CN116174733A - Alloy powder, preparation method and application thereof, and part model - Google Patents
Alloy powder, preparation method and application thereof, and part model Download PDFInfo
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- CN116174733A CN116174733A CN202310464343.2A CN202310464343A CN116174733A CN 116174733 A CN116174733 A CN 116174733A CN 202310464343 A CN202310464343 A CN 202310464343A CN 116174733 A CN116174733 A CN 116174733A
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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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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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
- 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
- B33Y70/00—Materials specially adapted for 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
- B33Y80/00—Products made by 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
- C22C21/00—Alloys based on aluminium
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention provides alloy powder, a preparation method and application thereof and a part model. The preparation method of the alloy comprises the following steps: s10: obtaining a metal raw material according to an alloy ratio, and mixing and smelting to obtain a metal melt; s20: transferring the metal melt into an atomization barrel, and atomizing and pulverizing under the environment of protective gas to obtain Al-Mg-Zr alloy powder; wherein, the Al-Mg-Zr alloy powder comprises the following elements in percentage by mass: 6.5 to 10 percent of Mg, 0.5 to 1.5 percent of Zr, 0.5 to 1.5 percent of Si, 0.3 to 1 percent of Mn, less than 0.1 percent of impurity and the balance of Al. The invention fully utilizes Mg, zr, mn, si and other elements to carry out solid solution strengthening, fine crystal strengthening and precipitation strengthening on the aluminum matrix, so that the tensile strength and the elongation of the alloy powder additive manufacturing tensile member are obviously superior to those of Al-Si alloy, the tensile strength can reach more than 450MPa, and the elongation can reach more than 10%.
Description
Technical Field
The invention relates to the technical field of alloy materials, in particular to alloy powder, a preparation method and application thereof and a part model.
Background
In recent years, the requirement of additive manufacturing of complex lightweight aluminum alloy components is also receiving increasing attention due to the important requirement of high-end equipment such as aerospace, rail transit and the like for lightweight and high-performance products. Additive manufacturing is an important method for solving the problem of manufacturing complex structural members, and is an important technology for preparing medium-high strength aluminum alloy.
Currently, the types of aluminum alloys suitable for additive manufacturing technology are limited, commercial aluminum alloys are mainly Al-Si series alloys, such as AlSi10Mg, but the mechanical properties are not high (room temperature tensile strength <400 MPa). Aluminum alloys modified in part by the rare earth scandium (Sc) can achieve high strength and elongation, but expensive Sc has hindered their large-scale use.
Therefore, there is a need in the art for a medium-high strength alloy suitable for additive manufacturing, which has excellent mechanical properties, low cost, and suitable for industrial applications.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of Al-Mg-Zr alloy powder for additive manufacturing, which comprises the following steps: s10: obtaining a metal raw material according to an alloy ratio, and mixing and smelting to obtain a metal melt; s20: transferring the metal melt into an atomization barrel, and atomizing and pulverizing under the environment of protective gas to obtain Al-Mg-Zr alloy powder; wherein, the Al-Mg-Zr alloy powder comprises the following elements in percentage by mass: 6.5 to 10 percent of Mg, 0.5 to 1.5 percent of Zr, 0.5 to 1.5 percent of Si, 0.3 to 1 percent of Mn, less than 0.1 percent of impurity and the balance of Al.
Preferably, in the Al-Mg-Zr alloy powder, the mass ratio of Mg is 7-9%; and/or Zr with the mass ratio of 0.7-1.2%; and/or Si in an amount of 0.7 to 1.2% by mass; and/or Mn in an amount of 0.5 to 0.8% by mass.
