CN110777276A - Method for enhancing performance of alloy by using aluminum oxide based on laser 3D printing - Google Patents

Method for enhancing performance of alloy by using aluminum oxide based on laser 3D printing Download PDF

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CN110777276A
CN110777276A CN201911012960.9A CN201911012960A CN110777276A CN 110777276 A CN110777276 A CN 110777276A CN 201911012960 A CN201911012960 A CN 201911012960A CN 110777276 A CN110777276 A CN 110777276A
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powder
alloy
laser
aluminum
printing
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CN110777276B (en
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陈汪林
李炳新
王成勇
颜安
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Guangdong University of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y80/00Products made by additive manufacturing

Abstract

The invention belongs to the technical field of additive manufacturing, and particularly relates to a method for enhancing alloy performance by using aluminum oxide based on laser 3D printing. The method creatively utilizes local high temperature formed in the printing process by the laser 3D printing technology to promote the in-situ exchange reaction of aluminum and ferric oxide, further limits the powder feeding quantity ratio of aluminum powder to ferric oxide powder to be 1 (2-5), has the particle size of 20-100 mu m, and can uniformly distribute the generated fine nano-grade aluminum oxide in an alloy system along with the promotion of the precipitation process of the alloy powder, thereby solving the problem of nano-phase agglomeration and floating, obviously enhancing the mechanical property and quality uniformity of the alloy, having simple operation and being suitable for large-scale industrial production.

Description

Method for enhancing performance of alloy by using aluminum oxide based on laser 3D printing
Technical Field
The invention belongs to the technical field of additive manufacturing. And more particularly, to a method for enhancing the performance of an alloy based on laser 3D printed aluminum oxide.
Background
The alloy is a substance with metal characteristics, which is synthesized by two or more than two metals and metals or nonmetals through a certain method, has the advantages of high hardness, corrosion resistance, excellent conductivity and the like, and is widely used in the fields of aerospace, petroleum, chemical industry, electric power, ocean and the like. The rapid development of modern industry has increased the demand for alloys, and higher requirements for the strength of the alloys are also put forward.
At present, the following three methods are commonly used for enhancing the performance of the alloy: firstly, microalloying refers to adding a proper amount of one or more microalloyed alloy elements on the basis of alloy to strengthen the alloy performance; secondly, fine grain strengthening refers to improving the strength of the alloy through grain size refinement; third, nano-reinforcement, refers to the enhancement of alloy properties by adding a nanophase during alloy preparation. Among them, the first and second methods have been studied in the industry for many years, and also achieved fruitful results; the third nano alloy strengthening method is still under exploration, the technology is not mature, and the problems of segregation and thermal cracking caused by the fact that nano phases are small in diameter, easy to agglomerate, much lower in density than alloy liquid and easy to agglomerate and float in the smelting process exist. Therefore, how to obtain the reinforced alloy material with the nano-phase dispersed distribution becomes a research difficulty in the industry at present.
On the other hand, the laser 3D printing technology is one of the emerging technologies in recent years, has the characteristics of highly concentrated heat source, small dilution, small heat affected zone and the like, and has the special advantage of combining excellent material performance with an accurate manufacturing process, and is very suitable for manufacturing functional parts with complex spatial structures and spatial arrangement of organization components, and can also be applied to the field of alloy manufacturing. For example, chinese patent application CN108465807A discloses a high-strength Al-Mg-Sc alloy powder, a preparation method thereof, an application in 3D printing, and a 3D printing method thereof, in which the method includes defining mass percentages of each element, preparing rare earth high-strength Al-Mg-Sc alloy powder by vacuum melting, and preparing high-strength and high-elongation aluminum alloy by 3D printing, but the method requires premixing and preparation of alloy powder, the preparation steps are complicated in the early stage, and if the alloy powder is not uniformly mixed, the quality of the aluminum alloy may be uneven.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects and shortcomings of nano-phase agglomeration and floating and complicated 3D alloy printing steps in the prior art during nano-reinforcement, and provides a method for dispersing and distributing nano-phase alumina based on laser 3D printing, improving the alloy performance and having simple steps.
The above purpose of the invention is realized by the following technical scheme:
a method for enhancing alloy performance based on aluminum oxide printed by laser 3D comprises the following steps:
starting a laser, setting powder feeding quantity parameters of alloy powder, ferric oxide powder and aluminum powder to enable the powder feeding quantity ratio of the aluminum powder to the ferric oxide powder to be 1 (2-5), and carrying out laser 3D printing on the cleaned alloy substrate to obtain an aluminum oxide reinforced alloy;
wherein the particle sizes of the iron oxide powder and the aluminum powder are 20-100 mu m.
