CN111250693A - High-entropy alloy powder for additive remanufacturing and preparation method thereof - Google Patents
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- 239000000956 alloy Substances 0.000 title claims abstract description 74
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 74
- 239000000843 powder Substances 0.000 title claims abstract description 64
- 239000000654 additive Substances 0.000 title claims abstract description 24
- 230000000996 additive effect Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 238000005516 engineering process Methods 0.000 claims abstract description 11
- 230000006698 induction Effects 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000007712 rapid solidification Methods 0.000 claims abstract description 10
- 238000009689 gas atomisation Methods 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000000889 atomisation Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
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- 150000002739 metals Chemical class 0.000 abstract description 4
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- 238000013401 experimental design Methods 0.000 abstract description 2
- 238000003723 Smelting Methods 0.000 abstract 2
- 238000010586 diagram Methods 0.000 description 4
- 238000004372 laser cladding Methods 0.000 description 4
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- 238000010438 heat treatment Methods 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- B22F1/0003—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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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
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention discloses high-entropy alloy powder for additive remanufacturing and a preparation method thereof, wherein the atomic expression of the high-entropy alloy powder is Al0.4CoCu0.6NiSi0.2The granularity interval is 50-150 mu m, and the preparation method comprises the following steps: sequentially putting the block materials of all metals into a vacuum induction smelting furnace according to the sequence of melting points from low to high in atomic percentage for vacuum induction smelting, and then adopting a gas atomization rapid solidification technology to prepare the alloy. The invention obtains a high-entropy alloy formula without Fe element and rare metal through a large number of experimental designs, and high-entropy alloy powder is prepared by combining a gas atomization rapid solidification technology, and the high-entropy alloy powder has relatively uniform structural components, higher sphericity and higher fluidityGood, low oxygen content, high powder yield, good quality, simple fcc + trace bcc solid solution phase structure, high microhardness, and can be applied to the field of high-entropy alloy additive remanufacturing and forming.
Description
Technical Field
The invention belongs to the technical field of high-entropy alloy additive remanufacturing, and particularly relates to high-entropy alloy powder for additive remanufacturing and a preparation method thereof.
Background
The high-entropy alloy is a high-mixed-entropy alloy with various main elements, and has excellent comprehensive properties of high strength, high hardness, good plasticity, excellent wear resistance and corrosion resistance, better thermal stability, high oxidation resistance and the like.
At present, relatively more researches are still conducted on the application of the high-entropy alloy in the preparation of the coating, and in recent years, the research on the application of the high-entropy alloy in the additive remanufacturing is gradually increased.
However, the high-entropy alloy powder for additive remanufacturing is basically pure metal powder which is mechanically mixed, and due to the difference of physical properties such as melting points of different metal powders, part of powder in a formed structural member/layer is not melted or is partially melted, so that the defects of uneven structure, serious component segregation, low solid solubility and the like are caused, and further the comprehensive performance of the formed structural member/layer is affected.
In addition, most of the conventional high-entropy alloy powders contain Fe element and/or rare metal.
For the high-entropy alloy powder containing rare metals, the rare metals are expensive, so that the cost is high, and the high-entropy alloy powder is not suitable for industrial large-scale application, and most of the high-entropy alloy powder containing rare metals is poor in plasticity and is not suitable for additive remanufacturing (see literature 1).
For high-entropy alloy powder containing Fe, many researches are currently conducted mainly on AlCoCrFeNi or cocrfmnni series, and when the two series are used for additive remanufacturing, most of the mechanical strength is not ideal under the condition of ensuring plasticity (see documents 2 and 3).
However, there is a problem with the high-entropy alloy powder containing Fe element: in the material increasing remanufacturing process, due to solid solution diffusion among elements, elements in the high-entropy alloy can be dissolved into a base body, the elements in the base body can also be dissolved into the high-entropy alloy, the Fe base body is the most commonly used base body in the aspect of material increasing remanufacturing, if the designed high-entropy alloy contains the Fe element, the high-entropy alloy components at the combination interface can be changed, and phase change is even caused, so that the comprehensive performance of the high-entropy alloy is greatly influenced.
