CN112792346A - Preparation method of TiB 2-enhanced high-entropy alloy powder for 3D printing - Google Patents
Preparation method of TiB 2-enhanced high-entropy alloy powder for 3D printing Download PDFInfo
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Abstract
The invention provides a TiB2The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: the method comprises the following steps: (1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby; (2) mixing the nano TiB2The first part of the screened high-entropy alloy powder and the first part of the screened high-entropy alloy powder are placed into a mixer according to the mass fraction of 3:97 to be fully and uniformly mixed; (3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and mechanically millingThe nano TiB2 is embedded into the high-entropy alloy powder in an alloying mode; (4) putting the ball-milled high-entropy alloy powder into a drying box for drying; (5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
Description
Technical Field
The invention relates to the technical field of special materials for 3D printing, in particular to a TiB2A preparation method of enhanced high-entropy alloy powder for 3D printing is provided.
Background
High Entropy Alloys (HEA), an emerging frontier technology in the field of metallic materials, have high mixed configuration entropies that tend to stabilize solid solutions based on simple lower surface Face Centered Cubic (FCC), Body Centered Cubic (BCC) or matrix centered cubic. Hexagonal Close Packed (HCP) structure. In general, the definition of HEA is based on composition or entropy. For composition-based definitions, HEA consists of five or more major elements, each element at a concentration between 5 and 35 atomic percent (at%). The constituent elements of the HEAs may be selected from transition metals, alkaline earth metals, basic metals, metalloids, and non-metals, with cobalt, chromium, copper, iron, manganese, nickel, hafnium, tantalum, titanium, molybdenum, niobium, vanadium, zirconium, tungsten, zinc, aluminum, silicon, and boron being commonly used. By screening appropriate combinations of its constituent elements and adjusting their proportions, HEAs can exhibit significant mechanical properties at high temperatures, excellent strength, ductility and fracture toughness at low temperatures, as well as superparamagnetism, superconductivity and excellent radiation resistance. Therefore, they are considered as alternatives to high temperature turbine blades, high temperature molds, hard coatings on cutting tools, and the like.
For example, chinese patent CN201510305783.9 discloses a high-entropy alloy powder for 3D printing and a method for preparing a high-entropy alloy coating using the same, the high-entropy alloy powder of the present invention is composed of Ni: 16% -25%, Co: 16% -25%, Cr: 16% -25%, Ti: 16% -25% and V: 16-25 percent. The preparation method comprises the following steps: firstly, ball-milling and mixing raw materials to obtain mixed powder; secondly, polishing and cleaning the substrate; and thirdly, placing the mixed powder in a powder feeder of 3D printing equipment, and forming a high-entropy alloy coating on the surface of the substrate by adopting laser selective sintering. At present, the tensile strength of 3D printing FeCoNiCr high-entropy alloy is generally about 600MPa, and the tensile strength cannot meet the mechanical property requirements of certain products, so that the mechanical property of the products needs to be enhanced by adding some strengthening phases, the performance of raw materials can be effectively improved by taking TiB2 as a secondary phase, and different from the traditional materials, the raw materials for 3D printing are metal powder with the specification of 15-53 mu m, so that how to efficiently introduce TiB2 powder into FeCoNiCr high-entropy alloy powder is the key point of the invention, and meanwhile, the fluidity of the powder is also kept without influencing the printing effect.
Disclosure of Invention
To overcome the high efficiency of TiB in the prior art2The invention provides a TiB (titanium boride) which is introduced into FeCoNiCr high-entropy alloy powder and can keep the flowability of the powder without influencing the printing effect2A preparation method of enhanced high-entropy alloy powder for 3D printing is provided.
The technical scheme adopted by the invention is as follows: TiB2The preparation method of the enhanced high-entropy alloy powder for 3D printing has the innovation points that: the method comprises the following steps:
(1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby;
(2) mixing the nano TiB2The first part of the screened high-entropy alloy powder and the first part of the screened high-entropy alloy powder are placed into a mixer according to the mass fraction of 3:97 to be fully and uniformly mixed;
(3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and mechanically alloying the nano TiB2Embedding the alloy powder into high-entropy alloy powder;
(4) putting the ball-milled high-entropy alloy powder into a drying box for drying;
(5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
In some embodiments, the FeCoNiCr high entropy alloy includes elements including Fe, Mn, Cr, Co, Nb, Mo, Ni.
In some embodiments, the weight fractions of the elements of the FeCoNiCr high-entropy alloy are Fe: 20-35%, Mn: 30-35%, Cr: 2-10%, Co: 3-15%, Nb: 2-10%, Mo: 15-25%, Ni: 5 to 25 percent.