In the technical scheme, the Al-Mg-Zr alloy powder is used in the field of additive manufacturing, and the characteristics of rapid solidification, improvement of alloy solid solution limit and the like of additive manufacturing are fully utilized to obtain the medium-high-strength Al-Mg-Zr alloy powder with high Mg content. Specifically, a supersaturated alloy melt is formed in the preparation process of alloy powder, and the solid solution strengthening effect of Mg in an aluminum matrix is fully exerted. Zr element forms a first precipitated phase Al in an aluminum matrix 3 Zr nano-particles, al 3 The lattice mismatch degree of the Zr nano particles and an aluminum matrix (fcc) is low, and the nucleation energy barrier is low, so that the Zr nano particles are preferentially nucleated, and serve as heterogeneous nucleation points to refine matrix tissues, play a role in fine-grain strengthening, and inhibit solidification cracks; can separate out Al during the heat treatment of the additive manufactured forming part 3 Zr is dispersed in the nano particles to play a role in precipitation strengthening. Mn element plays a further solid solution strengthening role in the aluminum matrix, and precipitates AlMn phase precipitation in the heat treatment of the formed part to strengthen the aluminum matrix, so that the mechanical property of the alloy is improved. The proper amount of Si element can improve the casting performance of the aluminum alloy, inhibit thermal crack formation in the additive manufacturing process, and ensure that the prepared alloy has stable additive manufacturing forming performance. Therefore, the technical proposal fully utilizes elements such as Mg, zr, mn, si and the like to carry out solid solution strengthening, fine crystal strengthening and precipitation strengthening on the aluminum matrix, so that the tensile strength and the elongation of the tensile member manufactured by the alloy powder additive are obviously superior to those of Al-Si alloy, the tensile strength can reach more than 450MPa, and the elongation can reach more than 10 percent. The mechanical property is excellent, the cost is lower than that of the aluminum alloy containing Sc, and the method is suitable for industrial application.
Further, in the process of mixed smelting, the smelting temperature is 800-820 ℃, and the tapping temperature is 760-780 ℃.
In the technical scheme, the smelting temperature is controlled to be 800-820 ℃, preferably 800 ℃; in the smelting process, it is important to control the temperature, and when the temperature is too high, the influence on the molten metal is relatively large, for example, the molten metal is easy to oxidize or the metal material may burn out, and when the temperature is too high, the more hydrogen is absorbed, and the coarser the crystal grains are, the more the aluminum alloy is. When the temperature is too low, the dissolution of metal elements and the discharge of gas and impurities are not facilitated, and some metal materials can not be alloyed, so that the performance of the prepared metal powder can be influenced finally. Therefore, in the technical proposal, a smaller range is required for the smelting temperature, and the fusion of the metal raw materials is better when the smelting temperature is about 800 ℃ and the tapping temperature is 760-780 ℃. In the specific implementation process, a crucible of a vacuum induction furnace is generally adopted for smelting.
Further, the technological parameters of atomization powder preparation are as follows: the minimum vacuum degree is 1Pa, and the gas pressure is 3.3-3.6 MPa.
In the technical scheme, when the gas pressure is small, atomized particles cannot be smoothly formed, the metal melt may be solidified into blocks, and as the gas pressure is increased, the surface tension of the metal melt is increased, so that the spheroidization degree of the prepared powder is increased, and the average particle size is reduced. Therefore, in the invention, the gas pressure is preferably 3.3-3.6 MPa, and the particle size of the powder prepared under the condition can meet the requirement of additive manufacturing to the greatest extent.
Further, the preparation method further comprises the following steps: s30: classifying the Al-Mg-Zr alloy powder by adopting an ultrasonic vibration sieve, and screening the Al-Mg-Zr alloy powder with the powder granularity of 15-63 mu m.
In the technical scheme, an ultrasonic vibration sieve is used for sieving the Al-Mg-Zr alloy powder, and can convert high-frequency electric energy into mechanical vibration, so that ultrafine powder is easy to sieve. The Al-Mg-Zr alloy powder provided by the invention is used for additive manufacturing, and the powder granularity is optimal at 15-63 mu m according to the application requirement.
The invention also provides Al-Mg-Zr alloy powder, which is prepared by adopting the preparation method.
