CN116145004B - High-density crack-free Al-containing high-entropy alloy and laser additive manufacturing method thereof - Google Patents
High-density crack-free Al-containing high-entropy alloy and laser additive manufacturing method thereof Download PDFInfo
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
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- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B33Y70/00—Materials specially adapted for additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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Abstract
The invention discloses a high-density crack-free Al-containing high-entropy alloy and a laser additive manufacturing method thereof, wherein the molecular formula of the high-entropy alloy is Fe 25Co25Cr18.75Ni25AlxNb(6.25‑x) (x= 0,2,4,6.25), the cluster mode is [ (Al xNb(6.25‑x))-(FeCoNi)75]Cr18.75 (x= 0,2,4,6.25), the high-entropy alloy is prepared by taking Fe, co, cr, ni, al, nb metal powder according to the atomic molar ratio, putting the prepared alloy powder into a ball milling tank for ball milling, taking 304L stainless steel as a base material, and overlapping, melting and depositing the alloy powder layer by layer on the surface of the base material by using a laser additive technology.
Description
Technical Field
The invention relates to the technical field of high-entropy alloy preparation, in particular to an Al-containing high-entropy alloy with high density and no cracks and a laser additive manufacturing method thereof.
Background
In recent years, high-entropy alloys have been attracting attention because they can achieve a higher hardness, a better toughness, and an excellent wear resistance than conventional alloys. The high-entropy alloy is prepared by mixing five or more metal elements in equimolar ratio or approximately equimolar ratio. The multi-component high-entropy alloy is easy to form complex structures such as intermetallic compounds and the like, so that the performance of the alloy is influenced, and the application of the alloy is limited. In most studies, for commonly used high entropy alloy systems, such as: fe. The elements with higher melting points such as Co, cr, ni and the like are very easy to generate pasty areas in the process of quick heating and quick cooling due to the lower melting point of Al element, so that the prepared high-entropy alloy containing the Al element is more easy to generate defects such as microcracks, micropores and the like, the high-entropy alloy system involved with the Al element is limited, and the high-entropy alloy is also a great difficulty in the design of high-entropy alloy components. As alloy composition design tends to be increasingly complex, we face a great challenge in designing high-quality high-entropy alloy compositions. In order to ensure that the prepared high-entropy alloy does not have cracks, the design of the high-entropy alloy component containing the Al element is quite complex, the content of the Al element is difficult to control, and the excessive content of the Al can raise the risk of the cracks. The high-entropy alloy with obvious cracks prepared by the original x=6.25 in the scheme, by controlling the proportion of the Al content, the obtained grain size is also reduced along with the reduction of the Al content, so that the cracks are eliminated and the structure is more compact. The mechanical properties of the high-entropy alloy are diversified by regulating and controlling the contents of different Al elements.
Because the texture obtained by the traditional method for preparing the high-entropy alloy is rough, holes or cracks can exist, the preparation process is complicated, and the cost is high. The laser additive manufacturing is used as one of the preparation methods of the metal powder with potential at present, and the characteristics of superposition of multiple melting pools are utilized, so that the powder has excellent high-temperature fluidity, hot cracks caused by serious component segregation are avoided, and the obtained compactness is higher. The process adjustability, heat concentration and rapid heating and cooling rate can enable elements to be distributed uniformly, the structure is more compact, gradient behaviors can be presented on a space layer, multiple performances are obtained, and therefore the mechanical properties of materials are improved, so that the laser additive manufacturing is the first choice process for solving the problems of high performance, difficult machining and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the high-entropy alloy containing Al with high density and no cracks and the laser additive manufacturing method thereof, so as to solve the problem that the high-entropy alloy containing Al elements prepared by the laser additive manufacturing process has typical cracks.
In order to achieve the above purpose, the invention provides a high-density crack-free Al-containing high-entropy alloy, wherein the molecular formula of the high-entropy alloy is Fe 25Co25Cr18.75Ni25AlxNb(6.25-x) (x= 0,2,4,6.25), and the cluster mode is [ (Al xNb(6.25-x))-(FeCoNi)75]Cr18.75 (x= 0,2,4,6.25).
The invention also provides a laser additive manufacturing method of the high-density crack-free Al-containing high-entropy alloy, which comprises the following steps:
S1, taking Fe, co, cr, ni, al, nb metal powder according to an atomic molar ratio to prepare alloy powder;
S2, placing the prepared alloy powder into a ball milling tank for ball milling, sieving with a 100-mesh sieve, and drying and preserving;
S3, using 304L stainless steel as a base material, removing oxide skin and surface stains on the cladding surface of the base material, and overlapping, melting and depositing alloy powder on the surface of the base material layer by layer from bottom to top by using a laser additive manufacturing technology to obtain a deposited high-entropy alloy sample.
