35 mu m;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, the temperature is 100 ℃, the time is 10 hours, then the mixture is naturally cooled to the room temperature, and the vacuum packaging and the storage are carried out;
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of a 3D printer, vacuumizing a cavity to 95ppm, and protecting Ar gas in the cavity, wherein the oxygen content of the cavity is 740ppm, the pressure of a forming chamber is 17mba, the working pressure is 3.8bar, and the blowing speed is 980 r/min;
step 4), setting the power of the 3D printer to be 250W, the scanning speed to be 1500mm/s, the rotation angle to be 30 degrees, the scanning interval to be 80 mu m, the powder laying amount to be 30 mu m and the powder feeding amount to be 80 mu m, then starting the equipment to prepare the alloy,
and 5) after the alloy preparation is finished, waiting for 2h to obtain the high-strength high-toughness high-entropy alloy.
Example 6
Step 1), taking the following materials in parts by mass: ni: 38, Cr: 16, W: 10, Fe: 29, Ti: 7, preparing the materials into spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity of the spherical alloy powder is 45 mu m;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, the temperature is 110 ℃, the time is 11 hours, then the mixture is naturally cooled to the room temperature, and the vacuum packaging and the storage are carried out;
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of a 3D printer, vacuumizing a cavity to 94ppm, and protecting Ar gas in the cavity, wherein the oxygen content of the cavity is 760ppm, the pressure of a forming chamber is 18mba, the working pressure is 3.8bar, and the blowing speed is 1000 r/min;
step 4), setting the power of the 3D printer to be 250W, the scanning speed to be 1500mm/s, the rotation angle to be 30 degrees, the scanning interval to be 80 mu m, the powder laying amount to be 30 mu m and the powder feeding amount to be 80 mu m, then starting the equipment to prepare the alloy,
and 5) after the alloy preparation is finished, waiting for 2h to obtain the high-strength high-toughness high-entropy alloy.
Example 7
Step 1), taking the following materials in parts by mass: ni: 39, Cr: 17, W: 8, Fe: 30, Ti: 6, preparing the materials into spherical alloy powder, wherein the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity of the spherical alloy powder is 53 mu m;
step 2), placing the alloy powder prepared in the step 1) in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, at the temperature of 120 ℃ for 12 hours, naturally cooling to room temperature, and carrying out vacuum packaging and storage;
step 3), placing the alloy powder prepared in the step 2) into a powder cylinder of a 3D printer, vacuumizing a cavity to 93ppm, and placing N in the cavity2Under the protection of gas, wherein the oxygen content of the cavity is 740ppm, the pressure of the forming chamber is 19mba, the working pressure is 4.0bar, and the blowing speed is 1050 r/min;
step 4), setting the power of the 3D printer to be 250W, the scanning speed to be 1500mm/s, the rotation angle to be 30 degrees, the scanning interval to be 90 mu m, the powder laying amount to be 50 mu m and the powder feeding amount to be 80 mu m, then starting the equipment to prepare the alloy,
and 5) after the alloy preparation is finished, waiting for 2h to obtain the high-strength high-toughness high-entropy alloy.
The invention provides a preparation method of high-strength high-toughness high-entropy alloy, which is characterized in that the performance data of high-entropy alloy blocks obtained under different process conditions are shown in table 1 and figures 1 to 3 through tests:
TABLE 1 Properties of the high strength and toughness high entropy alloy made by the invention
Figure BDA0001877955770000081
The foregoing is only a result of the preferred embodiments of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.

Claims (2)

1. A preparation method of a high-strength, high-toughness and high-entropy alloy is characterized by comprising the following steps:
step 1), taking the following raw materials in parts by mass: ni: 33% -39%, Cr: 16-24%, W: 7-15%, Fe: 25-35%, Ti: 1% -7%;
step 2), mixing the raw materials to prepare spherical alloy powder, and drying and deoxidizing;
the method specifically comprises the following steps: mixing elemental powder of Ni, Cr, W, Fe and Ti with the purity of more than or equal to 99.9 percent according to the element content proportion, uniformly mixing, and performing ball milling to prepare spherical alloy powder; or smelting Ni, Cr, W, Fe and Ti blocks with the purity of more than or equal to 99.9 percent according to the element content ratio to prepare bars, and preparing spherical alloy powder from the bars by using a gas atomization or rotary electrode method; the purity of the spherical alloy powder is more than or equal to 99.9 percent, and the granularity is 15-53 mu m;
the obtained spherical alloy powderPlacing in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-2Pa, the temperature is 60-120 ℃, the time is 6-12 h, then the natural cooling is carried out to the room temperature, and the vacuum packaging and the storage are carried out;
and 3) placing the dried and deoxidized spherical alloy powder into a powder cylinder of an S L M metal 3D printer, molding by adopting an S L M process under the environment of Ar gas protection, oxygen content of less than 200ppm and cavity pressure of 0-30mbar to obtain the high-strength and high-toughness high-entropy alloy, setting the power of the 3D printer to be 250-350W, the scanning speed to be 1500-3500 mm/S, the scanning distance to be 60-90 mu M at the rotation angle of 0-90 degrees, the powder laying amount to be 30 mu M, and the powder feeding amount to be 80 mu M.
2. The preparation method of the high-strength high-toughness high-entropy alloy as claimed in claim 1, wherein the density of the high-strength high-entropy alloy forming material is 8.5-8.9g/cm3The tensile strength is 800-830MPa, and the elongation after fracture is 21-23%.
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