In some embodiments, the ball milling speed is 300 to 400r/min, and the time is 6 to 10 hours.
In some embodiments, the drying is performed by placing the ball-milled metal powder into a vacuum drying oven for drying for 8-10 hours at a drying temperature of 80 ℃.
In some embodiments, the average particle size of the high entropy alloy powder is 15 to 53 μm.
In some embodiments, the ultrasonic power is 2-4 kw and the frequency is 2-3 GHz.
In some embodiments, the 3D printing comprises laser 3D printing, electron beam powder bed 3D printing, or laser powder feed 3D printing.
Compared with the prior art, the invention has the beneficial effects that:
(1) the main core of the invention is to mix the nano TiB2The powder is efficiently introduced into FeCoNiCr high-entropy alloy, and the powder with the particle size of less than 15 mu m is screened out, so that the mechanical property of the product is improved, and the powder laying effect in the 3d printing process is not influenced.
(2) The 15-53 mu m FeCoNiCr (TiB) is obtained by the preparation method2) The flowability of the high-entropy alloy powder is unchanged, and the Hall flow rate is as follows: 16-19S/50g, tensile strength of the product after 3D printing: 800-840MPa, the elongation is 15% -20%, compared with the non-reinforced high-entropy alloy, TiB2The tensile strength of the reinforced high-entropy alloy powder after 3D printing is improved by 30%, and the elongation and the Hall flow rate are basically unchanged.
(3) The preparation method of the invention can ensure the fluidity of the powder and efficiently mix the nano TiB2FeCoNiCr high-entropy alloy powder is embedded, so that the comprehensive mechanical property of the high-entropy alloy is improved.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the present invention;
FIG. 2 is a schematic flow chart of the preparation method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention discloses a TiB2The preparation method of the enhanced high-entropy alloy powder for 3D printing has the innovation points that: as shown in fig. 1 and 2: the method comprises the following steps:
(1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby;
(2) mixing the nano TiB2The first part of the screened high-entropy alloy powder and the first part of the screened high-entropy alloy powder are placed into a mixer according to the mass fraction of 3:97 to be fully and uniformly mixed;
(3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and mechanically alloying the nano TiB2Embedding the alloy powder into high-entropy alloy powder;
(4) putting the ball-milled high-entropy alloy powder into a drying box for drying;
(5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
Specifically, in this embodiment of the present invention, the FeCoNiCr high entropy alloy includes Fe, Mn, Cr, Co, Nb, Mo, Ni elements. Specifically, the weight fractions of the elements of the FeCoNiCr high-entropy alloy are respectively Fe: 20-35%, Mn: 30-35%, Cr: 2-10%, Co: 3-15%, Nb: 2-10%, Mo: 15-25%, Ni: 5 to 25 percent.
Specifically, the ball milling speed is 300-400 r/min, and the time is 6-10 h.
Specifically, the drying step is to dry the ball-milled metal powder in a vacuum drying oven for 8-10 hours at 80 ℃.
Specifically, the average grain diameter of the high-entropy alloy powder is 15-53 μm.
Specifically, the ultrasonic power is 2-4 kw, and the frequency is 2-3 GHz.
Specifically, the 3D printing comprises laser 3D printing, electron beam powder bed 3D printing or laser powder feeding 3D printing.
The main core of the invention is to mix the nano TiB2The powder is efficiently introduced into FeCoNiCr high-entropy alloy, and the powder with the particle size of less than 15 mu m is screened out, so that the mechanical property of the product is improved, and the powder laying effect in the 3d printing process is not influenced.
The 15-53 mu m FeCoNiCr (TiB) is obtained by the preparation method2) The flowability of the high-entropy alloy powder is unchanged, and the Hall flow rate is as follows: 16-19S/50g, tensile strength of the product after 3D printing: 800-840MPa, the elongation is 15% -20%, compared with the non-reinforced high-entropy alloy, TiB2The tensile strength of the reinforced high-entropy alloy powder after 3D printing is improved by 30%, and the elongation and the Hall flow rate are basically unchanged.
The preparation method of the invention can ensure the fluidity of the powder and efficiently mix the nano TiB2FeCoNiCr high-entropy alloy powder is embedded, so that the comprehensive mechanical property of the high-entropy alloy is improved. The method solves the problem that the high-entropy alloy powder prepared by the traditional method adopts pure-substance alloy billet ingots, and inevitably causes the volatilization of elements with low melting points in the smelting process due to different melting points of the elements and even overlarge melting point difference, so that the element content of the prepared powder is overlarge with the theoretical content difference.