In the scheme, the method comprises the following steps: the purity of the starting material Fe, co, ni, cr, al, nb is not less than 99.95wt.%.
In the scheme, the method comprises the following steps: raw materials Fe, co, ni, cr, al, nb are spherical powder.
In the scheme, the method comprises the following steps: preparing a deposition state high-entropy alloy sample by a laser additive manufacturing technology under the protection of argon atmosphere, wherein the pressure rate of the protective gas is 5L/min, and the oxygen content in an argon filling environment is not higher than 50ppm.
In the scheme, the method comprises the following steps: the laser power is 1000-1100w, the moving speed is 15mm/s, the powder feeding speed is 2r/min, the layer height is 0.35mm, and the laser spot diameter is 3mm.
In the scheme, the method comprises the following steps: the thickness of the deposited high-entropy alloy sample is 0.3-0.4mm.
In the scheme, the method comprises the following steps: ball milling the alloy powder in a stainless steel ball milling tank for 1h, sieving with a 100-mesh sieve, and placing in a vacuum drying oven at 100-120 ℃ for preservation for more than 2 h.
The beneficial effects of the invention are as follows: according to the invention, the excellent high-entropy alloy [ (Al xNb(6.25-x))-(FeCoNi)75]Cr18.75 (x= 0,2,4,6.25) ] is designed according to a cluster+connecting atomic model, the molar ratio of the Al content to the Nb content is coordinated by properly regulating the content of the Al element, so that the alloy component has high compactness and no cracks under the preparation of laser additive manufacturing, and excellent high-strength and high-plasticity matching is achieved at high temperature, fe 25Co25Ni25Cr18.75Al2Nb4.25 in the alloy component is subjected to ageing heat treatment at different temperatures, the sample structure is found to be more uniform and higher in compactness, micro holes are hardly seen, the existence of any micro cracks is completely not seen under high multiple, the tensile strength reaches 858.328MPa when the ageing heat treatment is carried out at 600 ℃ +4 hours, the elongation reaches 16.143%, the comprehensive performance of the traditional high-entropy alloy is exceeded, the problem that the high-entropy alloy containing the Al element is easy to crack is solved, and the excellent effects of high strength and high plasticity are also achieved.
Drawings
FIG. 1 is a graph of macroscopic morphology of a deposited state of Fe 25Co25Ni25Cr18.75Al6.25 high-entropy alloy for laser additive manufacturing.
FIG. 2 is a morphology graph of Fe 25Co25Ni25Cr18.75Al6.25 high-entropy alloy as-deposited structural cracks produced by laser additive manufacturing.
FIG. 3 is a microstructure morphology of a deposited state of Fe 25Co25Ni25Cr18.75Al4Nb2.25 high-entropy alloy produced by laser additive manufacturing.
FIG. 4 is a microstructure morphology of a deposited state of Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy produced by laser additive manufacturing.
FIG. 5 is a microstructure morphology of a deposited state of Fe 25Co25Ni25Cr18.75Nb6.25 high-entropy alloy produced by laser additive manufacturing.
Fig. 6 is an XRD pattern of different Al contents of Fe 25Co25Ni25Cr18.75AlxNb(6.25-x) (x= 0,2,4,6.25) high-entropy alloy produced by laser additive.
Fig. 7 is a plot of room temperature tensile engineering stress-strain for Fe 25Co25Ni25Cr18.75AlxNb(6.25-x) (x=0, 2, 4) high-entropy alloy samples of different Al contents for laser additive manufacturing.
FIG. 8 is a microstructure morphology graph of the Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy produced by laser additive at 600 ℃ +4h aging heat treatment.
FIG. 9 is a microstructure morphology graph of the Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy produced by laser additive after 700 ℃ +4h aging heat treatment.
FIG. 10 is a microstructure morphology of the Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy 800 ℃ plus 4h aging heat treatment manufactured by laser additive.
FIG. 11 is an XRD pattern of a Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy produced by laser additive manufacturing before and after heat treatment.
FIG. 12 is a plot of room temperature tensile engineering stress-strain for samples of Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy manufactured by laser additive at different heat treatment temperatures.
Detailed Description
Example 1
According to the cluster+connecting atomic model, the high-density crack-free Al-containing high-entropy alloy is designed, the molecular formula is Fe 25Co25Cr18.75Ni25AlxNb(6.25-x), the cluster model type is [ (Al xNb(6.25-x))-(FeCoNi)75]Cr18.75), and the atomic ratio sum of Al and Nb is 6.25.
