CN111168053B - Preparation method of raw material powder for high-entropy alloy selective laser melting additive manufacturing - Google Patents
Preparation method of raw material powder for high-entropy alloy selective laser melting additive manufacturing Download PDFInfo
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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Abstract
The invention provides a method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing, which is characterized in that alloy powder or simple substance metal powder is matched with alloy powder by adopting a raw material mixing method to obtain high-entropy alloy powder, so that the melting points of all component powder in the high-entropy alloy powder tend to be close, and the mole numbers of all metal elements in the high-entropy alloy powder are the same; the invention also discloses application of the preparation method of the raw material powder for selective laser melting additive manufacturing of the high-entropy alloy in a selective laser melting in-situ additive manufacturing process of the high-entropy alloy, and the obtained high-entropy alloy product has a good forming effect and is free of pores and macrocracks.
Description
Technical Field
The invention belongs to the technical field of alloy materials, and particularly relates to a preparation method of raw material powder for high-entropy alloy selective laser melting additive manufacturing.
Background
The concept of high-entropy alloy is a completely new alloy design concept proposed in recent years. Unlike conventional single or two-principal element alloys, which generally consist of 5 or more elements, each element is present in an amount of between 5% and 35%, most commonly high entropy alloys mixed in equimolar proportions. This alloy design substantially increases the entropy in the alloy system and is therefore referred to as a high entropy alloy. The high-entropy alloy has a series of excellent properties, such as higher hardness, higher tensile strength, wear resistance, corrosion resistance and the like.
The laser additive manufacturing technology has attracted more and more attention in recent years due to the advantages that the laser additive manufacturing technology is suitable for manufacturing of parts with complex structures, near net shape forming and the like, and the application of the laser additive manufacturing in the field of high-entropy alloy preparation is also a research focus in recent years. Laser additive manufacturing has two major branches, Laser Melting Deposition (LMD) and Selective Laser Melting (SLM). The LMD technology is fast in forming speed and large in size, but is poor in forming precision and generally requires post-machining treatment. Compared with the LMD technology, the SLM technology has extremely high precision of manufactured parts, and the machining error is usually within 30 microns. The principle is that laser is used as a heat source, and a geometric slicing mode is adopted to spread powder layer by layer for printing. Therefore, the SLM technology will become the main manufacturing method of future high-entropy alloy complex and precise components, and is worthy of deep research on the forming process and method thereof.
However, the existing domestic additive manufacturing powder production system is not complete, and the alloy powder for high-entropy alloy additive manufacturing needs huge waste of capacity for customization, so that the cost is extremely high. And the components of the alloy powder are fixed, which is not beneficial to the component adjustment in the alloy development process. The direct use of elemental powder for in-situ SLM manufacturing also faces the problem of large difference between the melting point and the boiling point of each elemental powder, so that in the printing process, the heat input is so low that the low-melting-point metal elemental can not melt the high-melting-point metal element to form unmelted particles when being melted, and when the heat input is high enough to completely melt the high-melting-point metal element, the low-melting-point metal elemental can be evaporated due to overheating, and gas can not overflow out of the molten pool to generate gas holes. Therefore, a printed matter having no or few defects cannot be obtained by directly using the single substance mixed powder. Therefore, the cheap and reasonable preparation method of the powder required by the high-entropy alloy in-situ SLM manufacturing is provided, so that the development speed of the high-entropy alloy is greatly increased, and the production cost is reduced. The method has important significance for the perfection of a high-entropy alloy theoretical system and the development of an SLM technology.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a method for preparing raw material powder for selective laser melting additive manufacturing of high-entropy alloy, improves the alloy development efficiency, obtains a compact high-entropy alloy structure, enables the in-situ synthesis of the high-entropy alloy by using an SLM (selective laser melting), and can obtain a product with good mechanical property.