Example 1
The preparation method and the parameter setting of the embodiment specifically comprise the following steps:
(1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby;
(2) mixing the nano TiB2The first part of the screened high-entropy alloy powder and the first part of the screened high-entropy alloy powder are placed into a mixer according to the mass fraction of 3:97 to be fully and uniformly mixed;
(3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and adopting a mechanical mixerThe nano TiB is formed by the way of gold plating2Embedding the alloy powder into high-entropy alloy powder;
(4) putting the ball-milled high-entropy alloy powder into a drying box for drying;
(5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
The weight fractions of the elements of the FeCoNiCr high-entropy alloy are respectively Fe: 20%, Mn: 35%, Cr: 10%, Co: 3%, Nb: 2%, Mo: 15%, Ni: 15 percent.
Specifically, the ball milling speed is 3000r/min, and the time is 6 h.
Specifically, the drying step is to dry the ball-milled metal powder in a vacuum drying oven for 8 hours at a drying temperature of 80 ℃.
Specifically, the average grain diameter of the high-entropy alloy powder is 15-53 μm.
Specifically, the ultrasonic power is 2kw, and the frequency is 2 GHz.
Example 2
The preparation method and the parameter setting of the embodiment specifically comprise the following steps:
(1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby;
(2) mixing the nano TiB2The first part of the screened high-entropy alloy powder and the first part of the screened high-entropy alloy powder are placed into a mixer according to the mass fraction of 3:97 to be fully and uniformly mixed;
(3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and mechanically alloying the nano TiB2Embedding the alloy powder into high-entropy alloy powder;
(4) putting the ball-milled high-entropy alloy powder into a drying box for drying;
(5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
The weight fractions of the elements of the FeCoNiCr high-entropy alloy are respectively Fe: 20%, Mn: 35%, Cr: 10%, Co: 3%, Nb: 2%, Mo: 15%, Ni: 155 percent.
Specifically, the ball milling speed is 400r/min, and the time is 10 h.
Specifically, the drying step is to dry the ball-milled metal powder in a vacuum drying oven for 10 hours at a drying temperature of 80 ℃.
Specifically, the average grain diameter of the high-entropy alloy powder is 15-53 μm.
Specifically, the ultrasonic power is 4kw, and the frequency is 3 GHz.
Example 3
The preparation method and the parameter setting of the embodiment specifically comprise the following steps:
(1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby;
(2) mixing the nano TiB2The first part of the screened high-entropy alloy powder and the first part of the screened high-entropy alloy powder are placed into a mixer according to the mass fraction of 3:97 to be fully and uniformly mixed;
(3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and mechanically alloying the nano TiB2Embedding the alloy powder into high-entropy alloy powder;
(4) putting the ball-milled high-entropy alloy powder into a drying box for drying;
(5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
The weight fractions of the elements of the FeCoNiCr high-entropy alloy are respectively Fe: 20%, Mn: 35%, Cr: 10%, Co: 3%, Nb: 2%, Mo: 15%, Ni: 15 percent.
Specifically, the ball milling speed is 350r/min, and the time is 8 h.
Specifically, the drying step is to dry the ball-milled metal powder in a vacuum drying oven for 9 hours at a drying temperature of 80 ℃.
Specifically, the average grain diameter of the high-entropy alloy powder is 15-53 μm.
Specifically, the ultrasonic power is 3kw, and the frequency is 2 GHz.
Example 4
The preparation method and the parameter setting of the embodiment specifically comprise the following steps:
(1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby;
(2) mixing the nano TiB2The first part of the screened high-entropy alloy powder and the first part of the screened high-entropy alloy powder are placed into a mixer according to the mass fraction of 3:97 to be fully and uniformly mixed;
(3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and mechanically alloying the nano TiB2Embedding the alloy powder into high-entropy alloy powder;
(4) putting the ball-milled high-entropy alloy powder into a drying box for drying;
(5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
The weight fractions of the elements of the FeCoNiCr high-entropy alloy are respectively Fe: 35%, Mn: 30%, Cr: 2%, Co: 10%, Nb: 3%, Mo: 15%, Ni: 5 percent.
Specifically, the ball milling speed is 350r/min, and the time is 8 h.
Specifically, the drying step is to dry the ball-milled metal powder in a vacuum drying oven for 9 hours at a drying temperature of 80 ℃.
Specifically, the average grain diameter of the high-entropy alloy powder is 15-53 μm.
Specifically, the ultrasonic power is 3kw, and the frequency is 2 GHz.
The high-entropy alloy powder prepared by the method has good fluidity, high apparent density, high compactness and high mechanical property of 3D printing parts. The invention provides a printing material with high quality and excellent performance for the field of 3D printing, and enriches the types of the printing material.