The invention also provides an application method of the Al-Mg-Zr alloy powder, and specifically, the Al-Mg-Zr alloy powder is applied to the field of additive manufacturing.
Further, the application method comprises the following steps: s100: layering and slicing are carried out according to the model of the part to be printed, and data of each layer are imported into the additive manufacturing device; s200: filling Al-Mg-Zr alloy powder into an additive manufacturing device, and setting a preheating temperature, laser power, a scanning speed and a scanning interval; s300: layer-by-layer printing is performed using an additive manufacturing apparatus until the entire part is obtained.
The invention also provides a part model which is obtained by additive manufacturing through adopting the Al-Mg-Zr alloy powder.
Drawings
FIG. 1 is an optical topography of the alloy powder provided in example 1;
FIG. 2 is a graph showing the particle size distribution of the alloy powder provided in example 1;
FIG. 3 is a SEM tissue morphology of the alloy formed article of example 1 incubated at 375℃for 6 h;
FIG. 4 is a stress-strain curve of the alloy molded part of example 1 heat-treated at 375℃for 6 hours;
FIG. 5 is a stress-strain curve of the alloy formed part of example 1 heat-treated at 375℃for 9 h;
FIG. 6 is a graph of the particle size distribution of the alloy powder provided in example 2;
FIG. 7 is a stress-strain curve for an alloy formed part of example 2 heat-treated at 375℃for 6 h;
FIG. 8 is a stress-strain curve for an alloy formed part of example 2 heat-treated at 375℃for 9 h;
FIG. 9 example 3 provides an alloy powder particle size distribution curve;
FIG. 10 is a stress-strain curve for an alloy formed part of example 3 heat-treated at 375℃for 6 h;
FIG. 11 is a stress-strain curve for an alloy formed part of example 3 heat-treated at 375℃for 9 h.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of embodiments of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of Al-Mg-Zr alloy powder for additive manufacturing, which comprises the following steps: s10: obtaining a metal raw material according to an alloy ratio, and mixing and smelting to obtain a metal melt; s20: transferring the metal melt into an atomization barrel, and atomizing and pulverizing under the environment of protective gas to obtain Al-Mg-Zr alloy powder; wherein, the Al-Mg-Zr alloy powder comprises the following elements in percentage by mass: 6.5 to 10 percent of Mg, 0.5 to 1.5 percent of Zr, 0.5 to 1.5 percent of Si, 0.3 to 1 percent of Mn, less than 0.1 percent of impurity and the balance of Al.
Preferably, in the Al-Mg-Zr alloy powder, the mass ratio of Mg is 7-9%; and/or Zr with the mass ratio of 0.7-1.2%; and/or Si in an amount of 0.7 to 1.2% by mass; and/or Mn in an amount of 0.5 to 0.8% by mass.
In the technical scheme, the Al-Mg-Zr alloy powder is used in the field of additive manufacturing, and the characteristics of rapid solidification, improvement of alloy solid solution limit and the like of additive manufacturing are fully utilized to obtain the medium-high-strength Al-Mg-Zr alloy powder with high Mg content. Specifically, a supersaturated alloy melt is formed in the preparation process of alloy powder, and the solid solution strengthening effect of Mg in an aluminum matrix is fully exerted. Zr element forms a first precipitated phase Al in an aluminum matrix 3 Zr nano-particles, al 3 The lattice mismatch degree of the Zr nano particles and an aluminum matrix (fcc) is low, and the nucleation energy barrier is low, so that the Zr nano particles are preferentially nucleated, and serve as heterogeneous nucleation points to refine matrix tissues, play a role in fine-grain strengthening, and inhibit solidification cracks; can separate out Al during the heat treatment of the additive manufactured forming part 3 Zr is dispersed in the nano particles to play a role in precipitation strengthening. Mn element plays a further solid solution strengthening role in the aluminum matrix, and precipitates AlMn phase precipitation in the heat treatment of the formed part to strengthen the aluminum matrix, so that the mechanical property of the alloy is improved. The proper amount of Si element can improve the casting performance of the aluminum alloy, inhibit thermal crack formation in the additive manufacturing process, and ensure that the prepared alloy has stable additive manufacturing forming performance. Therefore, the technical proposal fully utilizes the solid solution strength of Mg, zr, mn, si and other elements to the aluminum matrixThe tensile strength and the elongation rate of the tensile member manufactured by the alloy powder additive are obviously superior to those of Al-Si alloy, the tensile strength can reach more than 450MPa, and the elongation rate can reach more than 10%. The mechanical property is excellent, the cost is lower than that of the aluminum alloy containing Sc, and the method is suitable for industrial application.