The invention is realized by the following technical scheme:
a method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that alloy powder or simple substance metal powder is matched with alloy powder by adopting a raw material mixing method to obtain high-entropy alloy powder, so that the melting points of all component powder in the high-entropy alloy powder tend to be close, and the mole numbers of all metal elements in the high-entropy alloy powder are the same;
in the above technical scheme, the raw material mixing method includes mixing a mixed simple substance metal powder with M-X alloy powder and/or N-Y alloy powder and/or X-Y alloy powder to obtain high-entropy alloy powder, drying the mixed metal powder in a vacuum dryer, sealing and storing the dried mixed simple substance metal powder, wherein the mixed simple substance metal powder at least includes two of three kinds of simple substance metal powders of Fe, Co and Ni, the M-X alloy powder is an alloy powder formed by an M metal element and X, the M metal element is a metal element with the highest melting point in the high-entropy alloy, wherein X is at least one metal element appearing in the mixed simple substance metal powder, the N-Y alloy powder is an alloy powder formed by an N metal element and Y, and the N metal element is a metal element with the lowest melting point in the high-entropy alloy, wherein Y is at least one metal element appearing in the mixed simple substance metal powder, and the mole numbers of all the metal elements in the mixed metal powder are the same;
in the technical scheme, the mixed simple substance metal powder, the M-X alloy powder, the N-Y alloy powder and the X-Y alloy powder are spherical powders, the granularity of the spherical powders is 0-64 mu M, the mixed simple substance metal powder and the M-X alloy powder and/or the N-Y alloy powder are mixed in a three-dimensional mixer for 2-4 hours, the rotating speed of a cylinder body is 20-40 r/min, the uniformly mixed spherical powders are dried in a vacuum dryer for 5-10 hours, the temperature is 50-100 ℃, the vacuum degree is less than the absolute pressure of 10KPa, and the spherical powders are sealed and stored after being dried;
a method for preparing the raw material powder used for high-entropy selective laser melting additive manufacturing includes such steps as mixing the spherical Fe-Co elementary metal powder with Ni50Cr50The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 4 hours, enabling the rotating speed of a cylinder to be 20r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
A method for preparing the raw material powder used for high-entropy selective laser melting additive manufacturing includes such steps as mixing the spherical metal powder of Fe, Co and Ni with Ni20Cr80The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
A method for preparing the raw material powder used for high-entropy selective laser melting additive manufacturing includes such steps as mixing the spherical metal powder of Fe, Co and Ni with Ni30Cr70The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
HeightA process for preparing the raw material powder used for entropy alloy selective laser smelting additive includes such steps as mixing the elementary metal spherical powder of Fe, Co and Ni with Ni20Cr80、Mn75Fe25The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
A method for preparing the raw material powder used for high-entropy selective laser melting additive manufacturing includes such steps as mixing the spherical metallic powder of Fe, Co and Ni with Co35Cr65The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
A method for preparing the raw material powder used for high-entropy selective laser melting additive manufacturing includes such steps as mixing the spherical metallic powder of Fe, Co and Ni with Co35Cr65、Ti60Al40、Al35Fe65The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
The preparation method of the raw material powder for selective laser melting additive manufacturing of the high-entropy alloy is applied to a selective laser melting in-situ additive manufacturing process of the high-entropy alloy.
The invention has the advantages and beneficial effects that:
the material prepared by the method has high molding efficiency, and the part model is not restricted by the process and can be used for preparing parts with complex shapes. Secondly, unlike traditional subtractive manufacturing, the selective laser melting in-situ additive manufacturing method is one of laser additive manufacturing. The near-net-shape forming of the material can be realized, and the production cost of parts is greatly reduced.
The laser additive manufacturing of the high-entropy alloy can be successfully carried out by using the method. The sample has good forming effect, no air holes and macrocracks, good density and uniform tissue. The energy spectrometer is used for component detection, and the result shows that the components of the formed part are similar to those of the powder material, and the situation of large-amount element burning loss does not occur.
The method can greatly reduce the production and research and development cost of the high-entropy alloy. The high-entropy alloy amorphous grade needs to be customized for production and research and development, has extremely high cost and needs to be customized again if component modification is needed. The powder and the binary alloy powder used in the method are common powder in the market, and the price is low. Also, the composition modification is easy to perform by the present method.