The invention utilizes the local high temperature formed by the laser 3D printing technology in the printing process to promote the in-situ exchange reaction of aluminum and ferric oxide, and the generated fine nanometer alumina can be uniformly distributed in an alloy system along with the promotion of the precipitation process of alloy powder, thereby forming heterogeneous nucleation particles in the solidification process of a molten pool, refining the grain size of the alloy and obviously enhancing the mechanical property and quality uniformity of the alloy.
Preferably, the powder feeding amount ratio of the aluminum powder to the iron oxide powder is 1 (2-3).
More preferably, the ratio of the amount of the aluminum powder to the amount of the iron oxide powder fed is 1: 3.
Preferably, the particle sizes of the iron oxide powder and the aluminum powder are 40-80 μm.
More preferably, the particle sizes of the iron oxide powder and the aluminum powder are 80 μm.
Among them, the particle diameters and the powder feeding amounts of the aluminum powder and the iron oxide powder have a significant influence on the dispersion. The particle size is too large, so that the replacement reaction is insufficient, and the mechanical property of the alloy material is reduced due to the large particle size of the produced alumina particles; the particle size is too small, the powder is easy to agglomerate, the melting is insufficient, the pore content is increased, and the mechanical property of the alloy material is also reduced. Meanwhile, the proportion of the aluminum powder and the ferric oxide powder also needs to be reasonably controlled, and when the aluminum powder is excessive, the aluminum powder can react with the generated iron to produce a brittle FeAl intermetallic compound, so that the mechanical property of the alloy material is reduced; the mechanical properties of the alloy material are also reduced when the iron oxide powder is excessive.
Further, the amount of the aluminum powder fed is 0.3 to 1.7 g/min.
Preferably, the amount of the aluminum powder fed is 1 to 1.7 g/min.
More preferably, the amount of the aluminum powder to be fed is 1 g/min.
Further, the powder feeding amount of the iron oxide powder is 1 to 5 g/min.
Preferably, the powder feeding amount of the iron oxide powder is 3-5 g/min.
More preferably, the powder feeding amount of the iron oxide powder is 3 g/min.
Further, the powder feeding amount of the alloy powder is 10-15 g/min.
Preferably, the powder feeding amount of the alloy powder is 12-15 g/min.
More preferably, the powder feeding amount of the alloy powder is 12 g/min.
Still further, the parameters further include: the laser power is set to be 600-900W, the scanning speed is 8-12 mm/s, the diameter of a light spot is 2-3 mm, argon is used as shielding gas and powder conveying gas, and the flow rate is 10-15L/min.
Preferably, the parameters further include: setting the laser power at 800W, the scanning speed at 10mm/s, the spot diameter at 2mm, argon as the shielding gas and the powder feeding gas, and the flow rate at 12L/min.
Further, the alloy in the alloy substrate and the alloy powder is nickel-based alloy, iron-based alloy or aluminum-based alloy.
Preferably, the alloy in the alloy substrate and the alloy powder is a nickel-based alloy.
Furthermore, the laser 3D printing is powder feeding type laser 3D printing or selective laser 3D printing.
Preferably, the laser 3D printing is powder feeding type laser 3D printing.
Further, the cleaning method comprises deoiling and degreasing.
The invention has the following beneficial effects:
the invention creatively provides a brand-new method for enhancing the performance of an alloy by using aluminum oxide based on laser 3D printing, local high temperature formed in the printing process by using the laser 3D printing technology can promote the in-situ exchange reaction of aluminum and iron oxide, the powder feeding quantity ratio of aluminum powder and iron oxide powder is further limited to be 1 (2-5), the particle size is 20-100 mu m, the generated fine nano-grade aluminum oxide can be uniformly distributed in an alloy system along with the promotion of the precipitation process of the alloy powder, the problem of nano-phase agglomeration and floating is solved, the mechanical property and the quality uniformity of the alloy are obviously enhanced, the operation is simple, and the method is suitable for large-scale industrial production.
Drawings
FIG. 1 is a schematic diagram of a printing table for preparing an alumina reinforced nickel-based alloy based on powder feeding type 3D printing in embodiment 1 of the invention.
FIG. 2 is a scanning electron micrograph of nickel-based alloys prepared according to example 1 of the present invention and comparative example 1;
wherein, (a) -a scanning electron micrograph of the nickel-based alloy prepared in comparative example 1, 20 μm; (b) scanning electron micrograph of nickel-base alloy prepared in example 1, 20 μm; (c) scanning electron micrograph of the nickel-base alloy prepared in example 1, 3 μm.
