CN111636025A - High-entropy alloy containing Ti and C and preparation method thereof - Google Patents
High-entropy alloy containing Ti and C and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-entropy alloy containing Ti and C, which comprises the following components: fe. The alloy material comprises Co, Cr, Ni, Mn, Ti and C, wherein the Fe, Co, Cr, Ni and Mn are mixed in equal mass percent, the sum of the mass percent of Ti and C is 3-6%, and the mass percent ratio of Ti to C is 1: 2. The invention also relates to a preparation method of the high-entropy alloy containing Ti and C. The invention uses Ti powder and C powder to improve the defect of low strength of high-entropy alloy FeCoCrNiMn with a FCC structure, adopts a powder metallurgy method to controllably prepare the high-entropy alloy with a single-phase FCC structure, and has excellent comprehensive mechanical property, the yield strength is 1567-1834MPa, the Vickers hardness is 510-556HV, the plastic strain is 21.2-25.7%, the preparation process is simple, the cost is lower, the practicability is strong, and the popularization is convenient, so the invention has wide application prospect in the field of engineering structural materials.
Description
Technical Field
The invention relates to the technical field of high-entropy alloy materials, in particular to a high-entropy alloy containing Ti and C and a preparation method thereof.
Background
At present, the wide definition of high-entropy alloy refers to an alloy composed of 5 to 13 main elements. The multicomponent high-entropy alloy has become a new research hotspot in the field of metal materials because of the unique phase structure, the brand-new design concept and the excellent alloy performance, and is called three major breakthroughs in the field of alloying theories in recent years together with rubber metal and bulk metallic glass.
At present, the method for preparing the block high-entropy alloy mainly comprises a smelting method and a powder metallurgy method. The alloy prepared by the smelting method is easy to have the defects of segregation, shrinkage cavity and the like, and the volume is limited; the powder metallurgy method can obtain the alloy with uniform structure, saves materials, and is one of the main methods for preparing the block high-entropy alloy at present.
FeCoCrNiMn as a typical FCC structure high-entropy alloy shows excellent ductility and toughness, particularly excellent low-temperature plasticity, but has the defect of low strength, and the application of FeCoCrNiMn as a structural material is limited.
Therefore, those skilled in the art are dedicated to develop a high-entropy alloy material based on FeCoCrNiMn, which has excellent comprehensive mechanical properties, i.e., high strength and good plasticity.
Disclosure of Invention
The invention aims to provide a high-entropy alloy containing Ti and C and a preparation method thereof.
In order to achieve the purpose, the invention adopts a technical scheme that: a high entropy alloy containing Ti and C, comprising the following components: fe. The alloy material comprises Co, Cr, Ni, Mn, Ti and C, wherein the Fe, Co, Cr, Ni and Mn are mixed in equal mass percent, the sum of the mass percent of Ti and C is 3-6%, and the mass percent ratio of Ti to C is 1: 2.
In order to achieve the above purpose, the invention also adopts a technical scheme that: a preparation method of a high-entropy alloy containing Ti and C comprises the following steps:
step 1: respectively weighing Fe powder, Co powder, Cr powder, Ni powder, Mn powder, Ti powder and C powder according to the mass percentage;
step 2: carrying out ball milling on the Fe powder, the Co powder, the Cr powder, the Ni powder, the Mn powder and the C powder weighed in the step 1 to obtain mixed powder;
and step 3: and (3) performing vacuum hot-pressing sintering on the mixed powder obtained in the step (2), adding weighed Ti powder after the mixed powder is completely melted, and continuing performing vacuum hot-pressing sintering to obtain the block alloy.
Further, the specific process of ball milling in the step 2 is that the Fe powder, the Co powder, the Cr powder, the Ni powder, the Mn powder and the C powder weighed in the step 1 are poured into a vacuum ball milling tank, the tank is packaged in a vacuum glove box protected by high-purity argon atmosphere, and then the vacuum ball milling tank is placed into an all-directional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, and the ball milling time is 20-40 h.