Further, in the process of mixed smelting, the smelting temperature is 800-820 ℃, and the tapping temperature is 760-780 ℃.
In the technical scheme, the smelting temperature is controlled to be 800-820 ℃, preferably 800 ℃; in the smelting process, it is important to control the temperature, and when the temperature is too high, the influence on the molten metal is relatively large, for example, the molten metal is easy to oxidize or the metal material may burn out, and when the temperature is too high, the more hydrogen is absorbed, and the coarser the crystal grains are, the more the aluminum alloy is. When the temperature is too low, the dissolution of metal elements and the discharge of gas and impurities are not facilitated, and some metal materials can not be alloyed, so that the performance of the prepared metal powder can be influenced finally. Therefore, in the technical proposal, a smaller range is required for the smelting temperature, and the fusion of the metal raw materials is better when the smelting temperature is about 800 ℃ and the tapping temperature is 760-780 ℃. In the specific implementation process, a crucible of a vacuum induction furnace is generally adopted for smelting.
Further, the technological parameters of atomization powder preparation are as follows: the minimum vacuum degree is 1Pa, and the gas pressure is 3.3-3.6 MPa.
In the technical scheme, when the gas pressure is small, atomized particles cannot be smoothly formed, the metal melt may be solidified into blocks, and as the gas pressure is increased, the surface tension of the metal melt is increased, so that the spheroidization degree of the prepared powder is increased, and the average particle size is reduced. Therefore, in the invention, the gas pressure is preferably 3.3-3.6 MPa, and the particle size of the powder prepared under the condition can meet the requirement of additive manufacturing to the greatest extent.
Further, the preparation method further comprises the following steps: s30: classifying the Al-Mg-Zr alloy powder by adopting an ultrasonic vibration sieve, and screening the Al-Mg-Zr alloy powder with the powder granularity of 15-63 mu m.
In the technical scheme, an ultrasonic vibration sieve is used for sieving the Al-Mg-Zr alloy powder, and can convert high-frequency electric energy into mechanical vibration, so that ultrafine powder is easy to sieve. The Al-Mg-Zr alloy powder provided by the invention is used for additive manufacturing, and the powder granularity is optimal at 15-63 mu m according to the application requirement.
The invention also provides Al-Mg-Zr alloy powder, which is prepared by adopting the preparation method.
The invention also provides an application method of the Al-Mg-Zr alloy powder, and specifically, the Al-Mg-Zr alloy powder is applied to the field of additive manufacturing.
Further, the application method comprises the following steps: s100: layering and slicing are carried out according to the model of the part to be printed, and data of each layer are imported into the additive manufacturing device; s200: filling Al-Mg-Zr alloy powder into an additive manufacturing device, and setting a preheating temperature, laser power, a scanning speed and a scanning interval; s300: layer-by-layer printing is performed using an additive manufacturing apparatus until the entire part is obtained.
The invention also provides a part model which is obtained by additive manufacturing through adopting the Al-Mg-Zr alloy powder.