FIG. 3 is a spectrum of an alumina reinforced nickel-base alloy made in accordance with example 1 of the present invention.
FIG. 4 is a TEM topographic map of the alumina-enhanced nickel-based alloy prepared in example 1 of the present invention.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1 an alumina reinforced nickel base alloy based on laser 3D printing
The aluminum oxide reinforced nickel-based alloy is prepared by the following method:
firstly, deoiling and degreasing a 718 nickel-based alloy substrate purchased in the market, carrying out surface cleaning treatment, starting a laser, setting the powder feeding amount of aluminum powder to be 1g/min, the powder feeding amount of ferric oxide powder to be 3g/min, and the powder feeding amount of nickel-based alloy powder to be 12g/min, wherein the particle sizes of the ferric oxide powder and the aluminum powder are both 80 microns, and other process parameters are set as follows: the laser power is 800W, the scanning speed is 10mm/s, the diameter of a light spot is 2mm, argon gas is used as shielding gas and powder feeding gas, the flow rate is 12L/min, and laser 3D printing is carried out on the nickel-based alloy substrate with the surface being cleaned, so that the aluminum oxide reinforced nickel-based alloy is obtained.
Embodiment 2 an alumina reinforced nickel-based alloy based on laser 3D printing
The aluminum oxide reinforced nickel-based alloy is prepared by the following method:
firstly, deoiling and degreasing a 718 nickel-based alloy substrate purchased in the market, carrying out surface cleaning treatment, starting a laser, setting the powder feeding amount of iron oxide powder to be 1g/min, the powder feeding amount of aluminum powder to be 0.3g/min and the powder feeding amount of nickel-based alloy powder to be 8g/min, wherein the particle sizes of the iron oxide powder and the aluminum powder are both 60 micrometers, and other process parameters are set as follows: the laser power is 900W, the scanning speed is 8mm/s, the diameter of a light spot is 3mm, argon gas is used as shielding gas and powder feeding gas, the flow rate is 10L/min, and laser 3D printing is carried out on the nickel-based alloy substrate with the surface being cleaned, so that the aluminum oxide reinforced nickel-based alloy is obtained.
Embodiment 3 an alumina reinforced nickel-based alloy based on laser 3D printing
The aluminum oxide reinforced nickel-based alloy is prepared by the following method:
firstly, deoiling and degreasing a 718 nickel-based alloy substrate purchased in the market, carrying out surface cleaning treatment, starting a laser, setting the powder feeding amount of iron oxide powder to be 5g/min, the powder feeding amount of aluminum powder to be 1.7g/min and the powder feeding amount of nickel-based alloy powder to be 15g/min, wherein the particle sizes of the iron oxide powder and the aluminum powder are both 40 micrometers, and other process parameters are set as follows: the laser power is 600W, the scanning speed is 12mm/s, the diameter of a light spot is 3mm, argon gas is used as shielding gas and powder feeding gas, the flow rate is 15L/min, and laser 3D printing is carried out on the nickel-based alloy substrate with the surface being cleaned, so that the aluminum oxide reinforced nickel-based alloy is obtained.
Example 4 an alumina reinforced titanium-based alloy based on laser 3D printing
The difference from example 1 is that the alloy substrate and the alloy powder of example 4 are titanium-based alloy, and the rest parameters and operation refer to example 1, and the titanium-based alloy reinforced by alumina is prepared.
Example 5 an alumina reinforced iron-based alloy based on laser 3D printing
The difference from example 1 is that the alloy substrate and the alloy powder of example 5 are iron-based alloys, and the rest parameters and operations refer to example 1, and an alumina-reinforced iron-based alloy is prepared.
The specific schematic diagram of the aluminum oxide reinforced nickel-based alloy prepared based on laser 3D printing in example 1 is shown in fig. 1, and electron microscopic scanning and energy spectrum measurement are performed on the prepared aluminum oxide reinforced nickel-based alloy, so that fig. 2-4 are obtained.
As can be seen from fig. 3 and 4, the particle phase mainly contains Al and O elements, which indicates that the nano-scale particles are alumina nano precipitated phase; and the particles can effectively pin dislocation, and the precipitation strengthening effect of the particles is achieved. Examples 2-5 are illustrated with reference to example 1, and the electron micrographs and energy spectra of examples 2-5 are similar to example 1.
Comparative example 1 nickel-based alloy based on laser 3D printing
The nickel-based alloy is prepared by the following method:
firstly, deoiling and degreasing the surface of a 718 nickel-based alloy substrate purchased in the market, starting a laser, setting the powder feeding amount of nickel-based alloy powder to be 12g/min, and setting other process parameters as follows: the laser power is 800W, the scanning speed is 10mm/s, the diameter of a light spot is 2mm, argon gas is used as shielding gas and powder feeding gas, the flow rate is 12L/min, and laser 3D printing is carried out on the alloy substrate after surface cleaning treatment to obtain the nickel-based alloy.