According to the method, the metal simple substance powder and the alloy powder are mixed to prepare the raw material powder for selective laser melting in-situ additive manufacturing, the problems of unmelted metal particles and air holes generated in the process of printing the mixed powder by completely using the metal simple substance powder are solved by printing, and the problems that the effective sectional area is reduced due to the fact that the air holes are generated by the gasification of the unmelted high-melting-point metal particles and the low-melting-point metal, so that the material strength is reduced due to cracks and the like are solved.
Drawings
FIG. 1 is a scanning electron micrograph of a sample after printing in comparative example step 2;
FIG. 2 is an EDS profile of a Cr element energy spectrum of a sample printed in comparative example step 2;
FIG. 3 is a scanning electron microscope image of a sample after completing printing in step 2 of example 1 of the present invention;
FIG. 4 is a surface distribution diagram of Cr, Fe, Co and Ni elements in a sample printed in step 2 of example 1 (EDS surface distribution diagram);
a: spectral surface distribution diagram of Cr element, b: the spectrum surface distribution diagram of the Fe element, C: spectrum surface distribution diagram of Co element, D: the spectral surface distribution diagram of the Ni element.
FIG. 5 shows a sample after printing in step 2 of example 1 of the present invention
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
Comparative example: high-entropy alloy selective laser melting in-situ additive manufacturing by directly mixing metal simple substance powder serving as raw material
Step 1, 560g of Fe, 590g of Co, 520g of Cr and 590g of 590gNi elementary substance metal spherical powder (the particle size of the powder is 15-48 microns) with the purity of 99.9% is placed into a three-dimensional mixer to be mixed for 2-4 hours, the rotating speed of a cylinder body is 20-40 r/min, the uniformly mixed spherical powder is dried for 5-10 hours in a vacuum dryer at the temperature of 50-100 ℃ and the vacuum degree of 10KPa below the absolute pressure, and the spherical powder is sealed and stored after drying.
And 2, selecting 316L stainless steel as the substrate, wherein the size is 250mm multiplied by 15 mm. And (3) cleaning the greasy dirt and the smudged dirt on the surface respectively by using acetone and alcohol. The surface blasting treatment was performed using a sandblaster. The method comprises the steps of printing by using AM-400 laser 3D printing equipment produced by Renisshaw-Quantam, constructing a block body with the size of 5mm multiplied by 5mm in Renisshaw-Quantam with the power of 180-200W, enabling an interlayer rotation angle of 67 degrees to release residual stress, enabling exposure time to be 50-70 mu s and line point distance to be 30-50 micrometers, vacuumizing a printing bin before printing, enabling oxygen content to be lower than 500ppm, adopting argon protection, and cooling a printed test piece for 2 hours along with the bin.
Due to the large difference of the melting points of the metal simple substances (table 1), various defects such as unmelted particles, pores and the like (as shown in fig. 1) often occur in the production process and cannot be eliminated through process adjustment. The unmelted grains and pores also cause a reduction in the effective area of the sample in the direction of residual stress, thereby causing cracking (see fig. 1). The unmelted particles were found to be elemental particles of Cr by surface scan analysis (see fig. 2).
The differences between the melting points of the Cr simple substance and the Fe, Co and Ni simple substances in the FeCoCrNi simple substance mixed powder are all over 300 ℃. Therefore, in the printing process, the heat input is low enough to enable the Fe, Co and Ni simple substances to be incapable of melting the Cr element to form unmelted particles when melted, and the heat input is high enough to enable the Cr element to be completely melted, the Fe, Co and Ni simple substances are evaporated due to overheating, and gas cannot overflow a molten pool to generate air holes. Therefore, a printed matter having no or few defects cannot be obtained by directly using the single substance mixed powder.
TABLE 1 melting Point (. degree. C.) of Fe, Co, Cr, Ni simple substance
Therefore, in the invention, the metal element with higher melting point and/or the metal element with lower melting point in the high-entropy powder are added and mixed in the form of alloy powder, so that the melting points of the powders tend to be similar, and the metal element which cannot be melted or the gasified metal element is prevented from being generated when the same heat is input. In the specific embodiment, the metal with the highest melting point and the metal with the lowest melting point are combined to form alloy powder, the metal with the highest melting point and the metal with the middle melting point are combined to form alloy powder, the metal with the lowest melting point and the metal with the middle melting point are combined to form alloy powder, or the metal with the higher melting point and the metal with the lower melting point are combined to form alloy powder, so that the melting points of the powders are close to each other as a whole.