Example 1
The embodiment provides a preparation method of Al-Mg-Zr alloy powder for additive manufacturing, which comprises the following steps:
s10: smelting raw materials: smelting all component metal raw materials in a crucible of a vacuum induction furnace to obtain a metal melt, wherein the smelting temperature is 800 ℃ and the tapping temperature is 760 ℃;
s20: atomizing and pulverizing: transferring the smelted metal melt into an atomization barrel, introducing argon to replace air in the atomization barrel, and atomizing to prepare powder with the minimum vacuum degree of 1Pa and the gas pressure of 3.6MPa;
s30: powder screening: and carrying out ultrasonic vibration screening classification treatment on the atomized metal powder by adopting a 250-mesh screen and a 550-mesh screen to obtain the Al-Mg-Zr alloy powder with the powder granularity ranging from 15 mu m to 63 mu m.
Wherein, the Al-Mg-Zr alloy powder comprises the following elements in percentage by mass: 8.08% of Mg, 0.78% of Zr, 1.06% of Si, 0.64% of Mn, no more than 0.1% of impurity and the balance of Al.
The embodiment also provides Al-Mg-Zr alloy powder, which is prepared by adopting the preparation method; the optical morphology is shown in figure 1, and the particle size distribution is shown in figure 2.
The embodiment also provides an application method of the Al-Mg-Zr alloy powder in additive manufacturing; the method for printing the standard sample for performance test comprises the following steps:
s100: layering and slicing according to a model of a standard sample, and introducing data of each layer into an additive manufacturing device;
s200: filling Al-Mg-Zr alloy powder into an additive manufacturing device, and setting a preheating temperature, laser power, a scanning speed and a scanning interval;
s300: layer-by-layer printing was performed using an additive manufacturing apparatus until a standard sample was obtained.
In this embodiment, the additive manufacturing apparatus selects an S310 model SLM metal printer; the preheating temperature was 200 ℃, the laser power was 300W, the scanning speed was 1000 mm/s, the scanning pitch was 0.12 mm, and the thickness of each layer was 0.03 mm.
Further, the printed standard samples were subjected to different heat treatments, respectively, and parameters of the heat treatments were set as follows: heat preservation at 375 ℃ for 6 hours and 375 ℃ for 9 hours; as shown in fig. 3, which is an SEM tissue topography of a standard sample at 375 ℃ for 6 hours.
The standard sample after heat treatment is subjected to room temperature tensile mechanical property test, so that excellent mechanical property is obtained, the tensile strength can reach more than 450MPa, the tensile stress strain curve is shown in fig. 4 and 5, and the data are shown in table 1.
TABLE 1 room temperature tensile property data
Note that: the X/Y direction is parallel to the substrate direction, and the Z direction is the deposition direction, i.e., perpendicular to the substrate direction.
Example 2
The embodiment provides a preparation method of Al-Mg-Zr alloy powder for additive manufacturing, which comprises the following steps:
s10: smelting raw materials: smelting all component metal raw materials in a crucible of a vacuum induction furnace to obtain a metal melt, wherein the smelting temperature is 800 ℃, and the tapping temperature is 770 ℃;
s20: atomizing and pulverizing: transferring the smelted metal melt into an atomization barrel, introducing argon to replace air in the atomization barrel, and atomizing to prepare powder with the minimum vacuum degree of 1Pa and the gas pressure of 3.6MPa;
s30: powder screening: and carrying out ultrasonic vibration screening grading treatment on the atomized metal powder by adopting a 250-mesh screen to obtain the Al-Mg-Zr alloy powder with the powder granularity range of 15-63 mu m.
Wherein, the Al-Mg-Zr alloy powder comprises the following elements in percentage by mass: mg 7.69%, zr 0.91%, si 1.04%, mn 0.50%, impurities not exceeding 0.1%, and the balance Al.
The embodiment also provides Al-Mg-Zr alloy powder, which is prepared by adopting the preparation method; the particle size distribution is shown in FIG. 6.
The embodiment also provides an application method of the Al-Mg-Zr alloy powder in additive manufacturing; the method for printing the standard sample for performance test comprises the following steps:
s100: layering and slicing according to a model of a standard sample, and introducing data of each layer into an additive manufacturing device;
s200: filling Al-Mg-Zr alloy powder into an additive manufacturing device, and setting a preheating temperature, laser power, a scanning speed and a scanning interval;
s300: layer-by-layer printing was performed using an additive manufacturing apparatus until a standard sample was obtained.