The prepared nickel-based alloy was subjected to electron microscopic scanning, and as shown in fig. 2, when compared with the electron microscopic scanning image of the nickel-based alloy reinforced with alumina of example 1, it can be seen from fig. 2 that high-density nanophase was precipitated in the nickel-based alloys (b) and (c) of example 1, while nanophase was not precipitated in the nickel-based alloy (a) of comparative example 1.
Comparative example 2 nickel-based alloy based on laser 3D printing
The difference from example 1 is that in comparative example 2, the powder feeding amount of iron oxide powder was set to 1g/min and the powder feeding amount of aluminum powder was set to 1g/min, and the rest of the parameters and operations were referred to example 1 to prepare a nickel-based alloy.
Comparative example 3 Nickel-based alloy based on laser 3D printing
The difference from example 1 is that in comparative example 3, the powder feeding amount of iron oxide powder was set to 0.5g/min and the powder feeding amount of aluminum powder was set to 3g/min, and the rest of the parameters and operations refer to example 1, and a nickel-based alloy was prepared.
Comparative example 4 Nickel-based alloy based on laser 3D printing
Except for the difference from example 1 in that the iron oxide powder particle size and the aluminum powder particle size described in comparative example 4 are 150 μm, and the rest parameters and operations refer to example 1, a nickel-based alloy was prepared.
Experimental example 1 mechanical Property test
The mechanical properties of the alloys prepared in examples 1-5 and comparative examples 1-4 were determined with reference to the national standard GB/T3098.1-2010, and the results are shown in Table 1.
TABLE 1 determination of mechanical Properties of Nickel-base alloys
Group of Hardness (HV) Yield strength (MPa) Tensile strength (MPa) Elongation (%)
Example 1 356 1178.9 1488.6 10.7
Example 2 345 1126.3 1435.6 9.8
Example 3 336 1054.3 1385.8 8.5
Example 4 518 789.4 976.4 13.4
Example 5 568 719.2 867.6 7.4
Comparative example 1 316 898.4 1003.4 8.9
Comparative example 2 312 716.6 989.7 6.1
Comparative example 3 334 878.9 1088.6 6.7
Comparative example 4 306 918.4 1016.8 8.9
As can be seen from Table 1, compared with comparative example 1, the alumina reinforced nickel-based alloy prepared in the embodiments 1-3 of the invention enhances the hardness, yield strength and tensile strength of the material, and has little influence on the elongation of the material; compared with the nickel-based alloy prepared in the embodiment 1, the nickel-based alloy prepared in the comparative examples 2-4 has obviously reduced hardness, yield strength, tensile strength and elongation percentage.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. A method for enhancing the performance of an alloy by using aluminum oxide based on laser 3D printing is characterized by comprising the following steps:
starting a laser, setting powder feeding quantity parameters of alloy powder, ferric oxide powder and aluminum powder to enable the powder feeding quantity ratio of the aluminum powder to the ferric oxide powder to be 1 (2-5), and carrying out laser 3D printing on the cleaned alloy substrate to obtain an aluminum oxide reinforced alloy;
wherein the particle sizes of the iron oxide powder and the aluminum powder are 20-100 mu m.
2. The method according to claim 1, wherein the ratio of the amount of the aluminum powder to the amount of the iron oxide powder fed is 1 (2-3).
3. The method according to claim 2, wherein the aluminum powder and the iron oxide powder are fed at a powder feed ratio of 1: 3.
4. The method according to claim 1, wherein the iron oxide powder and the aluminum powder have a particle size of 40 to 80 μm.
5. The method according to claim 1, wherein the amount of the aluminum powder fed is 0.3 to 1.7 g/min.
6. The method according to claim 1, wherein the powder feeding amount of the iron oxide powder is 1 to 5 g/min.
7. The method according to claim 1, wherein the amount of the alloy powder fed is 10 to 15 g/min.
8. The method of claim 1, wherein the parameters further comprise: the laser power is set to be 600-900W, the scanning speed is 8-12 mm/s, the diameter of a light spot is 2-3 mm, argon is used as shielding gas and powder conveying gas, and the flow rate is 10-15L/min.
9. The method according to claim 1, wherein the alloy in the alloy substrate, alloy powder is a nickel-based alloy, an iron-based alloy or an aluminum-based alloy.
10. The method of claim 1, wherein the laser 3D printing is powder fed laser 3D printing or selective laser 3D printing.
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