Further, stopping adding a certain amount of n-heptane every 3h during ball milling in the step 2, and drying in a vacuum drying oven at 100 ℃ for 10h after the ball milling is finished.
And 3, filling the mixed powder obtained in the step 2 into a graphite mold, sintering in a vacuum hot-pressing sintering furnace at the sintering temperature of 800-.
Compared with the prior art, the high-entropy alloy containing Ti and C and the preparation method thereof have the beneficial effects that:
1. the invention uses Ti powder and C powder to improve the defect of low strength of high-entropy alloy FeCoCrNiMn with an FCC structure, and adopts a powder metallurgy method to controllably prepare the high-entropy alloy with a single-phase FCC structure, which shows excellent comprehensive mechanical property, the yield strength is 1567-1834MPa, the Vickers hardness is 510-556HV, and the plastic strain is 21.2-25.7%.
2. The mass percent ratio of Ti to C is 1:2, the cheaper C powder has higher ratio, and the cost is reduced.
3. The preparation process is simple, the cost is low, the practicability is strong, and the popularization is convenient, so that the preparation method has wide application prospect in the field of engineering structural materials.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to a high-entropy alloy containing Ti and C, which comprises the following components: fe. The alloy material comprises Co, Cr, Ni, Mn, Ti and C, wherein the Fe, Co, Cr, Ni and Mn are mixed in equal mass percent, the sum of the mass percent of the Ti and the mass percent of the C ranges from 3% to 6%, and the mass percent of the Ti and the mass percent of the C are in a ratio of 1: 2.
The invention relates to a preparation method of a high-entropy alloy containing Ti and C, which comprises the following steps:
step 1: respectively weighing Fe powder, Co powder, Cr powder, Ni powder, Mn powder, Ti powder and C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 20-40h, stopping the machine at intervals of 3h during ball milling, adding a certain amount of n-heptane, and drying the ball-milled powder in a vacuum drying box at 100 ℃ for 10h to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace, wherein the sintering temperature is 800-1000 ℃, the heating rate is 6-10 ℃/min, the sintering pressure is 40-50MPa, after the mixed powder is completely melted after heat preservation for 0.5h, adding weighed Ti powder, continuing to perform vacuum hot-pressing sintering, and cooling the unloading pressure to room temperature along with the furnace after heat preservation for 1h to obtain the block alloy.
Example 1:
a preparation method of a high-entropy alloy containing Ti and C comprises the following steps:
step 1: respectively weighing 19.4g of Fe powder, 19.4g of Co powder, 19.4g of Cr powder, 19.4g of Ni powder, 19.4g of Mn powder, 1g of Ti powder and 2g of C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 20h, a certain amount of n-heptane is added every 3h during ball milling, and drying the ball-milled powder in a vacuum drying box for 10h at 100 ℃ to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace, wherein the sintering temperature is 800 ℃, the heating rate is 6 ℃/min, the sintering pressure is 40MPa, after the mixed powder is completely melted after heat preservation for 0.5h, adding weighed Ti powder, continuing to perform vacuum hot-pressing sintering, and after heat preservation for 1h, cooling the unloading pressure to room temperature along with the furnace to obtain the block alloy.
Example 2:
a preparation method of a high-entropy alloy containing Ti and C comprises the following steps:
step 1: respectively weighing 19.1g of Fe powder, 19.1g of Co powder, 19.1g of Cr powder, 19.1g of Ni powder, 19.1g of Mn powder, 1.5g of Ti powder and 3g of C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 30h, a certain amount of n-heptane is added every 3h during ball milling, and drying the ball-milled powder in a vacuum drying box for 10h at 100 ℃ to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace, wherein the sintering temperature is 900 ℃, the heating rate is 8 ℃/min, the sintering pressure is 45MPa, after the mixed powder is completely melted after heat preservation for 0.5h, adding weighed Ti powder, continuing to perform vacuum hot-pressing sintering, and after heat preservation for 1h, cooling the unloading pressure to room temperature along with the furnace to obtain the block alloy.