Example one
A FeCoCrNi series high-entropy alloy selective laser melting in-situ additive manufacturing method comprises the following steps:
step 1, mixing raw materials, and mixing 560gFe and 590gCo elementary metal balls with the purity of 99.9%Shaped powder (powder particle size 15-48 microns) and 1110gNi50Cr50Putting the alloy spherical powder (the particle size of the powder is 15-48 microns) into a three-dimensional mixer, mixing for 4 hours, drying the uniformly mixed spherical powder in a vacuum dryer at the temperature of 50 ℃ and the vacuum degree of less than 10KPa absolute pressure at the rotation speed of 20r/min of a cylinder, and sealing and storing after drying.
2, additive manufacturing, namely polishing the surface of a substrate by using an angle grinder until no oxide exists, respectively cleaning oil stain and dirt on the surface by using acetone and alcohol, performing surface sand blasting by using a sand blasting machine, putting the mixed metal powder obtained after the step 1 is finished into a printer bin, performing laser additive manufacturing by using AM-400 laser 3D printing equipment produced by Renisshaw-Quantam, constructing a block body with the size of 5mm x 5mm in Renisshaw-Quantam, setting the rotation angle between layers to be 67 degrees to release residual stress, automatically performing laser walking off-line programming by software, vacuumizing the printing bin before printing, enabling the oxygen content to be lower than 200ppm, enabling the laser power to be 180-200W, enabling the exposure time to be 50-70 mus, enabling the line point distance to be 30-50 micrometers, and protecting argon gas, the argon flow was 15L/min and the printed sample was cooled with the bin for 2 hours.
After the printed sample is analyzed by a Scanning Electron Microscope (SEM), the result is shown in figure 3, the tissue of the sample is uniform, and no macroscopic defect occurs.
Fig. 4 was analyzed and evaluated, and the phenomenon and the obtained conclusion are discussed. According to the energy spectrum surface distribution diagram (figure 4), Fe and Co elements are slightly enriched at the bottom of the molten pool, and Cr and Ni elements are not enriched. On the whole, the four elements are uniformly distributed, and Fe, Co-poor, Cr-poor and Ni-poor regions are not seen.
Fig. 5 is a photograph of a printed sample, showing that the forming effect is good, the mark is clear and visible, and the edge angle of the sample is clear without adhesive powder.
The area energy spectrum detection is carried out on the sample (Table 2), and the detection result shows that the components are uniform and the situation of burning loss of a large amount of elements does not occur.
TABLE 2 regional energy Spectrum detection (at%)
In this embodiment, Fe and Co elemental metal powders and nichrome powders are mixed to prepare a raw material powder for selective laser melting in-situ additive manufacturing, and the raw material powder is printed, so that the problems of unmelted Cr particles and pores generated in the printing process of the mixed powder completely using the elemental metal powders are solved, and the problem of cracks caused by reduction of effective cross-sectional area due to the unmelted Cr particles and pores is solved. The test piece printed by the embodiment has uniform structure, fine crystal grains and no defect.
The unit prices of common simple substance powder, alloy powder and high-entropy alloy powder in the market are shown in table 3 (the unit prices of all manufacturers are slightly different). The simple substance powder and the binary alloy powder are widely applicable and are usually produced in batches, so the cost is lower. However, the high-entropy alloy powder is usually sold only by scientific research institutions and needs to be customized according to components, 1-2 ten thousand yuan is usually needed for one-time furnace opening of smelting and powder making, the labor cost is about 5000-8000 yuan, and the cost of the powder is added, so that the unit price of the high-entropy alloy powder is extremely high. It can be seen that the use of this method for powder preparation will result in substantial cost savings.