Document 1: yaojiang ZHao et al, "A hexagonal close-packed high-entry ally: the effect of error ", Materials & Design 2016, 96, pages 10-15.
Document 2: zhiguang Zhu et al, "high micro structure and string help mechanisms of a CoCrFeNiMn high entry aggregate augmented reality gained by systematic laser replacement", Scaripta Materialia 2018, p.154, p.20-24.
Document 3: yevgeni Brif et al, "The use of high-entry alloys in additive manufacturing" year 2015, 99 th year, pages 93-96.
Disclosure of Invention
The invention aims to solve the problems and provides high-entropy alloy powder for additive remanufacturing, which is uniform in components, good in flowability, low in oxygen content and particularly free of Fe element and rare metal, and a preparation method thereof.
The technical scheme for realizing the purpose of the invention is as follows: high-entropy alloy powder for additive remanufacturing, wherein the atomic expression of the high-entropy alloy powder is Al0.4CoCu0.6NiSi0.2。
The particle size interval of the high-entropy alloy powder for additive remanufacturing is 50-150 mu m.
The high-entropy alloy powder for additive remanufacturing is prepared by adopting an air atomization rapid solidification technology.
The preparation method of the high-entropy alloy powder for additive remanufacturing comprises the following steps:
① preparing block materials of each metal, removing impurities and oxide film on the surface of each metal block material by a grinder, and mixing according to atomic percentage.
② putting the metal block materials into a vacuum induction melting furnace in sequence from low melting point to high melting point, and carrying out vacuum induction melting under the protection of argon.
③ the Al is prepared by directly adopting the gas atomization rapid solidification technology to the metal liquid obtained by vacuum induction melting in the step ②0.4CoCu0.6NiSi0.2High entropy alloy powder.
The gas atomization rapid solidification technology in the step ③ adopts gas pressure of 2-5 MPa, gas flow velocity of 100-160 mm/s, liquid flow diameter of 5-10 mm and gas flow jet angle of 30-60 degrees.
The invention has the following positive effects: according to the invention, a high-entropy alloy formula without Fe element and rare metal is obtained through a large number of experimental designs, and high-entropy alloy powder is prepared by combining a gas atomization rapid solidification technology, and the high-entropy alloy powder has relatively uniform structural components, higher sphericity, better fluidity, lower oxygen content, higher powder yield and better quality, has a simple fcc + trace bcc solid solution phase structure, has higher microhardness, and can be applied to the field of high-entropy alloy additive remanufacturing and forming.
Drawings
FIG. 1 shows Al obtained in example 10.4CoCu0.6NiSi0.2SEM image of high entropy alloy powder; wherein, the a picture is a surface overall morphology SEM picture, and the b picture is a surface morphology SEM picture (partial enlarged view) of powder particles with larger particle sizes.
FIG. 2 shows Al obtained in example 10.4CoCu0.6NiSi0.2The relationship graph of the mass accumulation distribution of the high-entropy alloy powder and the particle size.
FIG. 3 shows Al obtained in example 10.4CoCu0.6NiSi0.2XRD patterns of the high-entropy alloy powder in different particle size intervals.
FIG. 4 shows Al obtained in example 10.4CoCu0.6NiSi0.2The microhardness of the high-entropy alloy powder in different particle size ranges.
Fig. 5 is a schematic diagram of the "staggered" forming path adopted in application example 1.
FIG. 6 shows Al obtained in application example 10.4CoCu0.6NiSi0.2The high-entropy alloy forming structure has the geometric shape of a real object.
FIG. 7 shows Al obtained in application example 10.4CoCu0.6NiSi0.2XRD pattern of high entropy alloy formed structure.
FIG. 8 shows Al obtained in application example 10.4CoCu0.6NiSi0.2The stress-strain curve diagram of the room-temperature tensile engineering of the high-entropy alloy forming structure.