Example 3:
a preparation method of a high-entropy alloy containing Ti and C comprises the following steps:
step 1: respectively weighing 19.1g of Fe powder, 19.1g of Co powder, 19.1g of Cr powder, 19.1g of Ni powder, 19.1g of Mn powder, 1.5g of Ti powder and 3g of C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 40h, stopping the machine at intervals of 3h during ball milling, adding a certain amount of n-heptane, and drying the ball-milled powder in a vacuum drying box at 100 ℃ for 10h to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace, wherein the sintering temperature is 900 ℃, the heating rate is 6 ℃/min, the sintering pressure is 50MPa, after the mixed powder is completely melted after heat preservation for 0.5h, adding weighed Ti powder, continuing to perform vacuum hot-pressing sintering, and after heat preservation for 1h, cooling the unloading pressure to room temperature along with the furnace to obtain the block alloy.
Example 4:
step 1: respectively weighing 18.8g of Fe powder, 18.8g of Co powder, 18.8g of Cr powder, 18.8g of Ni powder, 18.8g of Mn powder, 2g of Ti powder and 4g of C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 40h, stopping the machine at intervals of 3h during ball milling, adding a certain amount of n-heptane, and drying the ball-milled powder in a vacuum drying box at 100 ℃ for 10h to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace at the sintering temperature of 1000 ℃, at the heating rate of 10 ℃/min and at the sintering pressure of 50MPa, keeping the temperature for 0.5h, completely melting the mixed powder, adding weighed Ti powder, continuing to perform vacuum hot-pressing sintering, keeping the temperature for 1h, and cooling the unloading pressure to room temperature along with the furnace to obtain the block alloy.
Example 5:
a preparation method of a high-entropy alloy containing Ti and C comprises the following steps:
step 1: respectively weighing 18.8g of Fe powder, 18.8g of Co powder, 18.8g of Cr powder, 18.8g of Ni powder, 18.8g of Mn powder, 2g of Ti powder and 4g of C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 40h, stopping the machine at intervals of 3h during ball milling, adding a certain amount of n-heptane, and drying the ball-milled powder in a vacuum drying box at 100 ℃ for 10h to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace, wherein the sintering temperature is 900 ℃, the heating rate is 6 ℃/min, the sintering pressure is 50MPa, after the mixed powder is completely melted after heat preservation for 0.5h, adding weighed Ti powder, continuing to perform vacuum hot-pressing sintering, and after heat preservation for 1h, cooling the unloading pressure to room temperature along with the furnace to obtain the block alloy.
Comparative example 1:
step 1: respectively weighing 20g of Fe powder, 20g of Co powder, 20g of Cr powder, 20g of Ni powder and 20g of Mn powder according to the mass percentage;
step 2: pouring the mixture obtained in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, then placing the tank body into an all-directional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 40 hours, stopping the machine at intervals of 3 hours during ball milling, adding a certain amount of n-heptane, taking the n-heptane as a process control agent to prevent cold welding of mixed powder, and drying the mixed powder in a vacuum drying box for 10 hours at 100 ℃ after the ball milling is finished to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace at the sintering temperature of 900 ℃, at the heating rate of 6 ℃/min and at the sintering pressure of 50MPa, keeping the temperature for 1.5h, and cooling the unloading pressure along with the furnace to room temperature to obtain the bulk alloy.
Comparative example 2:
step 1: respectively weighing 19.1g of Fe powder, 19.1g of Co powder, 19.1g of Cr powder, 19.1g of Ni powder, 19.1g of Mn powder, 3g of Ti powder and 1.5g of C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 40h, stopping the machine at intervals of 3h during ball milling, adding a certain amount of n-heptane, and drying the ball-milled powder in a vacuum drying box at 100 ℃ for 10h to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace, wherein the sintering temperature is 900 ℃, the heating rate is 6 ℃/min, the sintering pressure is 50MPa, after the mixed powder is completely melted after heat preservation for 0.5h, adding weighed Ti powder, continuing to perform vacuum hot-pressing sintering, and after heat preservation for 1h, cooling the unloading pressure to room temperature along with the furnace to obtain the block alloy.