The preparation method comprises the following steps:
According to an atomic mole ratio of 25:25:25:18.75: x: (6.25-x) (x= 0,2,4,6.25) the Fe, co, cr, ni, al, nb metal powder was weighed and prepared as an alloy powder. The purity of raw material Fe, co, ni, cr, al, nb is not lower than 99.95wt.%, and raw material Fe, co, ni, cr, al, nb is spherical powder.
Placing the prepared alloy powder into a stainless steel ball grinding tank for ball milling for 1h, sieving by a 100-mesh sieve, and placing into a vacuum drying oven at 100-120 ℃ for preservation for more than 2 h.
304L stainless steel with the size of 100 multiplied by 10mm 3 is selected as a base material, and oxide skin and surface stains on the cladding surface of the base material are removed.
Under the protection of argon atmosphere, under the condition of a certain powder feeding rate, the alloy powder is lapped, melted and deposited on the surface of the base material layer by layer from bottom to top by adopting a coaxial powder feeding mode through a laser additive manufacturing technology, so as to obtain a deposited high-entropy alloy sample. Wherein the pressure rate of the protector is 5L/min, and the oxygen content in the argon filling environment is not higher than 50ppm; the laser power is 1000-1100w, the moving speed is 15mm/s, the powder feeding speed is 2r/min, the layer height is 0.35mm, and the laser spot diameter is 3mm; the thickness of the deposited high-entropy alloy sample is 0.3-0.4mm.
The high-entropy alloy sample in the deposition state of [ (Al 2Nb4.25)-(FeCoNi)75]Cr18.75) manufactured by laser additive is placed in a muffle furnace and subjected to ageing heat treatment for 4 hours at the temperature of 600 ℃ and the temperature of 700 ℃ and 800 ℃ respectively, the heat treatment can effectively eliminate component segregation and separate out beneficial phases, crystal grains can be refined to improve mechanical properties, internal stress is reduced to avoid cracks or slow down holes, the defect problem is effectively solved, the prepared high-entropy alloy has higher compactness and more uniform structure, the forming precision of the sample is higher, and the high-entropy alloy with high performance is obtained.
Experimental analysis
FIG. 1 is a graph of macroscopic morphology of a deposited state of Fe 25Co25Ni25Cr18.75Al6.25 high-entropy alloy for laser additive manufacturing. FIG. 2 is a morphology graph of as-deposited structural cracks of Fe 25Co25Ni25Cr18.75Al6.25 high-entropy alloy produced by laser additive, with significant voids and numerous cracks and typical along-grain cracking. FIG. 3 is a microstructure topography of a deposited state of a Fe 25Co25Ni25Cr18.75Al4Nb2.25 high-entropy alloy produced by laser additive manufacturing, with the structure being typical of dendrites, and void and crack elimination. FIG. 4 is a microstructure morphology of a Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy produced by laser additive manufacturing in a deposited state before heat treatment, the microstructure being dendrite and crack-free. FIG. 5 is a microstructure morphology of a deposited state of the Fe 25Co25Ni25Cr18.75Nb6.25 high-entropy alloy produced by laser additive, and the microstructure is more compact. Fig. 6 shows XRD patterns of Fe 25Co25Ni25Cr18.75AlxNb(6.25-x) (x= 0,2,4,6.25) high-entropy alloy manufactured by laser additive with different Al contents, the structure is a single FCC structure, and the main diffraction peaks shift to the right with increasing Al content. FIG. 7 is a plot of room temperature tensile engineering stress-strain for samples of Fe 25Co25Ni25Cr18.75AlxNb(6.25-x) (x=0, 2, 4) high-entropy alloy of laser additive manufacturing with different Al content; when x=0, the alloy has higher tensile strength, which is up to 782.842Mpa; when x=2, the strength and plastic matching of the alloy are balanced, wherein the tensile strength is 787.395Mpa, and the elongation is 14.1823%; when x=4, the elongation of the high-entropy alloy is up to 34.5572%, and the high-entropy alloy has excellent plasticity. FIG. 8 is a graph of the microstructure morphology of the Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy produced by laser additive at 600 ℃ and 4h aging heat treatment, wherein the holes of the microstructure are obviously reduced and the microstructure becomes more compact after the heat treatment. FIG. 9 is a microstructure morphology graph of the Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy produced by laser additive after 700 ℃ +4h aging heat treatment. FIG. 10 is a microstructure morphology of the Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy 800 ℃ plus 4h aging heat treatment manufactured by laser additive. FIG. 11 shows XRD patterns of a high-entropy alloy of Fe 25Co25Ni25Cr18.75Al2Nb4.25 produced by laser additive manufacturing before and after heat treatment, the microstructure is a single FCC structure, and the main diffraction peak shifts rightward as the temperature of aging heat treatment increases. FIG. 12 is a plot of room temperature tensile engineering stress-strain for a sample of a laser additive manufactured Fe 25Co25Ni25Cr18.75Al2Nb4.25 high-entropy alloy at different heat treatment temperatures; the strength plastic fit at 600 ℃ plus 4 hours is optimal, the sample structure is more uniform, the density is higher, micro holes are hardly seen, no micro cracks exist under high multiple, the tensile strength reaches 858.328MPa, and the elongation reaches 16.143%; the strength and plasticity at 700 ℃ plus 4h are obviously reduced.