Detailed Description
(example 1)
The preparation method of the high-entropy alloy powder for additive remanufacturing of the embodiment comprises the following steps:
① lump of Al, Co, Cu, Ni, SiRemoving impurities and oxide film on the surface of the metal by using a grinder (the purity is more than or equal to 99.9%), and then removing Al according to atomic percentage0.4CoCu0.6NiSi0.2Ingredients, the total weight is 20 kg.
② placing the metal block materials of step ① into a vacuum induction melting furnace in sequence from low melting point to high melting point, and vacuumizing until the vacuum degree is less than 2.5 multiplied by 10-3MPa, then argon is filled to the pressure of 5 multiplied by 10-2And Pa, under the condition of argon protection, heating and melting the alloy through an induction coil to start melting, wherein the melting time is 30min, and electromagnetic stirring is introduced in the melting process to ensure the uniformity of alloy components.
③ introducing nitrogen through a tightly coupled annular slot nozzle of an atomizing device until the pressure is 4MPa, the airflow velocity is 130mm/s, the liquid flow diameter is 8mm, the airflow jet angle is controlled at 45 degrees, and Al is prepared from the metal liquid obtained by vacuum induction melting in the step ② by directly adopting an air atomization rapid solidification technology0.4CoCu0.6NiSi0.2High entropy alloy powder.
(test example 1)
Observation of Al obtained in example 10.4CoCu0.6NiSi0.2SEM images of the high entropy alloy powder, and the results are shown in FIG. 1.
Wherein, the a picture is a surface overall morphology SEM picture, and the b picture is a surface morphology SEM picture (partial enlarged view) of powder particles with larger particle sizes.
As can be seen from diagram a in fig. 1: the high-entropy alloy powder prepared by the invention has uniform particles, is basically spherical and has good sphericity, which shows that the high-entropy alloy powder has good fluidity.
As can be seen from the b diagram in fig. 1: the satellite balls exist on the surfaces of the powder particles with larger particle sizes, mainly due to different cooling speeds of the powder, the cooling speed of the powder with small particle sizes is higher, the cooling speed of the powder with large particle sizes is relatively lower, when the smaller liquid drops are solidified, the large liquid drops can be still in a liquid state or a semi-solid state, and the small particles in the solidified state can be embedded on the surfaces of the large particles when colliding with the large particles which are not solidified.
(test example 2)
Al obtained in example 10.4CoCu0.6NiSi0.2The high-entropy alloy powder is sieved into three granularity intervals of-50 microns (namely less than 50 microns), 50-150 microns and +150 microns (namely more than 150 microns).
The graph of mass cumulative distribution versus particle size is shown in FIG. 2.
As can be seen from fig. 2: the high-entropy alloy powder prepared by the method has a wide particle size distribution range, the mass fraction of most of the high-entropy alloy powder is not more than 150 mu m (the mass fraction is about 90%), the mass fraction of the high-entropy alloy powder of 50-150 mu m (namely used for additive remanufacturing) is about 70%, and the powder yield is high.
(test example 3)
Al obtained in example 1 was tested0.4CoCu0.6NiSi0.2XRD patterns of three different particle size intervals of the high-entropy alloy powder show that the result is shown in figure 3.
As can be seen in fig. 3: the phase structure of three different particle size intervals is fcc + trace bcc, and the bcc phase content increases with decreasing particle size.
(test example 4)
Al obtained in example 1 was tested0.4CoCu0.6NiSi0.2The microhardness of the high-entropy alloy powder in three different particle size intervals is shown in figure 4.
As can be seen from fig. 4, the microhardness decreases significantly with increasing particle size.
(test example 5)
Al prepared in example 1 was tested by ON-3000 oxynitridometer0.4CoCu0.6NiSi0.2The oxygen content of the high-entropy alloy powder is 165ppm, the oxygen content of the powder is low, and the use requirement is met.
(application example 1)
The application example is to prepare a high-entropy alloy forming structure from the high-entropy alloy powder prepared in the embodiment 1, and the specific method comprises the following steps:
s1: and (4) preparing a substrate.