TABLE 3 unit price (Yuan/Kg) of spherical atomized powder
Example two
A FeCoCrNi series high-entropy alloy selective laser melting in-situ additive manufacturing method comprises the following steps:
step 1, mixing raw materials, namely 560g of Fe, 590g of Co and 442.5gNi elementary substance metal spherical powder (the particle size of the powder is 15-48 microns) with the purity of 99.9%, and 667.5gNi20Cr80And (3) placing the alloy spherical powder (the particle size of the powder is 15-48 microns) into a three-dimensional mixer, mixing for 2 hours, drying the uniformly mixed spherical powder in a vacuum dryer for 5 hours at the temperature of 100 ℃ and the vacuum degree of less than 10KPa absolute pressure at the rotation speed of 40r/min of a cylinder, and sealing and storing after drying.
2, additive manufacturing, namely polishing the surface of a substrate by using an angle grinder until no oxide exists, respectively cleaning oil stain and dirt on the surface by using acetone and alcohol, performing surface sand blasting by using a sand blasting machine, putting the mixed metal powder obtained after the step 1 is finished into a printer bin, performing laser additive manufacturing by using AM-400 laser 3D printing equipment produced by Renisshaw-Quantam, constructing a block body with the size of 5mm x 5mm in Renisshaw-Quantam, setting the rotation angle between layers to be 67 degrees to release residual stress, automatically performing laser walking off-line programming by software, vacuumizing the printing bin before printing, enabling the oxygen content to be lower than 200ppm, enabling the laser power to be 180-200W, enabling the exposure time to be 50-70 mus, enabling the line point distance to be 30-50 micrometers, and protecting argon gas, the argon flow was 15L/min and the printed sample was cooled with the bin for 2 hours.
EXAMPLE III
A FeCoCrNi series high-entropy alloy selective laser melting in-situ additive manufacturing method comprises the following steps:
step 1, mixing raw materials, namely 560g of Fe, 590g of Co, 337.1gNi elementary substance metal spherical powder (the particle size of the powder is 15-48 microns) with the purity of 99.9%, and 772.9gNi30Cr70And (3) placing the alloy spherical powder (the particle size of the powder is 15-48 microns) into a three-dimensional mixer, mixing for 3 hours, drying the uniformly mixed spherical powder in a vacuum dryer for 8 hours at the temperature of 80 ℃ and the vacuum degree of less than 10KPa absolute pressure at the rotation speed of 30r/min of a cylinder, and sealing and storing after drying.
2, additive manufacturing, namely polishing the surface of a substrate by using an angle grinder until no oxide exists, respectively cleaning oil stain and dirt on the surface by using acetone and alcohol, performing surface sand blasting by using a sand blasting machine, putting the mixed metal powder obtained after the step 1 is finished into a printer bin, performing laser additive manufacturing by using AM-400 laser 3D printing equipment produced by Renisshaw-Quantam, constructing a block body with the size of 5mm x 5mm in Renisshaw-Quantam, setting the rotation angle between layers to be 67 degrees to release residual stress, automatically performing laser walking off-line programming by software, vacuumizing the printing bin before printing, enabling the oxygen content to be lower than 200ppm, enabling the laser power to be 180-200W, enabling the exposure time to be 50-70 mus, enabling the line point distance to be 30-50 micrometers, and protecting argon gas, the argon flow was 15L/min and the printed sample was cooled with the bin for 2 hours.
Example four
A selective laser melting in-situ additive manufacturing method for FeCoCrNiMn high-entropy alloy comprises the following steps:
step 1, mixing raw materials, namely 373.3g of Fe, 590g of Co and 442.5gNi of elementary metal spherical powder (the particle size of the powder is 15-48 microns) with the purity of 99.9%, 736.7gMn75Fe25、667.5gNi20Cr80And (3) placing the alloy spherical powder (the particle size of the powder is 15-48 microns) into a three-dimensional mixer, mixing for 3 hours, drying the uniformly mixed spherical powder in a vacuum dryer for 8 hours at the temperature of 80 ℃ and the vacuum degree of less than 10KPa absolute pressure at the rotation speed of 30r/min of a cylinder, and sealing and storing after drying.