Claims (4)
1. A high-density crack-free laser additive manufacturing method of an Al-containing high-entropy alloy is characterized by comprising the following steps of: the high-entropy alloy has a molecular formula of Fe 25Co25Cr18.75Ni25AlxNb（6.25-x） and a cluster mode type of [ (Al xNb（6.25-x）)-（FeCoNi）75]Cr18.75) wherein x is equal to 2 or 4 ], and the laser additive manufacturing method of the high-entropy alloy comprises the following steps:
s1, according to an atomic mole ratio of 25:25:25:18.75: x: (6.25-x) weighing Fe, co, cr, ni, al, nb metal powder to prepare alloy powder;
s2, placing the prepared alloy powder into a ball milling tank for ball milling for 1h, sieving by a 100-mesh sieve, and placing the alloy powder into a vacuum drying oven at 100-120 ℃ for preservation for more than 2 h;
S3, taking 304L stainless steel as a base material, removing oxide skin and surface stains on the cladding surface of the base material, and performing lap joint, fusion and deposition of alloy powder on the surface of the base material layer by layer under the protection of argon atmosphere by using a laser additive manufacturing technology to obtain a deposited high-entropy alloy sample, wherein the argon pressure rate is 5L/min, and the oxygen content in an argon filling environment is not higher than 50ppm; the laser power is 1000-1100w, the moving speed is 15mm/s, the powder feeding speed is 2r/min, the layer height is 0.35mm, and the laser spot diameter is 3mm.
2. The high-density crack-free laser additive manufacturing method of an Al-containing high-entropy alloy according to claim 1, wherein the method comprises the following steps: the purity of the starting material Fe, co, ni, cr, al, nb is not less than 99.95wt.%.
3. The high-density crack-free laser additive manufacturing method of an Al-containing high-entropy alloy according to claim 1, wherein the method comprises the following steps: raw materials Fe, co, ni, cr, al, nb are spherical powder.
4. The high-density crack-free laser additive manufacturing method of an Al-containing high-entropy alloy according to claim 1, wherein the method comprises the following steps: the thickness of the deposited high-entropy alloy sample is 0.3-0.4mm.
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| CN111850543A (en) * | 2020-06-22 | 2020-10-30 | 昆明理工大学 | Laser cladding seven-element high-entropy alloy coating and preparation method thereof |
| CN114150205A (en) * | 2021-11-26 | 2022-03-08 | 中国航发北京航空材料研究院 | High-temperature-resistant high-entropy alloy with high room-temperature plasticity and preparation method thereof |
| CN114457272A (en) * | 2022-02-11 | 2022-05-10 | 吉林大学 | High-entropy alloy and method for repairing tungsten-based powder alloy die-casting die by laser cladding |
| WO2022252541A1 (en) * | 2021-06-01 | 2022-12-08 | 中国矿业大学 | Ni-co-fe-b eutectic high-entropy alloy, and preparation method therefor and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111850543A (en) * | 2020-06-22 | 2020-10-30 | 昆明理工大学 | Laser cladding seven-element high-entropy alloy coating and preparation method thereof |
| WO2022252541A1 (en) * | 2021-06-01 | 2022-12-08 | 中国矿业大学 | Ni-co-fe-b eutectic high-entropy alloy, and preparation method therefor and use thereof |
| CN114150205A (en) * | 2021-11-26 | 2022-03-08 | 中国航发北京航空材料研究院 | High-temperature-resistant high-entropy alloy with high room-temperature plasticity and preparation method thereof |
| CN114457272A (en) * | 2022-02-11 | 2022-05-10 | 吉林大学 | High-entropy alloy and method for repairing tungsten-based powder alloy die-casting die by laser cladding |
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