In this embodiment, the additive manufacturing apparatus selects an S310 model SLM metal printer; the preheating temperature was 200 ℃, the laser power was 300W, the scanning speed was 1000 mm/s, the scanning pitch was 0.12 mm, and the thickness of each layer was 0.03 mm.
Further, the printed standard samples were subjected to different heat treatments, respectively, and parameters of the heat treatments were set as follows: the temperature was kept at 375℃for 6 hours and at 375℃for 9 hours.
The standard sample after heat treatment is subjected to room temperature tensile mechanical property test, so that excellent mechanical property is obtained, the tensile strength can reach more than 450MPa, the tensile stress strain curve is shown in fig. 7 and 8, and the data are shown in table 2.
TABLE 2 room temperature tensile property data
Note that: the X/Y direction is parallel to the substrate direction, and the Z direction is the deposition direction, i.e., perpendicular to the substrate direction.
Example 3
The embodiment provides a preparation method of Al-Mg-Zr alloy powder for additive manufacturing, which comprises the following steps:
s10: smelting raw materials: smelting all component metal raw materials in a crucible of a vacuum induction furnace to obtain a metal melt, wherein the smelting temperature is 800 ℃, and the tapping temperature is 770 ℃;
s20: atomizing and pulverizing: transferring the smelted metal melt into an atomization barrel, introducing argon to replace air in the atomization barrel, and atomizing to prepare powder with the minimum vacuum degree of 1Pa and the gas pressure of 3.4MPa;
s30: powder screening: carrying out ultrasonic vibration screening classification treatment on the atomized metal powder by adopting a 250-635 mesh screen, reserving fine powder with the particle size of 250-500 meshes, and mixing the fine powder to obtain the Al-Mg-Zr alloy powder with the particle size of 15-63 mu m.
Wherein, the Al-Mg-Zr alloy powder comprises the following elements in percentage by mass: mg 7.52%, zr 0.71%, si 1.00%, mn 0.58%, impurities not exceeding 0.1%, and the balance Al.
The embodiment also provides Al-Mg-Zr alloy powder, which is prepared by adopting the preparation method; the particle size distribution is shown in FIG. 9.
The embodiment also provides an application method of the Al-Mg-Zr alloy powder in additive manufacturing; the method for printing the standard sample for performance test comprises the following steps:
s100: layering and slicing according to a model of a standard sample, and introducing data of each layer into an additive manufacturing device;
s200: filling Al-Mg-Zr alloy powder into an additive manufacturing device, and setting a preheating temperature, laser power, a scanning speed and a scanning interval;
s300: layer-by-layer printing was performed using an additive manufacturing apparatus until a standard sample was obtained.
In this embodiment, the additive manufacturing apparatus selects an S310 model SLM metal printer; the preheating temperature was 200 ℃, the laser power was 300W, the scanning speed was 1000 mm/s, the scanning pitch was 0.12 mm, and the thickness of each layer was 0.03 mm.
Further, the printed standard samples were subjected to different heat treatments, respectively, and parameters of the heat treatments were set as follows: the temperature was kept at 375℃for 6 hours and at 375℃for 9 hours.
The standard sample after heat treatment is subjected to room temperature tensile mechanical property test, so that excellent mechanical property is obtained, the tensile strength can reach more than 450MPa, the tensile stress strain curve is shown in fig. 10 and 11, and the data are shown in table 3.
TABLE 3 tensile property data at room temperature
Note that: the X/Y direction is parallel to the substrate direction, and the Z direction is the deposition direction, i.e., perpendicular to the substrate direction.
Example 4
The embodiment provides a modification method of Al-Mg-Zr alloy powder, which comprises the following steps:
A. mixing the alloy powder and the modified powder, adding a wetting agent, a coupling agent and an auxiliary agent, dispersing uniformly, and carrying out mechanical ball milling for the first time under the protection of inert gas; washing and drying to obtain modified alloy powder.