2, additive manufacturing, namely polishing the surface of a substrate by using an angle grinder until no oxide exists, respectively cleaning oil stain and dirt on the surface by using acetone and alcohol, performing surface sand blasting by using a sand blasting machine, putting the mixed metal powder obtained after the step 1 is finished into a printer bin, performing laser additive manufacturing by using AM-400 laser 3D printing equipment produced by Renisshaw-Quantam, constructing a block body with the size of 5mm x 5mm in Renisshaw-Quantam, setting the rotation angle between layers to be 67 degrees to release residual stress, automatically performing laser walking off-line programming by software, vacuumizing the printing bin before printing, enabling the oxygen content to be lower than 200ppm, enabling the laser power to be 180-200W, enabling the exposure time to be 50-70 mus, enabling the line point distance to be 30-50 micrometers, and protecting argon gas, the argon flow was 15L/min and the printed sample was cooled with the bin for 2 hours.
EXAMPLE five
A FeCoCrNi high-entropy alloy selective laser melting in-situ additive manufacturing method comprises the following steps:
step 1, mixing raw materials, and mixing 560 with the purity of 99.9%gFe, 272.3gCo, 590gNi simple substance metal spherical powder (the particle size of the powder is 15-48 microns) and 837.7gCo35Cr65And (3) placing the alloy spherical powder (the particle size of the powder is 15-48 microns) into a three-dimensional mixer, mixing for 3 hours, drying the uniformly mixed spherical powder in a vacuum dryer for 8 hours at the temperature of 80 ℃ and the vacuum degree of less than 10KPa absolute pressure at the rotation speed of 30r/min of a cylinder, and sealing and storing after drying.
2, additive manufacturing, namely polishing the surface of a substrate by using an angle grinder until no oxide exists, respectively cleaning oil stain and dirt on the surface by using acetone and alcohol, performing surface sand blasting by using a sand blasting machine, putting the mixed metal powder obtained after the step 1 is finished into a printer bin, performing laser additive manufacturing by using AM-400 laser 3D printing equipment produced by Renisshaw-Quantam, constructing a block body with the size of 5mm x 5mm in Renisshaw-Quantam, setting the rotation angle between layers to be 67 degrees to release residual stress, automatically performing laser walking off-line programming by software, vacuumizing the printing bin before printing, enabling the oxygen content to be lower than 200ppm, enabling the laser power to be 180-200W, enabling the exposure time to be 50-70 mus, enabling the line point distance to be 30-50 micrometers, and protecting argon gas, the argon flow was 15L/min and the printed sample was cooled with the bin for 2 hours.
EXAMPLE six
A selective laser melting in-situ additive manufacturing method for FeCoCrNiAlTi high-entropy alloy comprises the following steps of:
step 1, mixing raw materials, namely 213.3gFe with the purity of 99.9%, 272.3gCo, 590gNi elementary substance metal spherical powder (the particle size of the powder is 15-48 microns) and 837.7gCo35Cr65、630gTi60Al40、436.7gAl35Fe65Putting the alloy spherical powder (the particle size of the powder is 15-48 microns) into a three-dimensional mixer, mixing for 3 hours, drying the uniformly mixed spherical powder in a vacuum dryer for 8 hours at the temperature of 80 ℃ and the vacuum degree of less than 10 absolute pressure at the rotation speed of 30r/min of a cylinder bodyKPa, and sealing and storing after drying.
2, additive manufacturing, namely polishing the surface of a substrate by using an angle grinder until no oxide exists, respectively cleaning oil stain and dirt on the surface by using acetone and alcohol, performing surface sand blasting by using a sand blasting machine, putting the mixed metal powder obtained after the step 1 is finished into a printer bin, performing laser additive manufacturing by using AM-400 laser 3D printing equipment produced by Renisshaw-Quantam, constructing a block body with the size of 5mm x 5mm in Renisshaw-Quantam, setting the rotation angle between layers to be 67 degrees to release residual stress, automatically performing laser walking off-line programming by software, vacuumizing the printing bin before printing, enabling the oxygen content to be lower than 200ppm, enabling the laser power to be 180-200W, enabling the exposure time to be 50-70 mus, enabling the line point distance to be 30-50 micrometers, and protecting argon gas, the argon flow was 15L/min and the printed sample was cooled with the bin for 2 hours.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (9)
1. A method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that the raw material mixing method comprises the steps of mixing mixed simple substance metal powder with M-X alloy powder and/or N-Y alloy powder and/or X-Y alloy powder to obtain high-entropy alloy powder, drying the mixed metal powder in a vacuum dryer, sealing and storing after drying is finished, wherein the mixed simple substance metal powder at least comprises two of three kinds of simple substance metal powder of Fe, Co and Ni, the M-X alloy powder is alloy powder formed by an M metal element and X, the M metal element is a metal element with the highest melting point in the high-entropy alloy, and X is at least one metal element appearing in the mixed simple substance metal powder, the N-Y alloy powder is formed by N metal elements and Y, the N metal elements are metal elements with the lowest melting point in the high-entropy alloy, the Y is at least one metal element in the mixed simple substance metal powder, and the mole numbers of the metal elements in the mixed metal powder are the same.