In the description of the present invention, it is to be understood that the terms "coaxial", "bottom", "one end", "top", "middle", "other end", "upper", "one side", "top", "inner", "front", "center", "both ends", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "disposed," "connected," "secured," "screwed" and the like are to be construed broadly, e.g., as meaning fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; the terms may be directly connected or indirectly connected through an intermediate, and may be communication between two elements or interaction relationship between two elements, unless otherwise specifically limited, and the specific meaning of the terms in the present invention will be understood by those skilled in the art according to specific situations.
While the foregoing description shows and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. TiB2The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: the method comprises the following steps:
(1) the FeCoNiCr high-entropy alloy with the specification of 15-53 mu m is classified by air flow, and the weight proportion of powder with the particle size of less than 15 mu m in the powder is controlled within 1 percent for standby;
(2) mixing the nano TiB2And a first portion of sieved high entropy alloy powderPutting the materials into a mixer according to the mass fraction of 3:97, and fully and uniformly mixing;
(3) placing the mixed metal powder on a ball mill for ball milling, introducing ultrasonic waves to the periphery of the ball mill, and mechanically alloying the nano TiB2Embedding the alloy powder into high-entropy alloy powder;
(4) putting the ball-milled high-entropy alloy powder into a drying box for drying;
(5) and (3) classifying the dried ball-milled high-entropy alloy powder by airflow to ensure that the weight proportion of the powder with the particle size of less than 15 mu m is controlled within 1%.
2. The TiB of claim 12The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: the FeCoNiCr high-entropy alloy comprises Fe, Mn, Cr, Co, Nb, Mo and Ni elements.
3. The TiB of claim 22The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: the weight fractions of the elements of the FeCoNiCr high-entropy alloy are respectively Fe: 20-35%, Mn: 30-35%, Cr: 2-10%, Co: 3-15%, Nb: 2-10%, Mo: 15-25%, Ni: 5 to 25 percent.
4. The TiB of claim 12The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: and ball milling is carried out at the speed of 300-400 r/min for 6-10 h.
5. The TiB of claim 42The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: and the drying step is to dry the ball-milled metal powder in a vacuum drying oven for 8-10 h at 80 ℃.
6. The TiB of claim 12The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: the average grain diameter of the high-entropy alloy powder is15-53μm。
7. The TiB of claim 12The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: the ultrasonic power is 2-4 kw, and the frequency is 2-3 GHz.
8. The TiB of claim 12The preparation method of the enhanced high-entropy alloy powder for 3D printing is characterized by comprising the following steps of: the 3D printing comprises laser 3D printing, electron beam powder bed 3D printing or laser powder feeding 3D printing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113981291A (en) * | 2021-10-15 | 2022-01-28 | 中国航发北京航空材料研究院 | High-entropy alloy gradient material and preparation method thereof |
| CN114951644A (en) * | 2022-06-22 | 2022-08-30 | 西安交通大学 | High-entropy alloy composite material for additive manufacturing and preparation method and application thereof |
| CN115141967A (en) * | 2022-06-13 | 2022-10-04 | 哈尔滨工业大学（深圳） | High-entropy alloy composite material and preparation method and application thereof |
| JPWO2022260044A1 (en) * | 2021-06-08 | 2022-12-15 |
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| CN105734324A (en) * | 2016-03-04 | 2016-07-06 | 中南大学 | Preparing method for powder metallurgy high-entropy alloy based composite material |
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| JP7327704B2 (en) | 2021-06-08 | 2023-08-16 | 株式会社プロテリアル | Alloy materials, alloy products using alloy materials, and machinery equipped with alloy products |
| CN113981291A (en) * | 2021-10-15 | 2022-01-28 | 中国航发北京航空材料研究院 | High-entropy alloy gradient material and preparation method thereof |
| CN113981291B (en) * | 2021-10-15 | 2022-09-20 | 中国航发北京航空材料研究院 | High-entropy alloy gradient material and preparation method thereof |
| CN115141967A (en) * | 2022-06-13 | 2022-10-04 | 哈尔滨工业大学（深圳） | High-entropy alloy composite material and preparation method and application thereof |
| CN115141967B (en) * | 2022-06-13 | 2023-11-14 | 哈尔滨工业大学（深圳） | High-entropy alloy composite material and preparation method and application thereof |
| CN114951644A (en) * | 2022-06-22 | 2022-08-30 | 西安交通大学 | High-entropy alloy composite material for additive manufacturing and preparation method and application thereof |
| CN114951644B (en) * | 2022-06-22 | 2023-12-01 | 西安交通大学 | High-entropy alloy composite material for additive manufacturing and preparation method and application thereof |
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