Cutting No. 45 steel wire into rectangular block samples with the size of 150 × 100 × 30mm, sequentially grinding off oxide skin on the surfaces of the samples by 200#, 400# and 800# sandpaper, repeatedly cleaning the surfaces by acetone and alcohol respectively, finally drying and packaging to obtain a base for later use.
S2: and (4) preparing powder.
Al prepared in example 1 and having a particle size range of 50 to 150 μm0.4CoCu0.6NiSi0.2And (3) placing the high-entropy alloy powder in a drying oven, drying for 2h at the temperature of 120 ℃, and removing water to increase the flowability of the powder.
S3: and preparing the high-entropy alloy forming structure by adopting a laser cladding forming technology.
The forming path adopted by the laser cladding of S3 is a "staggered" forming path (see fig. 5), that is, a layer is deposited along the X direction (or Y direction), then two layers are deposited on the layer [ Z direction ] along the Y direction (or X direction), then two layers are deposited on the two layers along the X direction (or Y direction), and so on, and finally a layer is deposited along the X direction (or Y direction).
The main technological parameters adopted in the forming process are as follows: the diameter of a light spot is 4.5mm, the powder feeding rate is 25g/min, the laser power is 2600W, and the scanning speed is 12 mm/s.
In order to reduce the influence of oxidation in the forming process, argon continuously flowing (the flow rate is 15L/min) is adopted as a protective gas in the laser cladding process.
To reduce residual stress, the substrate is first prescanning three times before laser cladding forming deposition begins, and the substrate is preheated to reduce the temperature gradient between the forming structure and the substrate.
The high-entropy alloy forming structure object manufactured in the application example 1 is shown in fig. 6, and can be seen from fig. 6: the forming structure has good surface macroscopic appearance and average geometric dimension: the length x height is about 80 x 14 mm.
The XRD phase analysis result of the high-entropy alloy formed structure obtained in application example 1 is shown in FIG. 7, and it can be seen from FIG. 7 that: the phase composition of the formed structure is mainly fcc plastic phase, and contains trace bcc strengthening phase.
The high-entropy alloy forming structure prepared by the application example 1 is subjected to room temperature quasi-static compression, and the room temperature tensile engineering stress-strain curve is shown in fig. 8, which can be seen from fig. 8: the forming structure has the advantages that the tensile strength can reach 1195.6MPa, the yield strength can reach 662.0MPa, the elongation can reach 14.5 percent without heat treatment, the forming structure has high strength and excellent plasticity, and the strong plasticity balance is realized.
Claims (5)
1. High-entropy alloy powder for additive remanufacturing, wherein the atomic expression of the high-entropy alloy powder is Al0.4CoCu0.6NiSi0.2。
2. A high entropy alloy powder for additive remanufacturing according to claim 1, wherein: the particle size range is 50-150 μm.
3. A high entropy alloy powder for additive remanufacturing according to claim 1 or 2, wherein: is prepared by adopting an air atomization rapid solidification technology.
4. A method of preparing the high entropy alloy powder for additive remanufacturing of claim 1 or 2, having the steps of:
① preparing block materials of each metal, removing impurities and oxide films on the surface of each metal block material by a grinder, and mixing according to atomic percentage;
②, sequentially putting the metal block materials into a vacuum induction melting furnace according to the sequence of melting points from low to high, and carrying out vacuum induction melting under the protection of argon;
③ the Al is prepared by directly adopting the gas atomization rapid solidification technology to the metal liquid obtained by vacuum induction melting in the step ②0.4CoCu0.6NiSi0.2High entropy alloy powder.
5. The method for preparing high-entropy alloy powder for additive remanufacturing according to claim 4, wherein the gas atomization rapid solidification technology in the step ③ adopts gas pressure of 2-5 MPa, gas flow velocity of 100-160 mm/s, liquid flow diameter of 5-10 mm, and gas flow jet angle of 30-60 °.
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| CN111763868A (en) * | 2020-06-29 | 2020-10-13 | 安徽盛赛再制造科技有限公司 | High-entropy alloy powder for additive manufacturing and preparation method thereof |
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