2. The method for preparing the raw material powder for the selective laser melting additive manufacturing of the high-entropy alloy according to claim 1, wherein the mixed simple substance metal powder, the M-X alloy powder, the N-Y alloy powder and the X-Y alloy powder are all spherical powders, the particle size of the spherical powder is within a range of 0-64 μ M, the mixed simple substance metal powder and the M-X alloy powder and/or the N-Y alloy powder are mixed in a three-dimensional mixer for 2-4 hours, the rotating speed of a cylinder is 20-40 r/min, the uniformly mixed spherical powder is dried in a vacuum dryer for 5-10 hours at a temperature of 50-100 ℃ and a vacuum degree of less than 10KPa absolute pressure, and the spherical powder is sealed and stored after being dried.
3. A method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that Fe and Co simple substance metal spherical powder and Ni are mixed50Cr50The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 4 hours, enabling the rotating speed of a cylinder to be 20r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
4. A method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that Fe, Co and Ni simple substance metal spherical powder and Ni are mixed20Cr80Placing the alloy spherical powder into a three-dimensional mixer to be mixed for 2-4 hours at the rotating speed of 20-40 r/min, wherein the particle diameters of the simple substance metal spherical powder and the alloy spherical powder are both 15-48 microns, and drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours at a warm temperatureAnd (3) the temperature is 50-100 ℃, the vacuum degree is less than 10KPa of absolute pressure, the high-entropy alloy powder is obtained by sealing and storing after drying, and the mole number of each metal element in the mixed high-entropy alloy powder is the same.
5. A method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that Fe, Co and Ni simple substance metal spherical powder and Ni are mixed30Cr70The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
6. A method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that Fe, Co and Ni simple substance metal spherical powder and Ni are mixed20Cr80、Mn75Fe25The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
7. A method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that Fe, Co and Ni simple substance metal spherical powder and Co are mixed35Cr65Placing the alloy spherical powder into a three-dimensional mixer to be mixed for 2-4 hours at the rotating speed of 20-40 r/min, wherein the particle diameters of the simple substance metal spherical powder and the alloy spherical powder are both 15-48 microns, and uniformly mixingThe spherical powder is dried in a vacuum dryer for 5-10 hours at the temperature of 50-100 ℃ and the vacuum degree of less than 10KPa absolute pressure, and the spherical powder is sealed and stored after drying to obtain the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
8. A method for preparing raw material powder for high-entropy alloy selective laser melting additive manufacturing is characterized in that Fe, Co and Ni simple substance metal spherical powder and Co are mixed35Cr65、Ti60Al40、Al35Fe65The method comprises the following steps of putting alloy spherical powder into a three-dimensional mixer, mixing for 2-4 hours, enabling the rotating speed of a cylinder to be 20-40 r/min, enabling the particle sizes of the simple substance metal spherical powder and the alloy spherical powder to be 15-48 micrometers, drying the uniformly mixed spherical powder in a vacuum dryer for 5-10 hours, enabling the temperature to be 50-100 ℃, enabling the vacuum degree to be less than 10KPa, sealing and storing after drying is completed, and obtaining the high-entropy alloy powder, wherein the mole numbers of all metal elements in the mixed high-entropy alloy powder are the same.
9. Use of the method for preparing raw material powder for selective laser melting additive manufacturing of high-entropy alloy according to any one of claims 1 to 8 in a process for selective laser melting in-situ additive manufacturing of high-entropy alloy.
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