Wherein the modified powder comprises two nano-scale rare earth element amorphous alloys with different particle sizes.
The rare earth element amorphous alloy consists of scandium, zirconium and aluminum; the mass ratio of scandium to zirconium is 0.5-2:1; the mass ratio of the aluminum element in the rare earth element amorphous alloy is not more than 10 percent.
The modified powder comprises rare earth element amorphous alloy with the grain diameter of 20-80 nanometers and rare earth element amorphous alloy with the grain diameter of 600-900 nanometers in a mass ratio of 0.5-1:1.
The wetting agent is polypropylene glycol and triethanolamine; the coupling agent is tetraoctyloxybis (dilauryl phosphite) titanate and isopropyl tri (dioctyl pyrophosphate); the auxiliary agent is ethyl cellulose and polyethylene glycol.
The mass ratio of the alloy powder to the modified powder to the wetting agent to the coupling agent to the auxiliary agent is 100:10 (5-15): (5-8): (10-15).
The planetary ball mill is used for one-time mechanical ball milling, and the time between ball milling is 30 minutes and 5 minutes; the total time of the intermittent ball milling is 5-6 hours; the ball-to-material ratio is 13:1. Wherein, the process of one-time mechanical ball milling comprises three grinding balls with diameters of 9mm, 7mm and 4mm respectively; the mass ratio of the grinding balls is 2:1.5:3 in the order of the diameters from large to small.
B. Depositing ceramic particles on the surface of the modified alloy powder by adopting a physical vapor deposition mode; the method comprises the following steps:
dispersing the modified alloy powder in acetone to obtain mixed slurry;
the mixed slurry is in a fluidized state;
mixing ceramic particles in an inert gas and mixing the mixed slurry at a jet velocity of 5-10 m/s; vapor deposition to obtain modified alloy powder with ceramic particles deposited on the surface.
Wherein the mass ratio of the modified alloy powder to the ceramic particles is 95:5.
The ceramic particles are at least one of aluminum oxide and titanium nitride. The grain size of the ceramic particles is 200-300 nanometers.
C. And adding a coupling agent and an auxiliary agent into the modified alloy powder with the ceramic particles deposited on the surface, and performing secondary mechanical ball milling.
The coupling agent is tetraoctyloxybis (dilauryl phosphite) titanate and isopropyl tri (dioctyl pyrophosphate); the auxiliary agent is ethyl cellulose and polyethylene glycol.
The mass ratio of the modified alloy powder with ceramic particles deposited on the surface, the coupling agent and the auxiliary agent is 100 (5-8) to 10-15.
The secondary mechanical ball milling uses a stirring ball mill, wherein each ball milling time is 45 minutes, and the interval time is 5 minutes; the total time of the intermittent ball milling is 5-6 hours; the ball-to-material ratio is 10:1. Wherein, the process of one-time mechanical ball milling comprises two grinding balls with the diameters of 10mm and 4mm respectively; the mass ratio of the grinding balls is 2:3 in the order of the diameters from large to small.
In the embodiment, the alloy powder is further modified, firstly, the rare earth element amorphous alloy is introduced for modification, and the rare earth element can increase the absorptivity of the alloy powder to laser, so that the alloy powder can be molded by adopting smaller laser in the additive manufacturing process. Meanwhile, the granularity of the rare earth element amorphous alloy is designed into two different grades, namely 20-80 nanometers and 600-900 nanometers, and alloy powder and modified powder are crosslinked together in a ball milling mode. The advantages are that: the defects of alloy powder such as insufficient roundness, cracks on the surface, hollow powder and the like can be effectively improved by ball milling; and the modified powder is added for ball milling together, so that metals can be alloyed through mechanical collision, and rare earth elements can be embedded into the surfaces of alloy particles and are uniformly distributed. Modified powders of different particle sizes can achieve a more uniform coating. Particularly, the disordered structure of the amorphous alloy can enable the modified alloy powder to refine grains of the printing component and enable rare earth elements to be dispersed; further improving the wear resistance, corrosion resistance, strength, hardness and toughness of the member.