Comparative example 3:
step 1: respectively weighing 19.1g of Fe powder, 19.1g of Co powder, 19.1g of Cr powder, 19.1g of Ni powder, 19.1g of Mn powder, 1.5g of Ti powder and 3g of C powder according to the mass percentage;
step 2: pouring Fe powder, Co powder, Cr powder, Ni powder, Mn powder, Ti powder and C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, putting the tank body into an all-dimensional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, the ball milling time is 40h, stopping the machine at intervals of 3h during ball milling, adding a certain amount of n-heptane, and drying the ball-milled powder in a vacuum drying box at 100 ℃ for 10h to obtain mixed powder;
and step 3: and (3) filling the mixed powder obtained in the step (2) into a graphite die, sintering in a vacuum hot-pressing sintering furnace at the sintering temperature of 900 ℃, at the heating rate of 6 ℃/min and at the sintering pressure of 50MPa, keeping the temperature for 1.5h, and cooling the unloading pressure along with the furnace to room temperature to obtain the bulk alloy.
Experimental data
Mechanical property tests were performed on the high-entropy alloys prepared in examples 1 to 5 and comparative examples 1 to 3, respectively, to obtain the data in table 1.
TABLE 1
Of course, those skilled in the art will recognize that the above-described embodiments are illustrative only, and not intended to be limiting, and that changes and modifications may be made thereto without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. A high entropy alloy comprising Ti and C, characterized in that: comprises the following components: fe. The alloy material comprises Co, Cr, Ni, Mn, Ti and C, wherein the Fe, Co, Cr, Ni and Mn are mixed in equal mass percent, the sum of the mass percent of Ti and C is 3-6%, and the mass percent ratio of Ti to C is 1: 2.
2. A preparation method of a high-entropy alloy containing Ti and C is characterized by comprising the following steps: the method comprises the following steps:
step 1: respectively weighing Fe powder, Co powder, Cr powder, Ni powder, Mn powder, Ti powder and C powder according to the mass percentage;
step 2: carrying out ball milling on the Fe powder, the Co powder, the Cr powder, the Ni powder, the Mn powder and the C powder weighed in the step 1 to obtain mixed powder;
and step 3: and (3) performing vacuum hot-pressing sintering on the mixed powder obtained in the step (2), adding weighed Ti powder after the mixed powder is completely melted, and continuing performing vacuum hot-pressing sintering to obtain the block alloy.
3. A method of producing a high entropy alloy containing Ti and C as claimed in claim 2, characterized in that: and 2, pouring the Fe powder, the Co powder, the Cr powder, the Ni powder, the Mn powder and the C powder weighed in the step 1 into a vacuum ball milling tank, packaging the tank body in a vacuum glove box protected by high-purity argon atmosphere, and then putting the tank body into an all-directional planetary high-energy ball mill for ball milling, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 300r/min, the diameter of a grinding ball is 10mm, and the ball milling time is 20-40 h.
4. A method of producing a high entropy alloy containing Ti and C as claimed in claim 3, characterized in that: and (3) stopping adding a certain amount of n-heptane every 3h during ball milling in the step 2, and drying in a vacuum drying oven at 100 ℃ for 10h after the ball milling is finished.
5. A method of producing a high entropy alloy containing Ti and C as claimed in claim 2, characterized in that: and 3, filling the mixed powder obtained in the step 2 into a graphite mold, sintering in a vacuum hot-pressing sintering furnace at the sintering temperature of 800-1000 ℃, at the heating rate of 6-10 ℃/min and at the sintering pressure of 40-50MPa, keeping the temperature for 0.5h, completely melting the mixed powder, adding the weighed Ti powder, continuing to perform vacuum hot-pressing sintering, and cooling the unloading pressure to room temperature along with the furnace after keeping the temperature for 1 h.
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