The wetting agent, the coupling agent and the auxiliary agent are added in the ball milling process for auxiliary operation, and the surface of the alloy powder is roughened during ball milling, so that the uniformity of the surface roughness of the alloy powder can be promoted by adding the agent. Preferably, the coupling agent is tetraoctyloxybis (dilauryl phosphite) titanate and isopropyl tri (dioctyl pyrophosphate); the coupling agent is selected from titanate rich in phosphoric acid, so that the stability of the metal in the ball milling process can be improved.
Three different grinding balls are selected in the mechanical ball milling, and an intermittent ball milling mode is adopted, and the alloying degree between the alloy powder and the modified powder is improved by continuously hammering intermittent big balls.
Further, ceramic particles are deposited on the surface of the modified alloy powder in a physical vapor deposition mode, and on one hand, cracks can be effectively restrained by introducing the ceramic particles; on the other hand, the self-colored color of the ceramic particles can also realize the coloring function for the printing member.
In the embodiment, the surface of the alloy powder is modified by ball milling twice by adopting two materials of rare earth amorphous alloy and ceramic particles, so that the surface energy of the alloy powder can be reduced, and the flow property of the alloy powder can be improved; the adsorption between the powders is reduced, and the acting force and the adhesiveness between the powders are weakened.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A method for preparing an Al-Mg-Zr alloy powder for additive manufacturing, comprising the steps of:
s10: obtaining a metal raw material according to an alloy ratio, and mixing and smelting to obtain a metal melt;
s20: transferring the metal melt into an atomization barrel, and atomizing to prepare powder under the environment of protective gas to obtain the Al-Mg-Zr alloy powder;
wherein, the Al-Mg-Zr alloy powder comprises the following elements in percentage by mass:
6.5 to 10 percent of Mg, 0.5 to 1.5 percent of Zr, 0.5 to 1.5 percent of Si, 0.3 to 1 percent of Mn, less than 0.1 percent of impurity and the balance of Al.
2. The method according to claim 1, wherein, in the Al-Mg-Zr alloy powder,
the mass ratio of Mg is 7-9%; and/or
The mass ratio of Zr is 0.7-1.2%; and/or
Si accounts for 0.7 to 1.2 percent; and/or
Mn is 0.5-0.8% by mass.
3. The method according to claim 1, wherein, in the process of mixed smelting,
the smelting temperature is 800-820 ℃, and the tapping temperature is 760-780 ℃.
4. The method according to claim 1, wherein the process parameters of the atomized powder process are as follows:
the minimum vacuum degree is 1Pa, and the gas pressure is 3.3-3.6 MPa.
5. The method of manufacturing according to claim 1, further comprising the steps of:
s30: classifying the Al-Mg-Zr alloy powder by adopting an ultrasonic vibration sieve, and screening the Al-Mg-Zr alloy powder with the powder granularity of 15-63 mu m.
6. An Al-Mg-Zr alloy powder prepared by the preparation method according to any one of claims 1 to 5.
7. The method of using the Al-Mg-Zr alloy powder according to claim 6, wherein the Al-Mg-Zr alloy powder is applied to the field of additive manufacturing.
8. Application method according to claim 7, characterized in that it comprises the following steps:
s100: layering and slicing are carried out according to the model of the part to be printed, and data of each layer are imported into the additive manufacturing device;
s200: loading the Al-Mg-Zr alloy powder into the additive manufacturing device, and setting a preheating temperature, laser power, a scanning speed and a scanning interval;
s300: the additive manufacturing apparatus is used to print layer by layer until the entire part is obtained.
9. A part model, which is obtained by additive manufacturing using the Al-Mg-Zr alloy powder as set forth in claim 6.
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